• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:

    公开号:NL1019208A1
    申请号:NL1019208
    申请日:2001-10-22
    公开日:2002-11-12
    发明作者:William E Saver；E Ronald Mchenry
    申请人:Koppers Ind Of Delaware；
    IPC主号:
    专利说明:

    Process for the production of pitch mixtures from cage tar and hydrocarbons, using a highly efficient evaporative distillation process
    The present invention relates to the distillation of coal tar pitch or other coal-derived streams for the production of pitch mixtures of cage tar and hydrocarbons and other by-products, and in particular to the production of distillates and residues of mixtures of coal tar hydrocarbons using a highly efficient evaporative distillation method.
    Cage tar is a primary by-product obtained from the destructive distillation or carbonization of coal in coke. Although the coke is used as a fuel and as a reagent in the steel industry, the cage is distilled into a series of fractions, each of which are commercially suitable products in various fields of the art. An important part of the distilled cage tar is the pitch residue. This material is used in the production of anodes for aluminum smelting and also as electrodes for electric arc furnaces used in the steel industry. In assessing the qualitative characteristics of the pitch material, the art has hitherto mainly looked at the ability of the coal tar pitch material to provide a suitable binder used in anode and electrode manufacturing processes. Various characteristics such as softening point, specific density, percentage of material that is insoluble in quinoline (also known as QI, "quinoline insolubility"), and coke value have all served to provide charcoal pitch characteristics for applicability to these different manufacturing processes and these different manufacturing processes industries.
    The softening point determination is the basic determination used to determine the end point of the distillation process in the production of coal tar pitch and to determine the mixing, molding or mixing temperatures in the production of var. cabbage products. All softening points mentioned herein refer to the Mettler method or the ASTM Standard D3104. Additional features described herein include the QI, which is used to determine the amount of solid and high molecular weight material in the pitch. QI can also be referred to as α-resin and the standard test method used to determine the QI as a percentage by weight includes either ASTM Standard D4746 or ASTM Standard D2318. The percentage of material that is insoluble in toluene or the TI will also be used here and is determined by ASTM Standard D4072 or D4312.
    Mirtchi and Noël, in a publication preceded by Carbon '94 in Granada, Spain, entitled "Polycyclic Aromatic Hydrocarbons in Pitches Used in the Aluminum Industry", described and categorized the PAH content of coal tar pitch. These materials were classified for their carcinogenic or mutagenic effects on living organisms. The publication identified 14 PAH materials identified by the United States Environmental Protection Agency as potentially harmful to health. Each of the 14 materials is given a relative assessment of the carcinogenic potency that is based on a standard random assessment of a factor 1 associated with benzo (a) pyrene or B (a) P. Assessments of the potential toxicity of a pitch material can be made by converting the total PAH content to B (a) P equivalents, eliminating the need to name each of the 14 materials individually, and providing a useful more concise form for the assessment of the toxicity of a material.
    A typical coal tar binder pitch is characterized as shown in Table I.
    Two shortcomings with regard to the use of coal tar pitch in general and more particularly for the aluminum industry have recently become known. The first is an increased sensitivity to the environment of this material and application to aluminum melt anodes. The other is a decreasing supply of raw coal tar from the coke manufacturing process. Significant reductions in coke consumption, based on a variety of factors, have also reduced the availability of raw coal tar. This reduction in the production of these raw materials is likely to escalate in the near future and alternative sources of substitute products have been sought for some time. However, so far, no commercially attractive substitutes for coal tar pitch have been developed in the aluminum industry.
    There are two common methods for distilling coal tar, a continuous method and a batch method. Continuous distillation includes a constant supply of a material to be distilled, i.e., the coal tar, as well as the constant removal of the products or residue, i.e., the coal tar pitch. Traditional continuous distillations are typically performed at pressures of between 45 mm mercury and 60 mm mercury and at temperatures between 390 ° C and 400 ° C, usually producing a coal tar pitch with a maximum softening point of about 140 ° C. Batch distillation can be considered as a wprkwinzp in krnp.s en nl aatsvi ndendp. onnpvppr 7πρ1ς hpf kokpn of water. Large heat levels are developed due to the longer residence time of the coal tar in the crucible.
    Although higher softening purts of the tor. at 180 ° C using batch distillation, the combination of high heat and longer residence time can often lead to decomposition of the coal tar pitch and the formation of undesired mesc phase pitch. Processing times for coal tar distillation using this known continuous and batch distillation range from a few minutes to several hours, depending on the coal tar pitch to be obtained.
    Highly efficient evaporative distillation processes are known in which a material is subjected to an elevated temperature, generally in the range of 300 to 600 ° C and to reduced pressures, generally in the range of 5 Torr or less, in a distillation vessel, which releases lower molecular, more volatile components and separates them from highly molecular, less volatile components. Such a highly efficient evaporative distillation method can be performed using conventional distillation plants with an improved vacuum capability to operate in the aforementioned temperature and pressure ranges. In addition, highly efficient evaporative distillation processes can be carried out in an installation known as a "wiped film evaporator", or WFE (wiper film evaporator, or ironed film evaporator), and such a method is generally referred to as WFE processes. Accordingly, highly efficient evaporative distillation processes can be carried out in a device known as a thin film evaporator and such processes are commonly referred to as thin film evaporation processes. WFE and thin film evaporation processes are often used as efficient, relatively fast ways to continuously distill a material. In general, WFE and thin film evaporation methods include forming a thin layer of a material on a heated surface, usually the inner wall of a vessel or chamber, usually in the range of 300 to 600 ° C, while simultaneously applying a reduced pressure , usually in the range of 5 Torr or less. In a WFE process, the thin layer of the material is formed by a rotor, which is close to the inner wall of the vessel. In contrast, in a thin film evaporation method, the thin film evaporator is usually performed as a spinner configuration, such that the thin layer of material is formed on the inner wall of the vessel, due to the centrifugal force. WFE and thin film evaporation processes are continuous processes because they include the continuous supply of feedstock and the output of feedstock. Both the WFE installations and the thin filter evaporators are known in the art.
