CN102585902B - Environment-friendly rubber oil and preparation method thereof - Google Patents
Environment-friendly rubber oil and preparation method thereof Download PDFInfo
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- CN102585902B CN102585902B CN201210040850.5A CN201210040850A CN102585902B CN 102585902 B CN102585902 B CN 102585902B CN 201210040850 A CN201210040850 A CN 201210040850A CN 102585902 B CN102585902 B CN 102585902B
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Abstract
The invention discloses environment-friendly rubber oil and a preparation method thereof. The preparation method comprises the following steps of: (1) placing naphthenic-base distillate oil in a solvent refining tower to carry out solvent refining to obtain refined liquid at the top of the solvent refining tower and extracted liquid at the bottom of the solvent refining tower, recovering the solvent from the refined liquid to obtain refined oil and receiving the solvent from the extracted liquid to obtain extracted oil; and (2) hydrogenating the extracted oil to obtain hydrogenated oil; and distilling the hydrogenated oil for removing light fraction to obtain the environment-friendly rubber oil. The preparation method has the following beneficial effects: after raw material oil is refined with the solvent, the refined oil has the characteristics of low aromatic hydrocarbon content, high saturated hydrocarbon content and light color and is a high-quality naphthenic-base basic oil with a wide application scope; in addition, the non-environment-friendly extracted oil with low additional value is further subjected to the hydrogenation treatment and then is converted to be the environment-friendly rubber oil with high additional value, thus the integral economic benefits of the naphthenic-base distillate oil are greatly improved.
Description
Technical field
The present invention relates to a kind of environment-friendly rubber oil and preparation method thereof, belong to petrochemical industry.
Background technology
The oil product using in synthetic or Rubber processing process at rubber, is referred to as rubber oil.Rubber oil, as a kind of important auxiliary agent, is widely used in rubber industry.After rubber is oil-filled, processing characteristics and use properties improve, and have increased the output of rubber simultaneously, have reduced cost.China manufactures big country as tire, and tire has become the Application Areas of rubber oil maximum with oil, and domestic tire more than 1/3rd exports abroad.
The cry of environment in recent years protection is more and more higher, and the application of green material is extremely paid attention to, and traditional high aromatic rubber oil is to the harm of human health and the very big attention that the pollution of environment caused to national governments and researchist.European Union's 2005/69/EC instruction is implemented, requires to forbid poisonous rubber oil in tire production comprehensively.
Chinese patent application 200910088932.5 and 200910088931.0 all be take cycloalkyl vacuum distillate as raw material, through twice furfural treatment, obtains environment-friendly rubber oil.Solvent treatment technique belongs to physical process, when obtaining environment-friendly rubber oil, produces the low value-added extraction oil that is rich in a large number polycyclic aromatic hydrocarbons; U.S. Patent application US6110358 be take cycloalkyl distillate as raw material, first through one-stage hydrogenation, processes, and makes part aromatic saturation, distill afterwards, hydrotreatment oil after distillation is proceeded solvent treatment, and tower top refined liquid obtains treated oil after reclaiming solvent, and treated oil is as environment-friendly rubber oil.Adopt after this patented technology, solvent-refined oil yield reaches more than 80%, extracts oily yield out and significantly reduces.Treated oil saturated hydrocarbon content is up to 70% left and right, and aniline point is greater than 80 ℃.Although this technology significantly improves oil yield, environment-friendly rubber oil saturated hydrocarbon content is high, and this causes the consistency variation of environment-friendly rubber oil and rubber.
Prior art, by solvent treatment technique, while producing the rubber oil that meets European Union environmental protection requirement, produces a large amount of low value-added non-environmental protection and extracts oil out.Adopt the first hydrotreatment of stock oil, more solvent-refined technique, although the oily yield of low value-added extraction is significantly reduced, the aromatic hydrocarbons of rubber oil (or aromatic carbon) content is low, poor with the consistency of rubber.
