CN106010631B - A kind of method for refining solvent of rubber plastizing agent - Google Patents
A kind of method for refining solvent of rubber plastizing agent Download PDFInfo
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- CN106010631B CN106010631B CN201610347927.1A CN201610347927A CN106010631B CN 106010631 B CN106010631 B CN 106010631B CN 201610347927 A CN201610347927 A CN 201610347927A CN 106010631 B CN106010631 B CN 106010631B
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING 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
- C10G21/00—Refining of hydrocarbon oils, in the absence of hydrogen, by extraction with selective solvents
- C10G21/06—Refining of hydrocarbon oils, in the absence of hydrogen, by extraction with selective solvents characterised by the solvent used
- C10G21/12—Organic compounds only
- C10G21/20—Nitrogen-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L21/00—Compositions of unspecified rubbers
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING 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
- C10G21/00—Refining of hydrocarbon oils, in the absence of hydrogen, by extraction with selective solvents
- C10G21/06—Refining of hydrocarbon oils, in the absence of hydrogen, by extraction with selective solvents characterised by the solvent used
- C10G21/12—Organic compounds only
- C10G21/16—Oxygen-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING 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
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/10—Feedstock materials
- C10G2300/1074—Vacuum distillates
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- Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The invention discloses a kind of method for refining solvent of rubber plastizing agent.The method for refining solvent comprises the following steps：Vacuum distillate and solvent enter the extraction tower from the upper and lower part of extraction tower respectively, the vacuum distillate and the solvent carry out solvent refining in the extraction tower by counter current contacting, tapped oil is obtained after the bottom of towe of the extraction tower obtains Extract, recycling design；The part of the tapped oil is used as circulation tapped oil, the circulation tapped oil obtains feedstock oil after being mixed with the vacuum distillate, the feedstock oil enters the extraction tower from the bottom of the extraction tower, solvent refining is carried out by counter current contacting with the solvent that enters from the top of the extraction tower, refined liquid is obtained in the tower top of the extraction tower, recovered solvent obtains refined oil, as described rubber plastizing agent.The present invention is higher due to having carried out the circulation of aromatic hydrocarbons tapped oil, arene content, the operating condition in production process is more easy to realization, the product quality of acquisition improves.
Description
Technical field
The present invention relates to a kind of method for refining solvent of rubber plastizing agent, belong to PETROLEUM PROCESSING field.
Background technology
In the last few years, some effects were achieved in terms of the exploitation of various environment-friendly rubber plasticizer both at home and abroad, but with routine
Method for refining solvent production environment-friendly rubber plasticizer product arene content can be caused low, it is impossible to meet use requirement, therefore, grind
The person of studying carefully is improved Conventional solvents process for purification, also occurs in that many patent reports.Such as Chinese patent
200810224694.1 and Chinese patent 200810224695.6 disclose based on the secondary extraction process of solvent in high yield
Low condensed-nuclei aromatics content rubber plastizing agent manufacture method, but this method production cycle is longer, product yield is relatively low；Chinese patent
CN102140369A discloses a kind of method that back suction extraction solvent improvement aromatics seperation effect is added in refined main solvent, although
Effect is achieved, but little is improved to product yield, and has certain influence to the production of other lube products；Have with depressurize
Residual oil is raw material, and qualified environment-friendly rubber plasticizer is obtained using solvent deasphalting-solvent make-up purification techniques, but the product is deposited
It is too high in viscosity, it is inconvenient for use, and contain asphalitine, defined IP346 detection methods are not applied to, exists in the feature of environmental protection and strives
View.Accordingly, it is desirable to provide a kind of improved rubber plastizing agent solvent refining new technology for raw material with more preferable adaptability.
The content of the invention
Have it is an object of the invention to provide a kind of method for refining solvent of rubber plastizing agent there is provided one kind for raw material
The improved rubber plastizing agent solvent refining new technology of more preferable adaptability, can be carried while the quality of production suitable product
High product yield, with good application prospect.