    5 One known WFE installation is described in
    Baird, in U.S. Patent No. 4,093,479. The installation, as described by Baird, comprises a cylindrical process chamber or a vessel. The process chamber is surrounded by a temperature-controlled jacket, which is suitable for receiving a heat exchange fluid. The process chamber comprises a feed input at one end and a product output at the other end.
    The process chamber of the installation as described by Baird comprises a vapor chamber with a vapor outlet. A condenser and a vacuum means can be placed in communication with the vapor outlet to allow condensation of the vapor formed under sub-atmospheric conditions. Extending from one end of the process chamber to the other end is a tubular motor-driven rotor. Extending axially, looking outwards from the rotor shaft, are a plurality of radial rotor blades which are arranged non-symmetrically rotated to extend radially from one end of the chamber to the other between the feed inlet and the product outlet. The rotor blades extend in a narrow, but generally uniform, tightly packed thin film ratio with respect to the inner wall of the process chamber, so that when the rotor turns, the rotor blades form a thin, extruded or turbulent film of the process material. on the inner wall of the process chamber.
    During operation, it is honored. material to be processed fed into the feed inlet by a pump or by gravity. The material is moved downwards and is distributed as a thin film on the inner wall of the process chamber by means of the rotating rotor blades. A heat-exchanging fluid, such as steam, is introduced into the temperature-controlled jacket so that the inner wall of the process chamber is heated to a constant, preselected temperature, whereby the controlled evaporation of the relatively volatile components of the material to be processed is obtained. A relatively non-volatile material is withdrawn from the product outlet and the vaporized volatile material is withdrawn from the vapor chamber through the vapor outlet.
    The present invention relates to a method for manufacturing a high softening coal tar pitch using highly efficient evaporative distillation. According to this method, a coal tar pitch is fed as a feed with a softening point in the range of 70 to 160 ° C into a process vessel, the process vessel being heated to a temperature in the range of 300 to 600 ° C and a pressure in the process vessel being held in the range of 5 Torr or less. A coal tar pitch is withdrawn from the process vessel as an output. The coal tar pitch withdrawn as output has a softening point in the range of 140 to 300 ° C and has less than 5% mesophase. A mesophase content of more than 5% in the coal tar pitch performed will reduce applicability as a binder for carbon-carbon composites and friction materials, as well as the performance in the production of graphite electrodes and anodes used in aluminum production. Preferred ranges for the coal tar pitch performed include a softening point in the range of 150 to 250 ° C and less than 1% mesophase. Also, the coal tar pitch carried out preferably has a B (a) P equivalent of less than or equal to 500 ppm. The coal tar pitch supplied may preferably have a softening point in the range of 110 to 140 ° C and the process vessel may preferably be heated to a temperature in the range of 350 to 500 ° C.
    The coal tar pitch performed may also be combined with a softening agent such as a low viscosity coal tar, preferably between 2 and 5 centistokes at 210 ° F, a layer B (a) P equivalent, preferably no more than 500 ppm B (a) P, or such a coal tar can be combined with a petroleum oil, the petroleum oil making up 30 to 60% of the mixture.
    The present invention also relates to a method for making a coal tar pitch which has no quinoline insoluble content and no ash, but with a desired softening point. According to the method, a supplied coal tar pitch with a softening point in the range of 70 to 160 ° C is supplied to a process vessel, wherein the process vessel is heated to a temperature in the range of 300 to 600 ° C and where a pressure in the process vessel is in the range of 5 Torr or less. A distillate that has no non-quinoline-soluble substances and no ash with a softening point in the range of 25 to 60 ° C is obtained from the process vessel. The distillate is heat treated at a temperature in the range of 350 to 595 ° C for five minutes to forty hours.
    The heat-treated distillate can then be distilled to obtain a pitch with the desired softening point.
    The present invention also relates to a method for manufacturing a mesophase coal tar pitch with 70 to 100% mesophase. According to this method, a supplied coal tar pitch with a softening point in the range of 70 to 160 ° C is supplied to a process vessel, wherein the process vessel is heated to a temperature in the range of 300 to 600 ° C and where a pressure is in the process vessel in the range of 5 Torr or less. A distillate with no quinoline-insoluble material and no ash, and with a softening point in the range of 25 to 60 ° C is obtained from the process vessel. The distillate is heat treated at a temperature in the range of 370 to 595 ° C for three to forty hours.