Summary of the invention
The object of this invention is to provide a kind of environment-friendly rubber oil and preparation method thereof, by the combination process of solvent treatment-hydrotreatment, produce aromaticity content high, meet the method for the tyre rubber oil of European Union environmental protection requirement.
For this reason, the preparation method of a kind of environment-friendly rubber oil provided by the present invention, comprises the steps:
(1) cycloalkyl distillate is placed in to solvent treatment tower and carries out solvent treatment, at the tower top of described solvent treatment tower, obtain refined liquid, reclaim after solvent, obtain treated oil, at the bottom of tower, obtain Extract, reclaim after solvent, obtain extracting out oil;
(2) described extraction oil is carried out to hydrotreatment and obtain hydrotreatment oil; Described hydrotreatment oil is distilled, remove light ends, obtain described environment-friendly rubber oil.
In above-mentioned preparation method, described cycloalkyl distillate is the vacuum distillate that naphthenic base crude obtains through atmospheric and vacuum distillation, with GB/T 9168 methods, measures, and 2% of described cycloalkyl distillate is greater than 330 ℃, and 97% is less than 540 ℃; With GB/T 510 methods, measure, the condensation point of described cycloalkyl distillate is less than 20 ℃; With ASTM D2140 method, measure the C of described cycloalkyl distillate
avalue is greater than 10%;
In above-mentioned preparation method, 2% of described cycloalkyl distillate is greater than 350 ℃, and 97% is less than 530 ℃; Condensation point is less than 15 ℃, is preferably less than 10 ℃; The C of described cycloalkyl distillate
avalue is greater than 15%.
In above-mentioned preparation method, in step (1), described solvent-refined solvent can be selected from least one in furfural, phenol and N-Methyl pyrrolidone, preferably furfural or N-Methyl pyrrolidone; The ratio of quality and the number of copies of described solvent and described cycloalkyl distillate can be (2.0～3.5): 1, as 2.5: 1,2.7: 1 or 3.5: 1 etc.; When take N-Methyl pyrrolidone during as solvent, solvent comprises water 1.0～3.0% (weight percentage).
In above-mentioned preparation method, in step (1), in described solvent treatment process, the tower top temperature of described solvent treatment tower can be 90 ℃～140 ℃, and as 105 ℃, 110 ℃ or 130 ℃ etc., column bottom temperature can be 70 ℃～110 ℃, as 80 ℃ or 95 ℃ etc.; The temperature of described tower top temperature at the bottom of than described tower be high 10 ℃～and 45 ℃, preferably 20 ℃～35 ℃.
In above-mentioned preparation method, the aromatic carbon content that can control described treated oil (is C
avalue, ASTM D2140 method is measured) be less than 6.0%, be preferably less than 4.0%, adjust according to this refining service temperature of different material Oil solvent and agent-oil ratio.
In above-mentioned preparation method, in step (2), the temperature of described hydrotreatment can be 310 ℃～400 ℃, and preferably 335 ℃～370 ℃, as 345 ℃, 360 ℃ or 365 ℃ etc.; The oily volume parts ratio of hydrogen and described extraction can be (600～1500): 1, preferably (800～1000): 1, as 800: 1 or 1000: 1 etc.; The volume space velocity of hydrotreatment can be 0.2h
-1～1.5h
-1, preferred 0.3h
-1～0.9h
-1, as 0.3h
-1, 0.4h
-1or 0.8h
-1deng; Hydrogen dividing potential drop can be 6.0MPa～18.0MPa, and preferred 8.0MPa～15.0MPa, as 10.0MPa, 13.0MPa or 15.0MPa etc.
In above-mentioned preparation method's step (2), the hydrotreating catalyst of described hydrotreatment can be molybdenum-nickel type hydrogenation catalyst, tungsten-nickel type hydrogenation catalyst, molybdenum-cobalt type hydrogenation catalyst and/or molybdenum-tungsten-nickel type hydrogenation catalyst, as commercially available LH-23 catalyzer (standard catalyst company), CH-4 catalyzer (Sinopec Group's catalyzer Chang Ling branch office), CH-15 catalyzer (Sinopec Group's catalyzer Chang Ling branch office), FV-5 catalyzer (China Petroleum and Chemical Corporation Fushun Petrochemical Research Institute) or FV-10 catalyzer (China Petroleum and Chemical Corporation Fushun Petrochemical Research Institute) etc.