The method for refining solvent of rubber plastizing agent provided by the present invention, comprises the following steps：
Vacuum distillate and solvent enter the extraction tower, the vacuum distillate from the upper and lower part of extraction tower respectively
Solvent refining is carried out by counter current contacting in the extraction tower with the solvent, extracted out in the bottom of towe of the extraction tower
Tapped oil is obtained after liquid, recycling design；The part of the tapped oil subtracts as circulation tapped oil, the circulation tapped oil with described
Feedstock oil is obtained after pressure distillate mixing, the feedstock oil enters the extraction tower from the bottom of the extraction tower, and from described
The solvent that the top of extraction tower enters carries out solvent refining by counter current contacting, is refined in the tower top of the extraction tower
Liquid, recovered solvent obtains refined oil, as described rubber plastizing agent.
The method for refining solvent that the present invention is provided, it is described that the part tapped oil and the vacuum distillate are mixed to get
Feedstock oil inversely contacts extraction into the extraction tower with the solvent, and this process is constantly circulated.When circulation reaches certain time
Afterwards, obtain extracting tower top refined liquid, it is the low condensed-nuclei aromatics content rubber of target product-in high yield that this refined liquid, which is removed after solvent,
Plasticizer；The outer part aromatic hydrocarbons tapped oil got rid of can be used as the normal aromatic hydrocarbon tapped oil of the non-environmental protection of high arene content simultaneously.
Most of polycyclic aromatic hydrocarbon in said process removing vacuum distillate, while reducing the loss of low condensed-nuclei aromatics content.
In above-mentioned method for refining solvent, the physical and chemical parameter of the rubber plastizing agent is as follows：
Aniline point is less than 90 DEG C；
CA(aromatic carbon rate) value is higher than 10%, the C for the rubber plastizing agent that 1-5 of the embodiment of the present invention is preparedAValue is respectively
14.5%th, 12.5%, 16.7%, 26.0% and 13.1%；
Benzo [a] pyrene (BaP) content is less than 1mg/kg, the BaP for the rubber plastizing agent that 1-5 of the embodiment of the present invention is prepared
Content is respectively 0.8mg/kg, do not detect, 0.6mg/kg, 0.7mg/kg and do not detected；
Polycyclic aromatic hydrocarbon (aromatic hydrocarbons more than PCA, two rings and two rings) content is not more than 3%, and 1-5 of the embodiment of the present invention is prepared into
To the polycyclic aromatic hydrocarbon content of rubber plastizing agent be respectively 2.21%, 2.59%, 2.37%, 2.25% and 2.41%；
Carcinogenic Polycyclic Aromatic Hydrocarbons (PAHs) total content is less than 10mg/kg, and the rubber that 1-5 of the embodiment of the present invention is prepared increases
The PAHs contents for moulding agent are respectively 3.9mg/kg, 4.2mg/kg, 4.5mg/kg, 4.9mg/kg and 6.7mg/kg；The carcinogenicity
Polycyclic aromatic hydrocarbon be benzo [a] pyrene, benzo [e] pyrene, benzo [a] anthracene, bend, benzo [b] fluoranthene, benzo [j] fluoranthene, benzo [k] it is glimmering
Anthracene, hexichol [a, h] and anthracene, meet indices requirement of the EU REACH Legislation on tyre rubber plasticizer, and raw material comes
Source is sufficient.
In above-mentioned method for refining solvent, the vacuum distillate is common process hydrofinishing in petroleum refining industry, molten
The vacuum distillate obtained after agent industrial common one or several kinds of pretreating process processing such as refined, clay-filtered；
100 DEG C of kinematic viscosity ranges of the vacuum distillate can be 6mm2/ s~30mm2/ s, concretely 6mm2/ s~
10mm2/s、15mm2/ s~24mm2/ s or 24mm2/ s~30mm2/s；
The vacuum distillate is Light lube oil, the line distillate that subtracts three and at least one of the line distillate that subtracts four.
