CN109988652A - Pitch synergy wax and preparation method thereof - Google Patents

Pitch synergy wax and preparation method thereof Download PDF

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Publication number
CN109988652A
CN109988652A CN201711498282.2A CN201711498282A CN109988652A CN 109988652 A CN109988652 A CN 109988652A CN 201711498282 A CN201711498282 A CN 201711498282A CN 109988652 A CN109988652 A CN 109988652A
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China
Prior art keywords
short
wax
oiling
path distillation
pitch
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CN201711498282.2A
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Chinese (zh)
Inventor
李俊诚
潘金亮
苗恒
郑会月
郭良兰
葛建林
周岩
林强
马国清
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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 CN201711498282.2A priority Critical patent/CN109988652A/en
Publication of CN109988652A publication Critical patent/CN109988652A/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
    • C10G73/00Recovery or refining of mineral waxes, e.g. montan wax
    • C10G73/42Refining of petroleum waxes
    • 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
    • C10G73/00Recovery or refining of mineral waxes, e.g. montan wax
    • C10G73/42Refining of petroleum waxes
    • C10G73/44Refining of petroleum waxes in the presence of hydrogen or hydrogen-generating compounds
    • 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

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  • Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)

Abstract

A kind of pitch synergy wax and preparation method thereof, the pitch synergy wax are that successively hydrogenated purification, de-oiling and n grade short-path distillations cut resulting heavy distillat by Fischer Tropsch waxes, and n >=2, the fusing point of the heavy distillat is greater than 100 DEG C.Preparation method of the invention is using first hydrofinishing, de-oiling, the mode of short-path distillation separation afterwards, it avoids to high-melting-point fraction section (fusing point the is greater than 100 DEG C) situation that later period de-oiling is complicated for operation, de-oiling effect is undesirable, fraction section of the fusing point obtained greater than 100 DEG C can be directly used as pitch synergy wax product, have the characteristics that simple production process, properties of product are excellent.