    The present invention also relates to a method for manufacturing a coal tar pitch which does not have a qumoline-insoluble material and no ash. The method comprises steps var. feeding a supplied coal tar pitch with a softening point in the range of 70 to 160 ° C in a first process vessel, wherein the first process vessel is heated to a temperature in the range var. 300 to 600 ° C and with a pressure in the process vessel in the range of 5 Torr or less, obtaining a distillate free of non-quinoline-soluble substances and free of ash, with a softening point in the range of 25 to 60: C from the first process vessel, heat-treating the distillate at a temperature in the range of 350 to 595 ° C for five minutes to forty hours, distilling the heat-treated distillate to obtain a pitch with a desired softening point, supplying the pitch with a desired softening point to a second process vessel, wherein the second process vessel is heated to a temperature in the range var. 300 to 600 ° C, and withdrawing a coal tar pitch to be carried out from the second process vessel. The first and the second process vessel can be the same vessel or can be different vessels.
    Optionally, a hydrocarbon mixture, such as a mixture of coal tar pitch and petroleum pitch, can be used as a feed material instead of the coal tar pitch to be supplied in any of the methods of the present invention. The hydrocarbon mixture preferably has a collier pitch content of at least 50%.
    Any of the methods of the present invention can be performed using conventional distillation plants with the ability to operate at specific temperatures and pressures, a coated film evaporator (WFE) or a thin film evaporator.
    According to the present invention, a coal tar pitch with a high softening point and low volatility is produced by processing a feed coal tar pitch with a softening point in the range of 70 to 160 ° C and preferably in the range of 110 to 140 ° C, using of a highly effective evaporative distillation process carried out in a process vessel operating at temperatures of 300 to 600 ° C and pressures of 5 Torr or less. This temperature range is important because operating below the soil temperature will not provide the desired softening point in the output material and operating at a temperature higher than the upper temperature will result in thermal cracking and thermal degradation of the output material. Accordingly, the pressure range 5 is important because, if the pressure is higher than the specified highest pressure range, higher processing temperatures will be required to achieve the desired softening point, which higher temperatures will result in thermal cracking and thermal degradation of the output material.
    According to the present invention, the operation can be performed using a WFE installation and for purposes of illustration and not limitation, the present invention will be described with reference to an operation using a WFE installation. It will be understood, however, that conventional distillation plants and conventional thin film evaporators can be used as long as such plants and evaporators can operate at the temperatures and pressures described herein. In the cases where a thin film evaporator is used, the thin film evaporator will preferably form a film on the inner wall thereof with a minimum thickness not less than the thickness of the largest Q1 particles contained in the feed material.
    Any known WFE installation can be used as long as it is suitable for operating at temperatures of 300 to 600 ° C and pressures of 5 Torr or less. The WFE installation should preferably be suitable for processing a minimum film thickness of 1 millimeter and for applying a scraping speed of 200 to 3,000 revolutions per minute. The process chamber or vessel wall of the WFE is heated to a temperature of between 300 and 600 ° C, and preferably between 350 and 500 ° C. The appropriate feed rate of the feed coal tar pitch in the WFE plant will depend on the available processing surface of the vessel. The feed rate should be between 10 and 100 pounds per square foot of area per hour, and preferably between 35 and 50 pounds per square foot of area per hour. If the feed coal tar pitch is fed into the WFE installation at a speed between 10 and 100 pounds per square foot area per hour, the residence time of the feed coal tar pitch in the WFE installation will be approximately 1 to 60 seconds. If the feed coal tar pitch is supplied at the preferred rate between 35 and 50 pounds per square foot per hour, the residence time of the feed coal tar pitch in the WFE plant will be about 5 to 30 seconds. The WFE residue will be an output coal tar pitch with a softening point in the range of 140 to 300 ° C, preferably from 150 to 250 ° C, and with minimal mesophase formation from 0 to 51, preferably 0 to 1%. In the case where the conventional distillation plant is adapted to operate at the specified temperatures and pressures, the output coal tar pitch will have a softening point in the range of 140 to 180 ° C. In order to obtain softening points in the coal tar pitch to be carried out, which are higher than 180 ° C according to the present invention, it is necessary to use a WFE or a thin film evaporator, because the residence time required to obtain softening points of the output coal tar pitch of higher than 180 ° C using a conventional distillation plant, will produce undesirable results such as the production of excess mesophase. The use of a highly efficient evaporative distillation method such as a WFE method also allows the removal of PAHs, in particular benzo (a) pyrene, with high boiling points from the coal tar pitch to be supplied, resulting in a coal tar pitch to be carried out with a B (a) P equivalent of no more dar. 5 500 ppm. The yield of the coal tar pitch to be carried out at a certain vessel temperature depends on the softening point of the coal tar pitch to be supplied.
    EXAMPLES
    0
    Further details of the present invention are shown in the following examples:
    Example 1
    A coal tar pitch to be supplied with a softening point of 109 ° C is fed into a WFE installation with a barrel of 1.4 square feet and which operates at a temperature of 335 ° C and a feed rate of 77 pounds per square foot area per hour. The coal tar pitch from the WFE installation has a pitch yield of 0 85%. A laboratory analysis of the coal tar pitch carried out is summarized in the following Table II:
    Example 2
    A charcoal tar pitch with a softening point of 109 ° C is fed into a WFE installation with a 1.4 square foot barrel operating at a temperature of 335 ° C
    at a feeding rate of 95 pounds per square foot per hour. The coal tar pitch carried out by the WFE installation has a pitch yield of 73%.