In above-mentioned method for refining solvent, the condition of the solvent refining is as follows：
It is described extracting column overhead temperature can be 60~100 DEG C, concretely 60~90 DEG C, 60~80 DEG C, 80~90 DEG C,
80~100 DEG C, 60 DEG C, 80 DEG C, 90 DEG C or 100 DEG C；
The temperature of the extraction tower bottom of towe can be 40~80 DEG C, 40~60 DEG C, 40~50 DEG C, 50~80 DEG C, 50~60 DEG C,
40 DEG C, 50 DEG C, 60 DEG C or 80 DEG C；
In the feedstock oil, the mass ratio of the vacuum distillate and the circulation tapped oil can be 1~5：1；
The charge-mass ratio of the solvent and the feedstock oil can be 0.8~2：1, concretely 0.8~1.6：1st, 0.8~
1.5：1st, 0.8~1.2：1st, 1.2~2：1st, 1.5~2：1st, 1.6~2：1、0.8：1、1.2：1、1.5：1、1.6：1 or 2：1.
In above-mentioned method for refining solvent, the solvent can be at least one of furfural, 1-METHYLPYRROLIDONE and phenol.
In above-mentioned method for refining solvent, the mode that the circulation tapped oil is mixed with the vacuum distillate is Mixer pot
Reconcile and mix, stir mixing or static mixer mixing.
The inventive method comes into operation initial stage due to the limits throughput of the tapped oil, causes the circulation tapped oil can not be with institute
Vacuum distillate formation suitable proportion is stated, balance is realized as early as possible for guarantee system, other raw materials rich in aromatic hydrocarbons can be used to replace
Generation.It is a kind of mixed chemical material rich in aromatic component as the raw material of substitute, including but not limited to solvent refining, catalysis
Cracking, visbreaking, thermal cracking such as are hydrocracked at the aromatic naphtha rich in aromatic hydrocarbons that technique is obtained.
The method for refining solvent of rubber plastizing agent of the present invention has the following advantages that：
1st, control boiling range to cut appropriate fractions by vacuum distillation and obtain vacuum distillate, vacuum distillate passes through or not
It is refined by pretreatment, then through solvent extraction, during solvent extraction is refined gained aromatic hydrocarbons tapped oil part as raw material not
Disconnected circulation, makes the essential oil obtained after stable circulation be enriched with mononuclear aromatics and cycloalkane, removes most of Carcinogenic Polycyclic Aromatic Hydrocarbons, most
Finished product also obtain higher aromatic carbon rate while meeting environmental requirement, so as to obtain a kind of rubber of low condensed-nuclei aromatics content
Glue plasticizer, and with higher yield.
2nd, gained aromatic hydrocarbons tapped oil part is constantly recycled into extracting as raw material during being refined due to solvent extraction
Tower so that the actual production of aromatic hydrocarbons tapped oil is greatly decreased in extraction tower, the yield of refined oil significantly increases, that is, the target obtained
The yield of the low condensed-nuclei aromatics content environment-friendly rubber plasticizer of product is greatly improved.Relative to the method for the secondary extracting of solvent, this hair
It is bright that there is extremely obvious yield advantage；Relative to a traditional extraction process, the present invention is due to having carried out aromatic hydrocarbons tapped oil
Circulation, arene content is higher, the operating condition in production process is more easy to realization, and the product quality of acquisition has certain carry
It is high.
Brief description of the drawings
Fig. 1 is the flow chart of the method for refining solvent of rubber plastizing agent of the present invention.
Embodiment
Experimental method used in following embodiments is conventional method unless otherwise specified.
Material, reagent used etc., unless otherwise specified, are commercially obtained in following embodiments.
The following embodiments of the present invention and the raw materials used property of comparative example are as shown in table 1.