In above-mentioned preparation method, can collect higher than the cut of 370 ℃ as described environment-friendly rubber oil.
The present invention also provides the environment-friendly rubber oil being prepared by aforesaid method, with the method for IP346, detects, and its PCA (polycyclic aromatic hydrocarbon content) is less than 3%; With the methods analyst of ASTM D2140, its carbon type analysis C
avalue is greater than 13%; Methods analyst with GC-MS, its benzo [a] pyrene content < 1mg/kg, and PAHs < 10mg/kg (PAHs is benzo [a] pyrene, benzo [e] pyrene, benzo [a] anthracene, bend, the total content of benzo [b] fluoranthene, benzo [j] fluoranthene, benzo [k] fluoranthene and hexichol [a, h] 8 kinds of aromatic hydrocarbons of anthracene).
The present invention has following beneficial effect: stock oil is after solvent treatment, and treated oil has that aromaticity content is low, saturated hydrocarbon content is high, and light-colored feature, is the naphthenic base oils of high-quality, is widely used; Low value-added non-environmental protection is extracted oil out through further hydrotreatment, is converted into the environment-friendly rubber oil of high added value, has significantly improved the whole economic efficiency of cycloalkyl distillate.
Embodiment
The experimental technique using in following embodiment if no special instructions, is ordinary method.
In following embodiment, material used, reagent etc., if no special instructions, all can obtain from commercial channels.
The preparation of embodiment 1, environment-friendly rubber oil
(1) what take that Zhonghai Pitch Co., Ltd full scale plant produces subtracts three line distillates as raw material (stock oil character is in Table 1), at solvent treatment small testing device, test that (stock oil and solvent total feed are 3kg/h, in tower, place random packing, theoretical plate number is 3 theoretical stages), solvent is furfural, agent weight of oil ratio is 3.5: 1, and treating tower tower top temperature is 130 ℃, and column bottom temperature is 95 ℃; Treating tower bottom product is Extract, reclaims after solvent, obtains extracting out oil, extracts oil out as the raw material of hydrotreatment; Treating tower overhead product is refined liquid, and refined liquid obtains treated oil after reclaiming solvent, and treated oil is as naphthenic base oils.
(2) the extraction oil obtaining carries out hydrotreatment test at hydrotreatment pilot plant, and (Beijing is opened up river petrochemical industry evaluating apparatus technological development company limited and is produced, model is heavy-oil hydrogenation evaluation experimental device, loaded catalyst is 200ml, new hydrogen once passes through), temperature of reaction is 345 ℃, hydrogen to oil volume ratio is 1000: 1, and volume space velocity is 0.8h
-1, hydrogen dividing potential drop is 15.0MPa, hydrotreating catalyst is commercially available LH-23 catalyzer; The hydrotreatment oil obtaining is distilled, be greater than 370 ℃ of cuts and be environment-friendly rubber oil.
The performance perameter of environment-friendly rubber oil prepared by the present embodiment is as shown in table 2, and as seen from the data in Table 2, the yield of the relative vacuum distillate of environment-friendly rubber oil is 56.9%, the C of environment-friendly rubber oil
avalue is 14.1%, and polycyclic aromatic hydrocarbon content is that 2.2%, PAHs content is 4.0mg/kg, and wherein benzo [a] pyrene content does not detect.
The preparation of embodiment 2, environment-friendly rubber oil
(1) raw materials used oil, solvent treatment tower and refining solvent are in the same manner as in Example 1; Wherein, agent weight of oil ratio is 2.5: 1, and treating tower tower top temperature is 105 ℃, and column bottom temperature is 80 ℃, and treating tower bottom product is Extract, reclaims after solvent, obtains extracting out oil, extracts oil out as the raw material of hydrotreatment; Treating tower overhead product is refined liquid, and refined liquid obtains treated oil after reclaiming solvent, and treated oil is as naphthenic base oils.
