CN111205889A - Wax for high-temperature printing ink and preparation method thereof - Google Patents

Wax for high-temperature printing ink and preparation method thereof Download PDF

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Publication number
CN111205889A
CN111205889A CN201811390218.7A CN201811390218A CN111205889A CN 111205889 A CN111205889 A CN 111205889A CN 201811390218 A CN201811390218 A CN 201811390218A CN 111205889 A CN111205889 A CN 111205889A
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China
Prior art keywords
wax
fischer
temperature
tropsch synthesis
preparation
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Inventor
李俊诚
潘金亮
苗恒
钱震
菅青娥
郭良兰
马国清
周岩
郑会月
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Inner Mongolia Yitai Coal Based New Materials Research Institute Co Ltd
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Inner Mongolia Yitai Coal Based New Materials Research Institute Co Ltd
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Priority to CN201811390218.7A priority Critical patent/CN111205889A/en
Publication of CN111205889A publication Critical patent/CN111205889A/en
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    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10GCRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G67/00Treatment of hydrocarbon oils by at least one hydrotreatment process and at least one process for refining in the absence of hydrogen only
    • C10G67/02Treatment of hydrocarbon oils by at least one hydrotreatment process and at least one process for refining in the absence of hydrogen only plural serial stages only
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D11/00Inks
    • C09D11/02Printing inks
    • C09D11/12Printing inks based on waxes or bitumen
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D11/00Inks
    • C09D11/30Inkjet printing inks
    • C09D11/34Hot-melt inks
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10GCRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G2300/00Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
    • C10G2300/10Feedstock materials
    • C10G2300/1022Fischer-Tropsch products

Abstract

A wax for high-temperature ink and a preparation method thereof, wherein the preparation method comprises the following steps: carrying out hydrofining on the Fischer-Tropsch synthesis intermediate wax to obtain Fischer-Tropsch synthesis refined wax; separating the Fischer-Tropsch synthesis refined wax, sequentially separating soft wax, medium hard wax and hard wax, and taking the finally obtained fraction as the ultra hard wax as the target fraction; and refining the target fraction, and then carrying out micronization process treatment to obtain the micronized wax for the high-temperature ink. The wax for the high-temperature printing ink has excellent wear resistance and solvent resistance in the field of high-temperature application, and can better improve the scratch resistance and wear resistance of the surface, increase the smoothness, resist the back adhesion, avoid the adhesion and improve the hand feeling; and can improve the anti-blocking and anti-fouling performance, control the glossiness of the printing ink and prevent the pigment from settling.