Following embodiment 1-5 carry out solvent refining according to the flow shown in Fig. 1：It is heated to the vacuum distillate of certain temperature
Enter extraction tower from the upper and lower part of extraction tower respectively with solvent, vacuum distillate and solvent are connect in extraction tower by adverse current
Touch and carry out solvent refining, tapped oil is obtained after the bottom of towe of extraction tower obtains Extract, recycling design；The part conduct of tapped oil
Tapped oil is circulated, circulation tapped oil obtains feedstock oil after being mixed with vacuum distillate, feedstock oil enters from the bottom of extraction tower to be taken out
Stripper, passes through counter current contacting with the solvent that enters from the top of extraction tower and carries out solvent refining, constantly circulation, in the tower of extraction tower
Top obtains refined liquid, and recovered solvent obtains refined oil, produces low condensed-nuclei aromatics content rubber plastizing agent in high yield.
Specific embodiment is as follows, and wherein result of the test is as shown in table 1.
Embodiment 1,
Using Light lube oil as raw material, 100 DEG C of kinematic viscosity of Con trolling index are 6~10mm2/s；This Light lube oil
Extracting tower top refined liquid is refining to obtain through solvent refining unit extraction tower, this refined liquid obtains refined oil after solvent recovery,
Wherein solvent refining temperature is：Tower top temperature is 60 DEG C, and column bottom temperature is 40 DEG C, oil ratio 0.8：1, distillate feedstock is with circulating
Aromatic hydrocarbons tapped oil mass ratio 3：1.
Embodiment 2,
Using the line distillate that subtracts three as raw material, 100 DEG C of kinematic viscosity of Con trolling index are 15~24mm2/s；This subtracts three line cut
Oil is refining to obtain extracting tower top refined liquid through extraction tower, and this refined liquid obtains refined oil, wherein solvent essence after solvent recovery
Temperature processed is：Tower top temperature is 80 DEG C, and column bottom temperature is 50 DEG C, oil ratio 1.2：1, distillate feedstock is with circulating aromatic hydrocarbons tapped oil
Mass ratio 4：1.
Embodiment 3,
With the line distillate that subtracts three, 100 DEG C of kinematic viscosity of Con trolling index are 15~24mm2/s；This subtracts three line distillate is through taking out
Stripper is refining to obtain extracting tower top refined liquid, and this refined liquid obtains refined oil, wherein solvent refining temperature after solvent recovery
For：Tower top temperature is 90 DEG C, and column bottom temperature is 60 DEG C, oil ratio 2.0：1, distillate feedstock is with circulating aromatic hydrocarbons tapped oil mass ratio
3：1.
Embodiment 4,
Using the line distillate that subtracts three as raw material, 100 DEG C of kinematic viscosity of Con trolling index are 15~24mm2/s；This subtracts three line cut
Oil is refining to obtain extracting tower top refined liquid through extraction tower, and this refined liquid obtains refined oil, wherein solvent essence after solvent recovery
Temperature processed is：Tower top temperature is 100 DEG C, and column bottom temperature is 80 DEG C, oil ratio 1.6：1, distillate feedstock is extracted out with circulation aromatic hydrocarbons
Oil quality compares 2：1.
Embodiment 5,
Using the line distillate that subtracts four as raw material, 100 DEG C of kinematic viscosity of Con trolling index are 24~30mm2/s；This subtracts four line cut
Oil is refining to obtain extracting tower top refined liquid through extraction tower, and this refined liquid obtains refined oil, wherein solvent essence after solvent recovery
Temperature processed is：Tower top temperature is 90 DEG C, and column bottom temperature is 60 DEG C, oil ratio 1.5：1, distillate feedstock is with circulating aromatic hydrocarbons tapped oil
Mass ratio 5：1.
Above-described embodiment 1~5 is that the specific implementation of the present invention is showed, and listing embodiment 1~5 in table 1 obtains product
Data (yield is relative to raw material vacuum distillate), comparative example 1 is using the production of furfural treatment twice low condensed ring in high yield
The representative instance (wherein solvent refining condition is same as Example 1) of arene content rubber plastizing agent, comparative example 2 is using tradition
The representative instance for the low condensed-nuclei aromatics content rubber plastizing agent that solvent refining (solvent is furfural) technique is produced by primary purification
(wherein solvent refining condition is same as Example 1).