(2) hydrotreater used and hydrotreating catalyst are in the same manner as in Example 1; Wherein, hydrotreatment temperature of reaction is 365 ℃, and hydrogen to oil volume ratio is 1000: 1, and volume space velocity is 0.3h
-1, hydrogen dividing potential drop is 10.0MPa, and hydrotreatment oil is distilled, and is greater than 370 ℃ of cuts and is environment-friendly rubber oil.
The performance perameter of environment-friendly rubber oil prepared by the present embodiment is as shown in table 2, and as seen from the data in Table 2, the yield of the relative vacuum distillate of environment-friendly rubber oil is 39.3%, the C of environment-friendly rubber oil
avalue is 17.2%, and polycyclic aromatic hydrocarbon content is that 2.8%, PAHs content is 8.7mg/kg, and wherein benzo [a] pyrene content is 0.2mg/kg.
The preparation of embodiment 3, environment-friendly rubber oil
(1) what take that Zhonghai Pitch Co., Ltd full scale plant produces subtracts four line distillates as raw material (stock oil character is in Table 1), solvent treatment tower is identical with embodiment 1, using N-Methyl pyrrolidone as solvent-refined solvent (moisture 2.0%, weight percentage), and agent weight of oil ratio is 2.7: 1, treating tower tower top temperature is 110 ℃, column bottom temperature is 80 ℃, and treating tower bottom product is Extract, reclaims after solvent, obtain extracting out oil, extract oil out as the raw material of hydrotreatment; Treating tower overhead product is refined liquid, and refined liquid obtains treated oil after reclaiming solvent, and treated oil is as naphthenic base oils.
(2) the extraction oil obtaining carries out hydrotreatment test at hydrotreatment pilot plant, and hydrotreatment temperature of reaction is 360 ℃, and hydrogen to oil volume ratio is 800: 1, and volume space velocity is 0.4h
-1, hydrogen dividing potential drop is 13.0MPa, hydrotreating catalyst is commercially available CH-15; The hydrotreatment oil obtaining is distilled, be greater than 370 ℃ of cuts and be environment-friendly rubber oil.
The performance perameter of environment-friendly rubber oil prepared by the present embodiment is as shown in table 4, and as seen from the data in Table 4, the yield of the relative vacuum distillate of environment-friendly rubber oil is 45.2%, the C of environment-friendly rubber oil
avalue is 16.4%, and polycyclic aromatic hydrocarbon content is that 2.7%, PAHs content is 8.9mg/kg, and wherein benzo [a] pyrene content is 0.1mg/kg.
The preparation of comparative example 1, rubber oil
Raw materials used oil, solvent treatment tower, refining solvent, hydrotreater and hydrotreating catalyst are all identical with embodiment 1; Wherein, first stock oil carry out hydrotreatment and obtain hydrotreatment oil, and hydrotreatment temperature of reaction is 330 ℃, and hydrogen to oil volume ratio is 1000: 1, and volume space velocity is 1.3h
-1, hydrogen dividing potential drop is 15.0MPa; Hydrotreatment oil is distilled, be greater than 370 ℃ of cuts as solvent-refined raw material; Solvent refining agent weight of oil ratio is 2.0: 1, and treating tower tower top temperature is 90 ℃, and column bottom temperature is 65 ℃, and treating tower overhead product is refined liquid, and refined liquid obtains treated oil after reclaiming solvent, and treated oil is as environment-friendly rubber oil.
The performance perameter of the environment-friendly rubber oil that this comparative example prepares is as shown in table 3, and as seen from the data in Table 3, the yield of the relative vacuum distillate of environment-friendly rubber oil is 85.3%, C
avalue is 6.8%, and polycyclic aromatic hydrocarbon content is that 2.0%, PAHs content is 6.7mg/kg, and wherein benzo [a] pyrene content is 0.1mg/kg.