    A laboratory analysis of the coal tar pitch carried out is summarized in the following Table III:
    Example 3
    A feed coal tar pitch with a softening point of 109 ° C is supplied to a WFE plant with a 1.4 square foot barrel operating at a temperature of 350 ° C at a feed rate of 65 pounds per square foot per hour. The coal tar pitch of the WFE installation has a pitch yield of 74.2%. A laboratory analysis of the coal tar pitch carried out is summarized in the following table IV:
    Example 4
    A feed coal tar pitch with a softening point of 109 ° C is supplied to a WFE plant with a 1.4 square foot barrel operating at a temperature of 365 ° C at a feed rate of 67 pounds per square foot per hour. The coal tar pitch of the WFE installation has a pitch yield of 67%. A laboratory analysis of the coal tar pitch carried out is summarized in the following table V:
    The coal tar pitch carried has a softening point in the range of 140 to 300 ° C and preferably in the range of 150 to 250 ° C and this can be used as a binder for carbon-carbon composites and friction materials, as well as in the production of graphite electrodes and anodes used for aluminum production. In addition, the coal tar pitch carried out with a softening point in the range of 140 to 300 ° C, and preferably in the range of 150 to 250 ° C, can be combined with a plasticizer to yield a pitch with a softening point of 110 ° C, suitably for use in the production of aluminum anodes, including Söderberg binder pitch, and any other industrial application where very low PAH levels are required. The plasticizer can be a coal tar with a low viscosity, preferably between 2 and 5 centistokes at 210 ° F, a low B (a) P equivalent, preferably no more than 500 ppm E (a] 8, or such a cage tar in combination with a petroleum oil, the petroleum oil constituting 30 to 60% of the mixture A suitable plasticizer is the coal tar pitch mixture described by McHenry et al. in U.S. Patent No. 5,746,906, the contents of which are herein incorporated by reference. is included.
    Optionally, according to an alternative embodiment of the present invention, a hydrocarbon mixture, such as a mixture of coal tar pitch and petroleum pitch, may be used as a food material instead of the supplied coal tar pitch. The hydrocarbon mixture in this embodiment preferably has a coal tar pitch content of at least 50%. The distillate obtained by using a hydrocarbon mixture as a food material can then be used in the methods to be described below.
    The distillate that is released during the processing of the coal tar pitch supplied in the WFE plant will be free from quinoline-soluble materials, which, as used herein, means that it has a QI in the range of 0 to 0.5% as well as being ash-free, which, as used herein, means that it has an ash content in net trajact of 0 to 0.1%. A distillate that is Q1-free and ash-free is desirable for at least two reasons. First, the distillate can be used to form materials that will be used as an impregnating pitch to fill porosity in carbon structures, and QI and ash are known to prevent the ability to fill such a porosity. Second, the distillate can be used to form mesophase pitch, and QI is known as a material that impedes the coalescence of the mesophase beads. The distillate will comprise a pitch with a softening point in the range of 25 to 60 ° C.
    The distillate can be used to produce a Q1-free and ash-free pitch with a desired high softening point by first performing a heat treatment of the distillate at temperatures between 350 and 595 ° C for between 5 minutes and 40 hours. The heat treatment step can be carried out, for example, by placing a distillate in a flask containing a short distillation column and heating and stirring the distillate therein under a light vacuum of no more than 600 mm Hg absolute. The heat treatment step of the distillate will lead to a pitch with a softening point in the range of 60 to 110 ° C. The heat-treated distillate can then be distilled in the usual manner and by the usual means to obtain a pitch residue with a desired softening point. The resulting pitch can be used in the production of carbon fibers and fuel cells. Alternatively, a Q1-free pitch with a narrow boiling range can be obtained by further processing of the Q1-free and ash-free pitch as obtained by heat treatment and distillation using a highly efficient evaporating distillation method, such as a WFE or a thin film evaporation method at temperatures in the range of 300 to 600 ° C and pressures of no greater than 5 Torr, the narrow boiling pitch being the residue of such processing.
    EXAMPLE
    Further details of the present invention are shown in the following example:
    Example 1
    A distillate with a softening point of 25 to 30 ° C, obtained from a feed coal tar pitch with a softening point of 110 ° C is subjected to heat treatment at 360 ° C for about 8 hours to obtain a pitch with a softening point of 6 ° C. The pitch with a softening point of 60 ° C is distilled in a batch / pot distillation at an "overhead" temperature of 400 ° C to obtain a pitch with a softening point of 98.9 ° C at a 70% yield. A laboratory analysis of the resulting pitch is summarized in the following Table VI:
    Optionally, a mesophase pitch with a mesophase content in the range of 70 to 100%, and preferably in the range of 75 to 85%, can be made from the distillate by heat treatment of the distillate at temperatures between 370 and 595 ° C for between 3 and 3 40 hours. The yield of the mesophase pitch is generally in the range of 70 to 1001. The mesophase pitch can be used with carbon fibers, lithium batteries, and graphite foam. If the mesophase content is lower than 70%, the resulting product produced from the mesophase pitch will not have the necessary planar structure, leading to a finished product with unacceptably low strength.
    The terms and the expression used herein are used for description only and not for limitation, and with the use of these terms and expressions, there is no intention to express corresponding equivalents of properties as shown and described or parts thereof. and it should be noted that various modifications are possible within the scope of the invention. Although various particular embodiments of the present invention have been shown in the foregoing detailed description, it is further to be understood that the present invention is not limited to only these described embodiments, but that innumerable changes, modifications, and substitutions are possible.
    权利要求:
    Claims (106)
    [1]
    A method for manufacturing a coal tar pitch with a high softening point by using highly efficient evaporative distillation, comprising the steps of: feeding a feed coal tar pitch with a softening point in the range of 70 to 160 ° C in a process vessel, wherein process vessel is heated to a temperature in the range of 300 to 600 ° C and where a pressure in the process vessel is 5 Torr or less; and withdrawing an output coal tar pitch from the process vessel, the output coal tar pitch having a softening point in the range of 140 to 300 ° C and a mesophase content of less than 5%.