Description

Wax for high-temperature printing ink and preparation method thereof
Technical Field
The invention belongs to the technical field of chemical industry, and particularly relates to wax for high-temperature ink and a preparation method thereof.
Background
The wax is an auxiliary material of the ink, and the addition of the wax can increase the smoothness, the wear resistance and the print definition of the ink. Commonly used waxes are vegetable waxes, such as carnauba wax; animal waxes, such as beeswax; mineral waxes, such as ozokerite, paraffin, montan wax; synthetic waxes such as polyethylene wax, Fischer-Tropsch wax, higher fatty amide wax, and the like. The wax is added into the vehicle or the content of wax substances is increased, the aim is to reduce the problem of the printing ink caused by overlong filament head in the packaging and printing process, secondly, the problems of pigment and filler settlement and agglomeration of an ink system and the hardness of an ink film are solved, and the thickness of the ink film can be effectively improved. The addition of wax in the binder is very effective in solving the problems of printing paste, adhesion, insufficient coverage and the like. Meanwhile, wax is micronized, and the micronized wax is applied to printing ink, paint and coating, and is matched with matte powder to produce high-performance matte ink, paint and the like, so that the wax product is a main form for the application of the wax product in the production of the paint and the ink.
The wax is selected primarily with regard to melting point, crystallinity, melt viscosity, relative molecular mass distribution, and molecular structure. The high molecular weight wax has excellent wear resistance and solvent resistance, and the straight-chain high-crystallization wax has high density, high hardness and good solvent resistance.
The Fischer-Tropsch wax is a methylene polymer, is an alkane mixture obtained by catalytic polymerization of synthesis gas at medium temperature and pressure, and mainly comprises straight-chain saturated high-carbon alkane with the relative molecular mass of 500-1000. The carbon number distribution is wide, the highest carbon number can reach more than 100, the molecular weight is higher than that of paraffin, the composition is relatively simple, the content of normal straight-chain paraffin can reach more than 90%, the rest is basically branched-chain paraffin, cyclic hydrocarbon and aromatic hydrocarbon are basically not contained, compared with isoparaffin and cyclane, the normal paraffin is easy to form flaky large crystal when crystallized, the stability is good, the viscosity at high temperature is low, the fluidity of the ink can be improved, and the wettability to the printing surface is enhanced. This is precisely the greatest advantage of the use of fischer-tropsch waxes as waxes for producing high melting point, highly crystalline inks. Meanwhile, the Fischer-Tropsch wax has stable chemical properties, no corrosiveness, no pollution and no taste, so the Fischer-Tropsch wax is also an ideal raw material for producing the wax for the environment-friendly ink. However, the Fischer-Tropsch wax has a wide carbon number distribution range, and when the Fischer-Tropsch wax is directly used as a wax material for printing ink, the melting point is low, so that the high-temperature application performances such as wear resistance, solvent resistance and the like are affected, and therefore the Fischer-Tropsch wax needs to be processed.
In the existing report, aiming at the requirement of narrow carbon number distribution of hot-melt ink, the technology adopted is to distill a hydrofined Fischer-Tropsch synthesis product to obtain a target fraction (the final distillation point is below 550 ℃), then the fraction is used as a sweating raw material, and the wax for the ink with the melting point of above 70 ℃ is prepared by an improved sweating process treatment. The common sweating deoiling process can produce soap wax and low-melting-point paraffin with the melting point of 40-60 ℃, and is not suitable for producing wax products with the melting point of more than 70 ℃. It has been reported that fractions below 550 ℃ can be treated by improving the sweating process, but this is limited by the sweating process itself, which produces heavy fractions (melting point above 90 ℃) with a significant decrease in the yield accompanied by an increase in the carbon number concentration and n-alkane content of the sweating product.
Disclosure of Invention
In view of the above, the present invention provides a wax for high temperature ink and a preparation method thereof, which are used to provide a high molecular weight, high crystalline, low melt viscosity wax for ink.
In order to achieve the above object, in one aspect, the present invention provides a method for preparing a wax for high temperature ink, comprising:
carrying out hydrofining on the Fischer-Tropsch synthesis intermediate wax to obtain Fischer-Tropsch synthesis refined wax;
separating the Fischer-Tropsch synthesis refined wax, sequentially separating soft wax, medium hard wax and hard wax, and taking the finally obtained fraction as the ultra hard wax as the target fraction;
and refining the target fraction, and then carrying out micronization process treatment to obtain the micronized wax for the high-temperature ink.
In some embodiments, the Fischer-Tropsch wax has a melt drop point greater than 90 ℃ and an n-alkane content greater than 90 wt%.
In some embodiments, the hydrofinishing is operated at a temperature of 220 ℃ to 300 ℃ and at a pressure of 2 to 10 MPa.
In some embodiments, the separation is a two-stage or three-stage separation.
In some embodiments, the separation is a three-stage separation, wherein the first stage separation is operated at a pressure of 1-1000Pa and at a temperature of 100 ℃ and 200 ℃ for separating soft wax with a melting point of 40 + -5 ℃; the operation pressure of the second-stage separation is 0-100Pa, the operation temperature is 170-260 ℃ and is used for separating the medium-hard wax with the melting point of 70 +/-5 ℃, the operation pressure of the third-stage separation is 0-10Pa, the operation temperature is 270-320 ℃ and is used for separating the hard wax with the melting point of 90 +/-5 ℃.
In some embodiments, the first stage separation employs a vacuum distillation column or a thin film evaporator, and the second and third stage separations employ a short path evaporator.
In some embodiments, the ultra hard wax has a melt drop point greater than 110 ℃ and an end point greater than 550 ℃.
In some embodiments, the target fraction is purified by one or more methods selected from hydrofinishing, clay refining, or diatomaceous earth refining.