From above-described embodiment 1-3 and comparative example 1, vacuum distillate to different flow process scopes, adopt the technology of the present invention, under different solvents refining depth, when obtaining high-quality naphthenic base oils, extract oil out and all can produce environment-friendly rubber oil, compared with prior art, not only do not produce low value-added extraction oil, and environment-friendly rubber oil has higher C
avalue, better with the consistency of rubber.
Table 1 stock oil character
The operational condition of table 2 embodiment 1 and embodiment 2 and the environment-friendly rubber oil properties obtaining
The operational condition of table 3 comparative example 1 and the rubber oil properties obtaining
The operational condition of table 4 embodiment 3 and the environment-friendly rubber oil properties obtaining
Claims (4)
1. a preparation method for environment-friendly rubber oil, comprises the steps:
(1) cycloalkyl distillate is placed in to solvent treatment tower and carries out solvent treatment, at the tower top of described solvent treatment tower, obtain refined liquid, reclaim after solvent, obtain treated oil, at the bottom of tower, obtain Extract, reclaim after solvent, obtain extracting out oil;
(2) described extraction oil is carried out to hydrotreatment and obtain hydrotreatment oil; Described hydrotreatment oil is distilled, remove light ends, obtain described environment-friendly rubber oil;
Described cycloalkyl distillate is the vacuum distillate that naphthenic base crude obtains through atmospheric and vacuum distillation, with GB/T9168 method, measures, and 2% of described cycloalkyl distillate is greater than 330 ℃, and 97% is less than 540 ℃; With GB/T510 method, measure, the condensation point of described cycloalkyl distillate is less than 20 ℃; With ASTM D2140 method, measure the C of described cycloalkyl distillate
avalue is greater than 10%; In step (1), with ASTM D2140 method, measure, control the aromatic carbon content C of described treated oil
avalue is less than 6.0%;
In step (1), described solvent-refined solvent is selected from least one in furfural, phenol and N-Methyl pyrrolidone; In step (1), the ratio of quality and the number of copies of described solvent and described cycloalkyl distillate is (2.0～3.5): 1;
In step (2), the temperature of described hydrotreatment is 310 ℃～400 ℃, and the oily volume parts of hydrogen and described extraction is than being (600～1500): 1, and the volume space velocity of hydrotreatment is 0.2h
-1～1.5h
-1, hydrogen dividing potential drop is 6.0MPa～18.0MPa.
2. preparation method according to claim 1, is characterized in that: in step (1), in described solvent treatment process, the tower top temperature of described solvent treatment tower is 90 ℃～140 ℃, and column bottom temperature is 70 ℃～110 ℃; The temperature of the temperature of described tower top at the bottom of than described tower be high 10 ℃～and 45 ℃.
3. preparation method according to claim 1 and 2, it is characterized in that: in step (2), the hydrotreating catalyst of described hydrotreatment is molybdenum-nickel type hydrogenation catalyst, tungsten-nickel type hydrogenation catalyst, molybdenum-cobalt type hydrogenation catalyst and/or molybdenum-tungsten-nickel type hydrogenation catalyst.
4. the environment-friendly rubber oil that in claim 1-3 prepared by arbitrary described method.