The embodiment of table 1 is contrasted with comparative example product property
From embodiment 1-5 and comparative example 1 as can be seen that in addition to aniline point is slightly higher, other properties of product be it is suitable, still
The product yield of embodiment is significantly higher than comparative example, and yield generally improves nearly 60%, to the improvement effect of yield clearly,
Embody the advance of this preparation method.It can see from embodiment 1-5 and comparative example 2, product property is suitable, the production of embodiment
Product yield is significantly higher than comparative example, embodies the superiority of this preparation method.
Embodiment 1-5 low condensed-nuclei aromatics content property can be seen that with, second line of distillation, the line cut that subtracts three and subtract four line be
Raw material, can be high by the technique productions aromatic carbon content of the present invention, and PCA is not more than 3%, BaP mass contents less than 1mg/kg, eight
Plant the rubber plastizing agent for meeting EU REACH Legislation requirement that condensed-nuclei aromatics mass content is less than 10mg/kg.
Claims (1)
1. a kind of method for refining solvent of rubber plastizing agent, comprises the following steps：
Vacuum distillate and solvent enter the extraction tower, the vacuum distillate and institute from the bottom and top of extraction tower respectively
State solvent and solvent refining is carried out by counter current contacting in the extraction tower, obtain Extract in the bottom of towe of the extraction tower, return
Tapped oil is obtained after receiving solvent；The part of the tapped oil evaporates as circulation tapped oil, the circulation tapped oil with the decompression
Feedstock oil is obtained after point oil mixing, the feedstock oil enters the extraction tower from the bottom of the extraction tower, and from the extracting
The solvent that the top of tower enters carries out solvent refining by counter current contacting, and refined liquid is obtained in the tower top of the extraction tower,
Recovered solvent obtains refined oil, as described rubber plastizing agent；
The physical and chemical parameter of the rubber plastizing agent is as follows：
Aniline point is less than 90 DEG C；
CAValue is higher than 10%；
Benzo (a) pyrene content is less than 1mg/kg；
Polycyclic aromatic hydrocarbon content is not more than 3%；
Carcinogenic Polycyclic Aromatic Hydrocarbons total content be less than 10mg/kg, the Carcinogenic Polycyclic Aromatic Hydrocarbons be benzo [a] pyrene, benzo [e] pyrene,
Benzo [a] anthracene, in the wrong, benzo [b] fluoranthene, benzo [j] fluoranthene, benzo [k] fluoranthene and hexichol [a, h] and anthracene；
100 DEG C of kinematic viscosity ranges of the vacuum distillate are 6mm2/ s~30mm2/s；
The vacuum distillate is Light lube oil, the line distillate that subtracts three and at least one of the line distillate that subtracts four；
The condition of the solvent refining is as follows：
The temperature of the extracting column overhead is 60~100 DEG C；
The temperature of the extraction tower bottom of towe is 40~80 DEG C；
In the feedstock oil, the vacuum distillate and the mass ratio of the circulation tapped oil are 1~5：1；
The charge-mass ratio of the solvent and the feedstock oil is 0.8~2：1；
The solvent is at least one of furfural, 1-METHYLPYRROLIDONE and phenol；
The mode that the circulation tapped oil is mixed with the vacuum distillate reconciles for Mixer pot to be mixed, stirs mixing or static mixed
Clutch is mixed.
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| CN201962251U (en) * | 2011-03-08 | 2011-09-07 | 中国石油天然气股份有限公司 | Solvent refining equipment for producing environment-friendly rubber filling oil |
| CN102676212B (en) * | 2011-03-08 | 2014-04-02 | 中国石油天然气股份有限公司 | Raw oil optimization method and equipment for improving aromatic hydrocarbon content of environment-friendly rubber filling oil |
| CN103589453B (en) * | 2012-08-14 | 2015-07-29 | 中国石油化工股份有限公司 | A kind of preparation method of aromatic rubber oil |
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