Description

Pitch synergy wax and preparation method thereof
Technical field
The present invention relates to asphalt modifier technical fields more particularly to a kind of pitch synergy wax and preparation method thereof.
Background technique
For protection environment, energy saving, the middle and later periods the 1990s Europe and the countries such as U.S. carried out warm mix drip The research of green mixture, the purpose is to by reduce asphalt mix and stir and paving material, reach reduction asphalt Energy consumption in production process reduces pernicious gas and dust discharge amount, while guaranteeing that Warm-Mix Bitumen Mixture has and mixing drip with heat The essentially identical pavement performance of green mixture and construction workability.Pitch synergy wax is one kind under stirring, meeting and pitch Base forms homogeneous phase solution, and significantly reduces asphalt viscosity, so that it is dedicated to reduce the mix of asphaltic products and operation temperature Wax is one of the main study subject in Warm-Mix Bitumen Mixture.
Fischer Tropsch waxes are a kind of methylene based polyalcohols, are to utilize synthesis gas under medium temperature and medium pressure through catalytic polymerization Obtained alkanes mixture is mainly made of relative molecular mass in 500~1000 straight chain, the High-carbon alkane of saturation.Its Carbon number distribution is wide, and highest carbon number is often up to 100 or more, while its composition is relatively easy, and positive structure linear paraffin content is reachable 90% or more, remaining is essentially branched paraffin, is substantially free of cyclic hydrocarbon and aromatic hydrocarbons.Since Fischer Tropsch waxes have fine crystalline substance Body structure, makes it have that fusing point height, melting range narrow range, oil content is low, needle penetration is low, mobility is low and low-down melting The features such as viscosity, stability is high and hard, wear-resisting.This is exactly the advantage that Fischer Tropsch waxes are used as production pitch synergy wax.But take Synthetic wax carbon number distribution wider range is held in the palm, being directly used as pitch synergy wax influences product softening point, contains a small amount of isomery simultaneously Alkane influences the needle penetration of product.At present generally by Fischer Tropsch waxes and other modifying agent compositing formulas in asphalt It uses, is also rarely reported and Fischer Tropsch waxes are refined, modified are used as pitch synergy wax.
Summary of the invention
In view of this, the main purpose of the present invention is to provide a kind of pitch synergy waxes and preparation method thereof, at least Partly solve at least one of above-mentioned the technical issues of referring to.
To achieve the above object, technical scheme is as follows:
As one aspect of the present invention, a kind of pitch synergy wax is provided, for by Fischer Tropsch waxes successively hydrogenated essence System, de-oiling and n grades of short-path distillations cut resulting heavy distillat, wherein n >=2, and the fusing point of the heavy distillat is greater than 100 DEG C.
As another aspect of the present invention, a kind of preparation method of pitch synergy wax is provided, comprising:
Step 1: Fischer Tropsch waxes hydrofinishing is obtained into Fischer-Tropsch purification wax;
Step 2: Fischer-Tropsch purification wax deoiling is obtained into de-oiling Fischer-Tropsch purification wax;
Step 3: de-oiling Fischer-Tropsch purification wax through n grades of short-path distillations is cut to obtain 600 DEG C of boiling point > under normal pressure of weight Fraction, wherein n >=2, using the heavy distillat as pitch synergy wax.
Based on the above-mentioned technical proposal, the beneficial effects of the present invention are:
1, Fischer Tropsch waxes are sufficiently pre-processed with (including hydrofinishing and de-oiling operation), subsequent fraction can be reduced Section is processed into the operating cost of product, avoids the occurrence of the case where heavy distillat is difficult to de-oiling, and the quality of target product can be improved.
2, gained fraction can be produced directly as pitch synergy wax after sufficiently pretreated de-oiling Fischer-Tropsch purification wax separation Product, without re-refining modification.
3, the whole simple production process of pitch synergy wax, operating flexibility is high, can be suitable according to the actual conditions of target product When increase and decrease process and change operating condition, develops the pitch synergy wax that freezing point is high, needle penetration is low, performance is stable, at low cost Product.