In some embodiments, the micronization process comprises: the refined target fraction is firstly crushed to 200 meshes of 100-.
On the other hand, the invention also provides the wax for the high-temperature printing ink prepared by the preparation method.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the application field of target products, the Fischer-Tropsch synthesis intermediate wax with the drop melting point of more than 90 ℃ and the normal paraffin content of more than 90 percent is preferably selected as the raw material, and the raw material is subjected to hydrofining treatment and narrow fraction separation, so that the production process is simplified;
2. the Fischer-Tropsch micronized wax for high-temperature ink has excellent wear resistance and solvent resistance in the field of high-temperature application, and can better improve the scratch resistance and wear resistance of the surface, increase the smoothness, resist the after-tack, avoid the adhesion and improve the hand feeling; the anti-blocking and anti-fouling performance is improved, the glossiness of the printing ink can be controlled, and the pigment is prevented from settling.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments.
The Fischer-Tropsch synthesis refined wax is obtained by hydrofining by taking Fischer-Tropsch synthesis intermediate wax (the drop melting point is more than 90 ℃ and the normal alkane content is more than 90 wt%) obtained by a low-temperature Fischer-Tropsch process as a raw material; separating the wax by N grade (N is more than or equal to 2), sequentially separating soft wax (melting point 40 +/-5 ℃), medium hard wax (melting point 70 +/-5 ℃) and hard wax (melting point 90 +/-5 ℃), and finally obtaining fraction (dropping melting point more than 110 ℃) which is super hard wax, refining and upgrading the target fraction, and carrying out micronization process to obtain the wax for the high-temperature micro-powder ink.
In some embodiments, the hydrofinishing is carried out at a temperature of 220 ℃ to 300 ℃, and in particular at 270 ℃ or 280 ℃, and at a pressure of 2 to 10MPa, and in particular at 5 or 6 MPa. The purpose of hydrofining is to hydrogenate a small amount of olefins in the saturated Fischer-Tropsch synthesis intermediate wax, hydrogenate a small amount of oxygen-containing organic matters in the reduced Fischer-Tropsch synthesis intermediate wax and hydrogenate and break a small amount of polycyclic hydrocarbons in the Fischer-Tropsch synthesis intermediate wax. If the substances are not removed, the color of the Fischer-Tropsch wax is influenced, and on the other hand, the substances are easy to generate coking and carbon deposition in subsequent processing treatment, so that the product quality and the normal production are influenced.
In some embodiments, the separation mode adopts two-stage or three-stage separation, preferably three-stage separation, the first-stage separation equipment can be a vacuum distillation tower or a thin film evaporator, the operation pressure is 1-1000Pa, the operation temperature is 100-200 ℃, and the soft wax component (the melting point is 40 +/-5 ℃) is separated; the second stage separation adopts a short-range evaporator with the operating pressure of 0-100Pa and the operating temperature of 170-260 ℃ to separate out medium hard wax (the melting point is 70 +/-5 ℃), the third stage separation adopts a short-range evaporator with the operating pressure of 0-10Pa and the operating temperature of 270-320 ℃ to separate out hard wax (the melting point is 90 +/-5 ℃), and the finally obtained fraction is the target fraction (the melting point is above 110 ℃ and the final distillation point is more than 550 ℃). The target fraction refining may be one or more of hydrofinishing, clay refining or diatomaceous earth refining. And crushing the refined target fraction to 100-200 meshes, and crushing to 500-1000 meshes by using a low-temperature freezing crusher to finally obtain the Fischer-Tropsch micronized wax for the high-temperature ink.
Example 1
The Fischer-Tropsch synthesis intermediate wax obtained by a Fischer-Tropsch synthesis process is used as a raw material, and is subjected to hydrofining to obtain the Fischer-Tropsch synthesis refined wax, wherein the hydrogenation temperature is 300 ℃, the operation pressure is 7Mpa, the Fischer-Tropsch refined wax has a melting point of 95 ℃, and the normal alkane content is 94.3 wt%.
Preheating Fischer-Tropsch synthesis refined wax in a raw material tank to 120 ℃, feeding the Fischer-Tropsch synthesis refined wax into a three-stage cascade evaporator (a first-stage evaporator is a thin-film evaporator, and a second-stage evaporator and a third-stage evaporator are short-range evaporators) at a feeding rate of 9kg/h, wherein the temperature of the first-stage evaporator is 190 ℃ and the pressure of 100Pa to obtain a fraction of less than 400 ℃, a fraction section of more than 400 ℃ enters a second-stage evaporator at an operating temperature of 220 ℃ and an operating pressure of 10Pa to evaporate a 400-plus-490 fraction section, a fraction section of more than 490 ℃ enters a third-stage evaporator at an operating temperature of 300 ℃ and an operating pressure of 1Pa to evaporate a 490-plus-fraction section, a fraction section of more than 630 ℃ serves as a target fraction, carrying out clay refining, adding clay in an amount which is 3% of the raw material, stirring and decolorizing for 0.5h, filtering the clay to obtain a wax primary product for the, the working temperature is-75 ℃, and the Fischer-Tropsch micronized wax for the high-temperature printing ink is obtained.
The product indexes are as follows:
Figure BDA0001873788180000041
Figure BDA0001873788180000051
example 2
Taking Fischer-Tropsch synthesis intermediate wax obtained by another Fischer-Tropsch synthesis process as a raw material, and firstly carrying out hydrofining to obtain the Fischer-Tropsch synthesis refined wax, wherein the hydrogenation temperature is 270 ℃, the operation pressure is 5Mpa, the Fischer-Tropsch refined wax has a melting point of 95 ℃ and the normal hydrocarbon content is 92.7 wt%.
Vacuum rectifying the Fischer-Tropsch synthesis refined wax, wherein the pressure of a rectifying tower is 1000Pa, the operation temperature of the tower top is 210-. Firstly, primarily crushing to 150 meshes, and crushing to 1000 meshes in a low-temperature freezing crusher at the working temperature of-50 ℃ to obtain the Fischer-Tropsch micronized wax for the high-temperature ink.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are only exemplary embodiments of the present invention and are not intended to limit the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (10)