    [2]
    The method of claim 1, wherein the output coal tar pitch has a softening point in the range of 150 to 250 ° C.
    [3]
    The method of claim 1, wherein the output coal tar pitch has less than 1% mesophase content.
    [4]
    The method of claim 1, wherein the feed coal tar pitch has a softening point in the range of 110 to 140 ° C.
    [5]
    The method of claim 1, wherein the process vessel is heated to a temperature in the range of 350 to 500 ° C.
    [6]
    The method of claim 1, wherein the output coal tar pitch has a B (a) P equivalent of less than or equal to 500 ppm.
    [7]
    The method of claim 1, wherein the feeding step comprises feeding the feed coal tar pitch into a coated film evaporator, which coated film evaporator comprises the process vessel.
    [8]
    The method of claim 7, wherein a feed rate of the feed coal tar pitch in the coated film evaporator is in the range of 10 to 100 pounds per 5 square feet of area per hour.
    [9]
    The method of claim 7, wherein a feed rate of the feed coal tar pitch in the coated film evaporator is in the range of 35 to 50 pounds per square foot area per hour.
    [10]
    The method of claim 8, wherein a residence time of the feed coal tar pitch in the process vessel is in the range of 1 to 60 seconds.
    [11]
    The method of claim 9, wherein a residence time of the feed coal tar pitch in the process vessel is in the range of 5 to 30 seconds.
    [12]
    The method of claim 7, wherein the coated film evaporator forms a film of the feed coal tar pitch on an inner wall of the process vessel, which film has a minimum thickness of 1 millimeter.
    [13]
    The method of claim 1, wherein the feeding step comprises supplying the feed coal tar pitch to a thin film evaporator, wherein the thin film evaporator comprises the process vessel.
    [14]
    The method of claim 13, wherein a feed rate of the feed coal tar pitch in the thin film evaporator is in the range of 10 to 100 pounds per square foot area per hour.
    [15]
    The method of claim 13, wherein a feed rate of the feed coal tar pitch in the thin film evaporator is in the range of 35 to 50 pounds per square foot area per hour.
    [16]
    The method of claim 14, wherein a residence time of the feed coal tar pitch in the process vessel is in the range of 1 to 60 seconds.
    [17]
    The method of claim 15, wherein a residence time of the feed coal tar pitch in the process vessel is in the range of 5 to 30 seconds.
    [18]
    The method of claim 13, wherein the thin film evaporator forms a film of the feed coal tar pitch on an inner wall of the process vessel, the feed coal tar pitch comprising a plurality of QI particles, said film having a minimum thickness not less than the thickness of a largest Ql particle.
    [19]
    19. Method according to claim 1, wherein the feeding step comprises supplying the feed coal tar pitch to a conventional distillation plant, which conventional distillation plant comprises the process vessel, wherein the output coal tar pitch has a softening point in the range of 140 to 180 ° C.
    [20]
    20. A method of manufacturing a pitch using high efficient evaporative distillation, comprising the steps of: feeding a feed coal tar pitch with a softening point in the range of 70 to 160 ° C in a process vessel, the process vessel being heated to a temperature in the range of 300 to 600 ° C and wherein a pressure in the process vessel is 5 Torr or less; L5 withdrawing an output coal tar pitch from the process vessel, which output coal tar pitch has a softening point in the range of 140 to 300 ° C and has less than 5% mesophase content; and combining the output coal tar pitch with a plasticizer.
    [21]
    The method of claim 20, wherein the plasticizer comprises a coal tar with a viscosity in the range of 2 to 5 centistokes at 210 ° F and a B (a) P equivalent of no more than 500 ppm B (a) P.
    [22]
    The method of claim 21, wherein the plasticizer comprises a mixture of the coal tar and a petroleum oil, which petroleum oil constitutes 30 to 60% of the mixture.
    [23]
    The method of claim 20, wherein the feeding step comprises supplying the coal tar pitch to a 50-coated film evaporator, which coated film evaporator comprises the process vessel.
    [24]
    The method of claim 20, wherein the feeding step comprises supplying the coal tar pitch to a thin film evaporator, which thin film evaporator comprises the process vessel 55.
    [25]
    The method of claim 20, wherein the feeding step comprises supplying the feed coal tar pitch to a conventional distillation plant, which conventional distillation plant comprises the process vessel, wherein the output coal tar pitch has a softening point in the range of 140 to 180 ° C.
    [26]
    The method of claim 20, wherein the output coal tar pitch has a softening point in the range of 150 to 250 ° C.
    [27]
    The method of claim 20, wherein the feed coal tar pitch has a softening point in the range of 110 to 140 ° C.
    [28]
    The method of claim 20, wherein the process vessel is heated to a temperature in the range of 350 to 500 ° C.
    [29]
    A method for making a Q1-free and ash-free coal tar pitch with a desired softening point, comprising the steps of: supplying a feed coal tar pitch with an original softening point in the range of 70 to 160 ° C in a process vessel, the process vessel being heated to a temperature in the range of 300 to 600 ° C and wherein a pressure in the process vessel is 5 Torr or less; obtaining a distillate from the process vessel, which distillate has a softening point in the range of 25 to 60 ° C and is Q1-free and ash-free; heat treating the distillate at a temperature in the range of 350 to 595 ° C for between five minutes and forty hours; and distilling the heat-treated distillate to obtain a pitch with the desired softening point.