Specific embodiment
To make the objectives, technical solutions, and advantages of the present invention clearer, below in conjunction with specific embodiment, to this Invention is described in further detail.
The present invention provides a kind of pitch synergy wax and preparation method thereof, Fischer Tropsch waxes are successively passed through hydrofinishing and After deoiling treatment, de-oiling Fischer-Tropsch purification wax is obtained, then to its short-path distillation accurate cutting, fusing point is greater than 100 DEG C of fraction section It can be directly used as pitch synergy wax product, have the characteristics that simple production process, properties of product are excellent.
Wherein, the term " Fischer Tropsch waxes " in the present invention refers to using coal as raw material, through gasification obtain synthesis gas (CO and H2) the alkanes mixture that is obtained under certain temperature and pressure through catalytic polymerization;Term " pitch synergy wax " is that one kind exists Under stirring, can and asphaltic base form homogeneous phase solution, and significantly reduce asphalt viscosity, thus make the mix of asphaltic products with The Wax special that operation temperature reduces.
Specifically, pitch synergy wax of the invention, for by Fischer Tropsch waxes successively hydrogenated purification, de-oiling and n grades short Resulting heavy distillat is cut in journey distillation, wherein n >=2, and the fusing point of the heavy distillat is greater than 100 DEG C.
Wherein, can effectively remove alkene and oxygenatedchemicals etc. in Fischer-Tropsch wax by hydrofinishing influences product stability And the component of product quality, isoparaffin can be removed by de-oiling, using first carry out hydrofinishing, de-oiling the step of, rear short distance Isolated mode is distilled, de-oiling effect complicated for operation to high-melting-point fraction section (fusing point is greater than 100 DEG C) later period de-oiling is avoided Undesirable situation.
In some embodiments, the operation temperature of hydrofinishing is 250~350 DEG C, and operating pressure is 5~10Mpa.
In some embodiments, de-oiling mode is sweating de-oiling or solvent deoiling, and sweating de-oiling and solvent deoiling are this Routine techniques in technical field, and it is unrelated with creativeness of the invention, therefore its concrete operation step is not repeated at this.
In some embodiments, the step of n grades of short-path distillation cutting includes: to make to go out when prime short-path distillation is separated Heavy distillat enter in next stage short-path distillation and further separate, finally obtain 600 DEG C of boiling point > under normal pressure of fraction section.
Wherein, the n grades of short-path distillation is preferably 2 grades of short-path distillations or 3 grades of short-path distillations, to simplify production technology.
A kind of preparation method of pitch synergy wax of the present invention, specifically includes the following steps:
Step 1: Fischer Tropsch waxes hydrofinishing is obtained into Fischer-Tropsch purification wax;
Step 2: Fischer-Tropsch purification wax deoiling is obtained into de-oiling Fischer-Tropsch purification wax;
Step 3: de-oiling Fischer-Tropsch purification wax through n grades of short-path distillations is cut to obtain 600 DEG C of boiling point > under normal pressure of weight Fraction, wherein n >=2, using the heavy distillat as pitch synergy wax.
In some embodiments, the operation temperature of the hydrofinishing in step 1 be 250~350 DEG C, operating pressure be 5~ 10Mpa。
In some embodiments, the mode of the de-oiling in step 2 is sweating de-oiling or solvent deoiling.In some embodiments In, the step of n grades of short-path distillation includes:
Sub-step 1: de-oiling Fischer-Tropsch purification wax is preheated to 100~150 DEG C;
Sub-step 2: it is that 1~10kg/h enters in molecule evaporator with feed rate, improves temperature and/or vacuum step by step Degree enters the heavy distillat gone out when prime short-path distillation is separated in next stage short-path distillation and further separates, finally obtains often The heavy distillat of 600 DEG C of boiling point > of pressure.
In some embodiments, the n grades of short-path distillation is 2 grades of short-path distillations, and sub-step 2 specifically includes:
Sub-step 2a: first order short-path distillation is carried out, at 100~200 DEG C, 10~100pa to cut off light fraction;