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|---|---|---|---|---|
| CN103242905B (en) * | 2013-05-27 | 2014-12-24 | 中国海洋石油总公司 | High-aromatic hydrocarbon environmental-friendly rubber oil and preparation method thereof |
| CN103320165B (en) * | 2013-07-11 | 2014-12-03 | 中国海洋石油总公司 | Method for producing environmentally-friendly rubber oil through using inferior cycloalkyl heavy wax oil, and environmentally-friendly rubber oil prepared therethrough |
| CN107987876B (en) * | 2016-10-26 | 2020-04-28 | 中国石油化工股份有限公司 | Method for preparing environment-friendly naphthenic rubber oil |
| CN107129693B (en) * | 2017-06-21 | 2020-04-10 | 中海油气(泰州)石化有限公司 | Environment-friendly rubber oil and preparation method thereof |
| CN111170904B (en) * | 2018-11-12 | 2022-12-02 | 中国石油天然气股份有限公司 | Petroleum sulfonate raw material and preparation method thereof, petroleum sulfonate and production method thereof |
| CN115651289B (en) * | 2022-11-15 | 2024-01-26 | 中国海洋石油集团有限公司 | High C A Aromatic rubber plasticizer with value and preparation method thereof |
| CN115651699A (en) * | 2022-11-15 | 2023-01-31 | 中国海洋石油集团有限公司 | High-viscosity high-aromatic-hydrocarbon rubber plasticizer and preparation method thereof |
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|---|---|---|---|---|
| US3732154A (en) * | 1969-02-19 | 1973-05-08 | Sun Oil Co | Catalytic hydrofinishing of lube oil product of solvent extraction of petroleum distillate |
| US6110358A (en) * | 1999-05-21 | 2000-08-29 | Exxon Research And Engineering Company | Process for manufacturing improved process oils using extraction of hydrotreated distillates |
| CN101386687A (en) * | 2008-10-24 | 2009-03-18 | 中国海洋石油总公司 | Aromatic rubber oil and producing method thereof |
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Effective date of registration: 20170220 Address after: 100010 Beijing, Chaoyangmen, North Street, No. 25, No. Patentee after: CHINA NATIONAL OFFSHORE OIL Corp. Patentee after: CNOOC OIL & PETROCHEMICALS Co.,Ltd. Patentee after: CNOOC RESEARCH INSTITUTE OF REFINING AND PETROCHEMICALS (BEIJING) Co.,Ltd. Address before: 100010 Beijing, Chaoyangmen, North Street, No. 25, No. Patentee before: CHINA NATIONAL OFFSHORE OIL Corp. Patentee before: CHINA OFFSHORE OIL & GAS DEVELOPMENT & UTILIZATION Co. Patentee before: CNOOC (QINGDAO) HEAVY OIL PROCESSING ENGINEERING TECHNOLOGY RESEARCH CENTER Co.,Ltd. |
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Address after: 100010 Chaoyangmen North Street, Dongcheng District, Dongcheng District, Beijing Co-patentee after: CNOOC OIL & PETROCHEMICALS Co.,Ltd. Patentee after: CHINA NATIONAL OFFSHORE OIL Corp. Co-patentee after: CNOOC RESEARCH INSTITUTE OF REFINING AND PETROCHEMICALS (BEIJING) Co.,Ltd. Address before: 100010 Chaoyangmen North Street, Dongcheng District, Dongcheng District, Beijing Co-patentee before: CNOOC OIL & PETROCHEMICALS Co.,Ltd. Patentee before: CHINA NATIONAL OFFSHORE OIL Corp. Co-patentee before: CNOOC RESEARCH INSTITUTE OF REFINING AND PETROCHEMICALS (BEIJING) Co.,Ltd. |
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Effective date of registration: 20180508 Address after: 100010 Chaoyangmen North Street, Dongcheng District, Dongcheng District, Beijing Co-patentee after: CNOOC OIL & PETROCHEMICALS Co.,Ltd. Patentee after: CHINA NATIONAL OFFSHORE OIL Corp. Co-patentee after: CNOOC RESEARCH INSTITUTE OF REFINING AND PETROCHEMICALS (BEIJING) Co.,Ltd. Co-patentee after: CNOOC (QINGDAO) HEAVY OIL PROCESSING ENGINEERING TECHNOLOGY RESEARCH CENTER Co.,Ltd. Address before: 100010 Chaoyangmen North Street, Dongcheng District, Dongcheng District, Beijing Co-patentee before: CNOOC OIL & PETROCHEMICALS Co.,Ltd. Patentee before: CHINA NATIONAL OFFSHORE OIL Corp. Co-patentee before: CNOOC RESEARCH INSTITUTE OF REFINING AND PETROCHEMICALS (BEIJING) Co.,Ltd. |
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