    [30]
    The method of claim 29, wherein the feeding step comprises supplying the feed coal tar pitch to a coated film evaporator, which coated film evaporator comprises the process vessel.
    [31]
    The method of claim 29, wherein the feeding step comprises supplying the feed coal tar pitch to a thin film evaporator, which thin film evaporator comprises the process vessel.
    [32]
    The method of claim 29, wherein the feeding step comprises supplying the feed coal tar pitch to a conventional distillation plant, which conventional distillation plant comprises the process vessel.
    [33]
    The method of claim 29, wherein the heat-treated distillate has a softening point in the range of 60 to 110 ° C.
    [34]
    A method of manufacturing a mesophase coal tar pitch comprising the steps of: feeding a feed coal tar pitch with a softening point in the range of 70 to 160 ° C in a process vessel, the process vessel being heated to a temperature in the range of 300 up to 600 ° C and wherein a pressure in the process vessel is 5 Torr or less; Obtaining a distillate from the process vessel, which distillate has a softening point in the range of 25 to 60 ° C and is Q1-free and ash-free; and heat treating the distillate at a temperature in the range of 370 to 595 ° C for between three and forty hours.
    [35]
    The method of claim 34, wherein the feeding step comprises supplying the feed coal tar pitch to a coated film evaporator, which coated film evaporator comprises the process vessel.
    [36]
    The method of claim 34, wherein the feeding step comprises supplying the feed coal tar pitch to a thin film evaporator, which thin film evaporator comprises the process vessel.
    [37]
    The method of claim 34, wherein the feeding step comprises supplying the feed coal tar pitch to a conventional distillation plant, which conventional distillation plant comprises the process vessel.
    [38]
    38. A method for manufacturing a Q1-free and ash-free coal tar pitch, comprising the steps of: supplying a feed coal tar pitch with a softening point in the range of 70 to 160 ° C in a first process vessel, wherein the first process vessel is heated to a temperature in the range of 300 to 600 ° C and wherein a pressure in the first process vessel is 5 Torr or less; obtaining a distillate from the first process vessel, which distillate has a softening point in the range of 25 to 60 ° C and is QI-free and ash-free; heat treating the distillate at a temperature in the range of 350 to 595 ° C for between five minutes and forty hours; distilling the heat-treated distillate to obtain a pitch with a desired softening point; supplying the pitch with a desired softening point in a second process vessel, wherein the second process vessel is heated to a temperature in the range of 300 to 600 ° C; and withdrawing an output coal tar pitch from the second process vessel.
    [39]
    The method of claim 38, wherein the first process vessel and the second process vessel are the same vessel.
    [40]
    The method of claim 39, wherein the first and second process vessels are a coated film evaporator.
    [41]
    The method of claim 38, wherein the first process vessel comprises a coated film evaporator.
    [42]
    The method of claim 38, wherein the second process vessel comprises a coated film evaporator.
    [43]
    The method of claim 39, wherein the first and second process vessels are a thin film evaporator.
    [44]
    The method of claim 38, wherein the first process vessel is a. thin film evaporator.
    [45]
    The method of claim 38, wherein the second process vessel comprises a thin film evaporator.
    [46]
    The method of claim 39, wherein the first and second process vessels comprise a conventional distillation plant.
    [47]
    The method of claim 38, wherein the first process vessel further comprises a conventional distillation plant.
    [48]
    The method of claim 38, wherein the second process vessel further comprises a conventional distillation plant.
    [49]
    49. A method of manufacturing a high softening point hydrocarbon blend pitch using high efficient evaporative distillation, comprising the steps of: feeding a feed hydrocarbon blend pitch with a softening point in the range of 70 to 160 ° C to a process vessel wherein the process vessel is heated to a temperature in the range of 300 to 600 ° C and wherein a pressure in the process vessel is 5 Torr or less; and withdrawing an output hydrocarbon mixture pitch from the process vessel, the output hydrocarbon mixture pitch having a softening point in the range of 140 to 300 ° C and having less than 5% mesophase content.
    [50]
    The method of claim 49, wherein the output hydrocarbon blend pitch has a softening point in the range of 150 to 250 ° C.
    [51]
    The method of claim 49, wherein the output hydrocarbon mixture pitch has less than 1% mesophase content.
    [52]
    The method of claim 49, wherein the feed hydrocarbon blend pitch has a softening point in the range of 110 to 140 ° C.
    [53]
    The method of claim 49, wherein the process vessel is heated to a temperature in the range of 3 350 to 500 ° C.
    [54]
    The method of claim 49, wherein the output hydrocarbon mixture pitch has a B (a) P equivalent of less than or equal to 500 ppm.
    [55]
    55. The method of claim 49, wherein the feeding step comprises supplying the feed hydrocarbon mixture pitch to a coated film evaporator, which coated film evaporator comprises the process vessel.
    [56]
    The method of claim 55, wherein a feed rate of the feed hydrocarbon blend pitch to the coated film evaporator is in the range of IC to 10 pounds per square foot area per hour.
    [57]
    The method of claim 55, wherein a feed rate of the feed hydrocarbon blend pitch to the coated film evaporator is in the range of 35 to 50 pounds per square foot area per hour.
    [58]
    The method of claim 56, wherein a residence time of the feed hydrocarbon mixture pitch to the process vessel is in the range of 1 to 60 seconds.