1. A method for preparing wax for high-temperature ink is characterized by comprising the following steps:
carrying out hydrofining on the Fischer-Tropsch synthesis intermediate wax to obtain Fischer-Tropsch synthesis refined wax;
separating the Fischer-Tropsch synthesis refined wax, sequentially separating soft wax, medium hard wax and hard wax, and taking the finally obtained fraction as the ultra hard wax as the target fraction;
and refining the target fraction, and then carrying out micronization process treatment to obtain the micronized wax for the high-temperature ink.
2. The preparation method of claim 1, wherein the Fischer-Tropsch synthesis intermediate wax has a dropping melting point of more than 90 ℃ and a normal paraffin content of more than 90 wt%.
3. The production method according to claim 1, wherein the hydrorefining is carried out at an operating temperature of 220 ℃ to 300 ℃ and an operating pressure of 2 to 10 MPa.
4. The production method according to claim 1, wherein the separation is two-stage or three-stage separation.
5. The preparation method as claimed in claim 4, wherein the separation is a three-stage separation, wherein the first stage separation is operated at a pressure of 1-1000Pa and at a temperature of 100 ℃ and 200 ℃ for separating the soft wax having a melting point of 40 ± 5 ℃; the operation pressure of the second-stage separation is 0-100Pa, the operation temperature is 170-260 ℃ and is used for separating the medium-hard wax with the melting point of 70 +/-5 ℃, the operation pressure of the third-stage separation is 0-10Pa, the operation temperature is 270-320 ℃ and is used for separating the hard wax with the melting point of 90 +/-5 ℃.
6. The production method according to claim 5, wherein the first stage separation uses a vacuum distillation column or a thin film evaporator, and the second stage separation and the third stage separation use a short path evaporator.
7. The method of claim 1, wherein the ultra hard wax has a melt drop point of greater than 110 ℃ and an end point of greater than 550 ℃.
8. The production method according to claim 1, wherein the target fraction is purified by one or more methods selected from the group consisting of hydrorefining, clay refining, and diatomaceous earth refining.
9. The preparation method according to claim 1, wherein the micronization process comprises: the refined target fraction is firstly crushed to 200 meshes of 100-.
10. A wax for high temperature ink prepared by the preparation method according to any one of claims 1 to 9.
CN201811390218.7A 2018-11-21 2018-11-21 Wax for high-temperature printing ink and preparation method thereof Pending CN111205889A (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114106880A (en) * 2021-11-27 2022-03-01 浙江皇星化工股份有限公司 Production method of organic high-temperature alkane material

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CN106554823A (en) * 2015-09-29 2017-04-05 亚申科技研发中心(上海)有限公司 A kind of method that use Fischer-Tropsch waxy stone produces advanced wax
CN108219842A (en) * 2018-01-30 2018-06-29 公安县瑞凯高分子材料股份有限公司 Amide waxe is modified micronizing Fischer-Tropsch wax and its preparation method and application

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CN104673383A (en) * 2015-03-03 2015-06-03 上海兖矿能源科技研发有限公司 Method for producing high-melting-point wax through fischer-tropsch synthesis product
CN106554823A (en) * 2015-09-29 2017-04-05 亚申科技研发中心(上海)有限公司 A kind of method that use Fischer-Tropsch waxy stone produces advanced wax
CN108219842A (en) * 2018-01-30 2018-06-29 公安县瑞凯高分子材料股份有限公司 Amide waxe is modified micronizing Fischer-Tropsch wax and its preparation method and application

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CN114106880A (en) * 2021-11-27 2022-03-01 浙江皇星化工股份有限公司 Production method of organic high-temperature alkane material

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