Sub-step 2b: heavy distillat obtained by sub-step 2a is subjected to the steaming of second level short distance in 300~350 DEG C, 0.1~1pa It evaporates, obtains 600 DEG C of > of heavy distillat.
In some embodiments, the n grades of short-path distillation be 3 grades of short-path distillations, sub-step 2 specifically includes the following steps:
Sub-step 2a ': first order short-path distillation is carried out, at 100~200 DEG C, 10~100pa to cut off light fraction;
Sub-step 2b ': heavy distillat obtained by sub-step 2a ' is subjected to the steaming of second level short distance in 270~300 DEG C, 0.1~1pa It evaporates;
Sub-step 2c ': heavy distillat obtained by sub-step 2b ' is subjected to the steaming of third level short distance in 300~330 DEG C, 0.1~1pa It evaporates, obtains 600 DEG C of > of heavy distillat.
It is exemplified below specific embodiment, to be further explained explanation to technical solution of the present invention.In following embodiments Reagent, material used etc., are commercially available unless otherwise specified.
Embodiment 1
The Fischer Tropsch waxes obtained using fischer-tropsch synthesis process are hydrogenated first to be refining to obtain Fischer-Tropsch purification wax as raw material, add Hydrogen temperature is 300 DEG C, operating pressure 6Mpa, then sweating de-oiling operation is carried out to it, obtains de-oiling Fischer-Tropsch purification wax.
De-oiling Fischer-Tropsch purification wax is preheating to 120 DEG C in head tank, is that 9kg/h enters the first molecule with feed rate In evaporator carry out first order short-path distillation, control 195 DEG C of temperature, pressure 35pa, cut off 400 DEG C of components of <, remaining ingredient into Enter progress second level short-path distillation in the second molecule evaporator, controlled at 280 DEG C, pressure 0.3pa obtains 400~580 DEG C and 580 DEG C of fraction sections of >.Using 580 DEG C of fraction sections of > as raw material, third level short-path distillation is carried out, 310 DEG C of operation temperature, is grasped Make pressure 0.3Pa, evaporate 580~630 DEG C of fraction sections, 630 DEG C of fraction sections of remaining > can be used as pitch synergy wax product. Product index is as shown in table 1 below:
Table 1
Embodiment 2
The Fischer Tropsch waxes obtained using fischer-tropsch synthesis process are hydrogenated first to be refining to obtain Fischer-Tropsch purification wax as raw material, add Hydrogen temperature is 290 DEG C, operating pressure 8Mpa, then sweating de-oiling operation is carried out to it, obtains de-oiling Fischer-Tropsch purification wax.
De-oiling Fischer-Tropsch purification wax is preheating to 120 DEG C in head tank, is that 6kg/h enters the first molecule with feed rate In evaporator carry out first order short-path distillation, control 200 DEG C of temperature, pressure 45pa, cut off 400 DEG C of components of <, remaining ingredient into Enter in the second molecule evaporator progress second level short-path distillation, controlled at 330 DEG C, pressure 0.5pa, evaporate 400~ 630 DEG C of fraction sections, 630 DEG C of fraction sections of remaining > can be used as pitch synergy wax product.Product index is as shown in table 2 below:
Table 2
Analysis project 630 DEG C of fraction section indexs of > 400-630 DEG C of fraction section index
Freezing point DEG C ≥100 76-80
Oil content (m/m) % ≤0.5 ≤1.5
Color (range estimation) Canescence is faint yellow White
25 DEG C of needle penetration@, 1/10mm ≤1 ≤12
135 DEG C of viscosity@, mm2/s 10-14 4-7
Pitch synergy wax obtained by above-mentioned two embodiment can form homogeneous phase solution with asphaltic base under stirring, and show Writing reduces asphalt viscosity.This can make the mix of asphaltic products and operation temperature reduce by 10~30 DEG C.If reasonably optimizing mix is set It is standby with technique of paving the way, higher temperature can be reduced.The reduction of mix and operation temperature will be greatly reduced CO in operating process2Row It puts, also reduces energy consumption.In pitch cooling procedure, the pitch synergy wax can crystallize precipitation and formed network-like structure to Increase the stability of pitch.
Particular embodiments described above has carried out further in detail the purpose of the present invention, technical scheme and beneficial effects Describe in detail bright, it should be understood that the above is only a specific embodiment of the present invention, is not intended to restrict the invention, it is all Within the spirit and principles in the present invention, any modification, equivalent substitution, improvement and etc. done should be included in protection of the invention Within the scope of.