    [59]
    The method of claim 57, wherein a residence time of the feed hydrocarbon mixture pitch in the process vessel is in the range of 5 to 30 seconds.
    [60]
    The method of claim 55, wherein the coated film evaporator forms a film of the feed hydrocarbon mixture pitch on an inner wall of the process vessel, which film has a minimum thickness of 1 millimeter.
    [61]
    The method of claim 49, wherein the feeding step comprises supplying the feed hydrocarbon mixture pitch to a thin film evaporator, which thin film evaporator comprises the process vessel.
    [62]
    The method of claim 61, wherein a feed rate of the feed hydrocarbon blend pitch to the thin film evaporator is in the range of 10 to 100 pounds per square foot area per hour.
    [63]
    The method of claim 61, wherein a feed rate of the feed hydrocarbon blend pitch to the thin film evaporator is in the range of 35 to 50 pounds per square foot area per hour.
    [64]
    The method of claim 62, wherein a residence time of the feed hydrocarbon mixture pitch at the process vessel is in the range of 1 to 60 seconds.
    [65]
    The method of claim 63, wherein a residence time of the feed hydrocarbon mixture pitch at the process vessel is in the range of 5 to 30 seconds.
    [66]
    The method of claim 5461, wherein the thin film evaporator forms a film of the feed hydrocarbon mixture pitch on an inner wall of the process vessel, the feed hydrocarbon mixture pitch comprising a plurality of Q1 particles, which film has a minimum thickness not less than a thickness of one largest Ql particle.
    [67]
    The method of claim 49, wherein the feeding step comprises supplying the feed hydrocarbon mixture pitch to a conventional distillation plant, which conventional distillation plant comprises the process vessel.
    [68]
    The method of claim 49, wherein the feed hydrocarbon mixture pitch comprises a mixture of coal tar pitch and petroleum pitch.
    [69]
    The method of claim 68, wherein the feed hydrocarbon mixture pitch comprises at least 50 minste coal tar pitch.
    [70]
    70. A method for manufacturing a pitch using high efficient evaporative distillation, comprising the steps of: feeding a 7 feed hydrocarbon mixture pitch with a softening point in the range of 70 to 160 ° C to a process vessel, the process vessel being heated to a temperature in the range of 300 to 600 ° C and wherein a pressure in the process vessel is 5 Torr or less; Withdrawing an output hydrocarbon mixture pitch from the process vessel, which output hydrocarbon mixture pitch has a softening point in the range of 140 to 300 ° C and contains less than 5% mesophase content; and 7 combining the output hydrocarbon mixture pitch with a plasticizer.
    [71]
    The method of claim 70, wherein the plasticizer comprises a coal tar with a viscosity in the range of 2 to 5 centistokes at 210 ° C and a B (a) P equivalent of not more than 500 ppm B (a) P.
    [72]
    The method of claim 71, wherein the plasticizer comprises a mixture of the coal tar and a petroleum oil, which petroleum oil constitutes 30 to 601 of the mixture.
    [73]
    The method of claim 70, wherein the supplying step comprises supplying the feed hydrocarbon mixture pitch to a coated film evaporator, which coated film evaporator comprises the process vessel.
    [74]
    The method of claim 70, wherein the feeding step comprises supplying the feed hydrocarbon mixture pitch to a thin film evaporator, which thin film evaporator comprises the process vessel.
    [75]
    The method of claim 70, wherein the feeding step comprises supplying the feed hydrocarbon mixture pitch to a conventional distillation plant, which conventional distillation plant comprises the process vessel.
    [76]
    The method of claim 70, wherein the output hydrocarbon mixture pitch has a softening point in the range of 150 to 250 ° C.
    [77]
    The method of claim 70, wherein the feed hydrocarbon blend pitch has a softening point in the range of 110 to 140 ° C.
    [78]
    The method of claim 70, wherein the process vessel is heated to a temperature in the range of 350 and 500 ° C.
    [79]
    The method of claim 70, wherein the feed hydrocarbon mixture pitch comprises a mixture of coal tar pitch and petroleum pitch.
    [80]
    The method of claim 79, wherein the feed hydrocarbon mixture pitch comprises at least 50% coal tar pitch.
    [81]
    A method for producing a Q1-free and ash-free hydrocarbon mixture pitch with a desired softening point, comprising the steps of: supplying a feed hydrocarbon mixture pitch with an initial softening point in the range of 70 to 160 ° G to a process vessel, wherein the process vessel. is heated to a temperature in the range of 300 to 600 ° C and wherein a pressure in the process vessel is 5 Torr or less; obtaining a distillate from the process vessel, which distillate has a softening point in the range of 25 to 60 ° C and is Q1-free and ash-free; heat treating the distillate at a temperature in the range of 350 to 595 ° C for between five minutes and forty hours; and distilling the heat-treated distillate to obtain a pitch with the desired softening point.
    [82]
    The method of claim 81, wherein the feeding step comprises supplying the feed hydrocarbon mixture pitch to a coated film evaporator, which coated film evaporator comprises the process vessel.
    [83]
    The method of claim 81, wherein the feeding step comprises supplying the feed hydrocarbon mixture pitch to a thin film evaporator, which thin film evaporator comprises the process vessel.
    [84]
    The method of claim 81, wherein the feeding step comprises supplying the feed hydrocarbon mixture pitch to a conventional distillation plant, which conventional distillation plant comprises the process vessel.
    [85]
    The method of claim 81, wherein the heat-treated distillate has a softening point in the range of 60 to 110 ° C.
    [86]
    The method of claim 81, wherein the feed hydrocarbon mixture pitch comprises a mixture of coal tar pitch and petroleum pitch.
    [87]
    The method of claim 86, wherein the feed hydrocarbon mixture pitch comprises at least 50% coal tar pitch.
    [88]
    88. A method for making a mesophase hydrocarbon mixture pitch, comprising the steps of: supplying a feed hydrocarbon mixture pitch with a softening point in the range of 70 to 160 ° C to a process vessel, wherein the process vessel is heated to a temperature in the range of 300 up to 600 ° C and wherein a pressure in the process vessel is 5 Torr or less; obtaining a distillate from the process vessel, which distillate has a softening point in the range of 25 to 60 ° C and is Q1-free and ash-free; and heat treating the distillate at a temperature in the range of 370 to 595 ° C for between three and forty hours.
    [89]
    The method of claim 88, wherein the feeding step comprises supplying the feed hydrocarbon mixture pitch to a coated film evaporator, which coated film evaporator comprises the process vessel.
    [90]
    The method of claim 88, wherein the feeding step comprises supplying the feed hydrocarbon mixture pitch to a thin film evaporator, which thin film evaporator comprises the process vessel.
    [91]
    The method of claim 88, which feeding step comprises supplying the feed hydrocarbon mixture pitch to a conventional distillation plant, which conventional distillation plant comprises the process vessel.
    [92]
    The method of claim 88, wherein the feed hydrocarbon mixture pitch comprises a mixture of coal tar pitch and petroleum pitch.
    [93]
    The method of claim 92, wherein the feed hydrocarbon mixture pitch comprises at least 50% coal tar pitch.
    [94]
    A method for making a Q1-free and ash-free hydrocarbon mixture pitch, comprising the steps of: supplying a feed hydrocarbon mixture pitch with a softening point in the range of 70 to 160 ° C to a first process vessel, wherein the first process vessel is heated to a temperature in the range of 300 to 600 ° C and wherein a pressure in the first process vessel is 5 Torr or less; obtaining a distillate from the first process vessel, which distillate has a softening point in the range of 25 to 60 ° C and is Q1-free and ash-free; heat treating the distillate at a temperature in the range of 350 to 595 ° C for between five minutes and forty hours; distilling the heat-treated distillate to obtain a pitch with a desired softening point; supplying the pitch with a desired softening point to a second process vessel, wherein the second process vessel is heated to a temperature in the range of 300 to 500 ° C; and withdrawing an output hydrocarbon mixture pitch from the second process vessel.
    [95]
    The method of claim 94, wherein the first process vessel and the second process vessel are the same vessel.
    [96]
    The method of claim 95, wherein the first and the second process vessels are a coated film evaporator.
    [97]
    The method of claim 94, wherein the first process vessel comprises a coated film evaporator.
    [98]
    The method of claim 94, wherein the second process vessel comprises a coated film evaporator.
    [99]
    The method of claim 95, wherein the first and the second process vessels are a thin film evaporator.
    [100]
    The method of claim 94, wherein the first process vessel comprises a thin film evaporator.
    [101]
    The method of claim 94, wherein the second process vessel comprises a thin film evaporator.
    [102]
    The method of claim 95, wherein the first and the second process vessels comprise a conventional distillation plant.
    [103]
    The method of claim 94, wherein the first process vessel further comprises a conventional distillation plant.
    [104]
    The method of claim 94, wherein the second process vessel further comprises a conventional distillation plant.
    [105]
    The method of claim 94, wherein the feed hydrocarbon mixture pitch comprises a mixture of coal tar pitch and petroleum pitch.
    [106]
    The method of claim 105, wherein the feed hydrocarbon mix pitch comprises at least 50% coal tar pitch.
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    同族专利:
    公开号 | 公开日
    AU2002305517A1|2002-11-25|
    EP2363446A2|2011-09-07|
    US20050081752A1|2005-04-21|
    EP2363619A3|2014-08-06|
    US20040168612A1|2004-09-02|
    DE10138657A1|2002-11-28|
    US20050263436A1|2005-12-01|
    CA2446789A1|2002-11-21|
    US7033485B2|2006-04-25|
    US20020185411A1|2002-12-12|
    WO2002092728A2|2002-11-21|
    US7465387B2|2008-12-16|
    EP1401960A2|2004-03-31|
    CA2357237A1|2002-11-11|
    WO2002092728A3|2004-01-15|
    JP2002338967A|2002-11-27|
    EP2363619A2|2011-09-07|
    JP2004526658A|2004-09-02|
    ZA200506071B|2006-03-29|
    JP2005325364A|2005-11-24|
    ZA200308434B|2005-10-26|
    US7066997B2|2006-06-27|
    EP1401960A4|2010-02-17|
    US20060230982A1|2006-10-19|
    EP2363446A3|2013-05-15|
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    法律状态:
    2003-01-06| AD1A| A request for search or an international type search has been filed|
    2003-04-01| RD2N| Patents in respect of which a decision has been taken or a report has been made (novelty report)|Effective date: 20030203 |
    优先权:
    申请号 | 申请日 | 专利标题
    US09/853,372|US7033485B2|2001-05-11|2001-05-11|Coal tar and hydrocarbon mixture pitch production using a high efficiency evaporative distillation process|
    US85337201|2001-05-11|
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