Claims (10)

1. a kind of pitch synergy wax, for obtained by Fischer Tropsch waxes successively hydrogenated purification, de-oiling and n grades of short-path distillation cuttings Heavy distillat, the fusing point of wherein n >=2, the heavy distillat is greater than 100 DEG C.
2. pitch synergy wax according to claim 1, which is characterized in that the step of n grades of short-path distillation includes: to make to work as The separated heavy distillat out of prime short-path distillation, which enters in next stage short-path distillation, further to be separated, and boiling point under normal pressure is finally obtained The fraction section that 600 DEG C of >.
3. pitch synergy wax according to claim 1, which is characterized in that the operation temperature of the hydrofinishing be 250~ 350 DEG C, operating pressure is 5~10Mpa.
4. pitch synergy wax according to claim 1, which is characterized in that the mode of the de-oiling is sweating de-oiling or solvent De-oiling.
5. a kind of preparation method of pitch synergy wax, comprising the following steps:
Step 1: Fischer Tropsch waxes hydrofinishing is obtained into Fischer-Tropsch purification wax;
Step 2: Fischer-Tropsch purification wax deoiling is obtained into de-oiling Fischer-Tropsch purification wax;
Step 3: de-oiling Fischer-Tropsch purification wax through n grades of short-path distillations is cut to obtain 600 DEG C of boiling point > under normal pressure of heavy distillat, Wherein n >=2, using the heavy distillat as pitch synergy wax.
6. preparation method according to claim 5, which is characterized in that in step 1, the operation temperature of the hydrofinishing is 250~350 DEG C, operating pressure is 5~10Mpa.
7. preparation method according to claim 5, which is characterized in that in step 2, the mode of the de-oiling is sweating de-oiling Or solvent deoiling.
8. preparation method according to claim 5, which is characterized in that the step of n grades of short-path distillation includes:
Sub-step 1: de-oiling Fischer-Tropsch purification wax is preheated to 100~150 DEG C;
Sub-step 2: it is that 1~10kg/h enters in molecule evaporator with feed rate, improves temperature and/or vacuum degree step by step, make The heavy distillat gone out when prime short-path distillation is separated, which enters in next stage short-path distillation, further to be separated, and is finally obtained and is boiled under normal pressure The heavy distillat of 600 DEG C of point >.
9. preparation method according to claim 8, which is characterized in that the n grades of short-path distillation is 2 grades of short-path distillations, son Step 2 specifically includes:
Sub-step 2a: first order short-path distillation is carried out, at 100~200 DEG C, 10~100pa to cut off light fraction;
Sub-step 2b: heavy distillat obtained by sub-step 2a is subjected to second level short-path distillation in 300~350 DEG C, 0.1~1pa, is obtained The heavy distillat that 600 DEG C of >.
10. preparation method according to claim 8, which is characterized in that the n grades of short-path distillation is 3 grades of short-path distillations, son Step 2 specifically includes:
Sub-step 2a ': first order short-path distillation is carried out, at 100~200 DEG C, 10~100pa to cut off light fraction;
Sub-step 2b ': heavy distillat obtained by sub-step 2a ' is subjected to second level short-path distillation in 270~300 DEG C, 0.1~1pa;
Sub-step 2c ': heavy distillat obtained by sub-step 2b ' is subjected to third level short-path distillation in 300~330 DEG C, 0.1~1pa, is obtained To 600 DEG C of heavy distillat of >.
CN201711498282.2A 2017-12-29 2017-12-29 Pitch synergy wax and preparation method thereof Pending CN109988652A (en)

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Cited By (1)

* 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

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102061098A (en) * 2010-11-25 2011-05-18 重庆鹏方路面工程技术研究院有限公司 Asphalt mixture warm-mixing modifier and preparation method thereof
CN103554926A (en) * 2013-10-16 2014-02-05 中国石油化工股份有限公司 Low-strength and high-grade road asphalt and preparation method thereof
CN105542856A (en) * 2015-12-31 2016-05-04 中科合成油技术有限公司 Method for processingFischer-Tropsch wax production series products
CN106633944A (en) * 2015-11-02 2017-05-10 中国石油化工股份有限公司 Asphalt warm mixing agent as well as preparation method and application thereof
CN107513278A (en) * 2016-06-17 2017-12-26 中国石油化工股份有限公司 Warm mix modified pitch, contain its compound and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102061098A (en) * 2010-11-25 2011-05-18 重庆鹏方路面工程技术研究院有限公司 Asphalt mixture warm-mixing modifier and preparation method thereof
CN103554926A (en) * 2013-10-16 2014-02-05 中国石油化工股份有限公司 Low-strength and high-grade road asphalt and preparation method thereof
CN106633944A (en) * 2015-11-02 2017-05-10 中国石油化工股份有限公司 Asphalt warm mixing agent as well as preparation method and application thereof
CN105542856A (en) * 2015-12-31 2016-05-04 中科合成油技术有限公司 Method for processingFischer-Tropsch wax production series products
CN107513278A (en) * 2016-06-17 2017-12-26 中国石油化工股份有限公司 Warm mix modified pitch, contain its compound and preparation method thereof

Cited By (1)

* 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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Application publication date: 20190709