CN103923062B - The precision processing technique of high pressure sulfide isobutene - Google Patents
The precision processing technique of high pressure sulfide isobutene Download PDFInfo
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- CN103923062B CN103923062B CN201410113562.7A CN201410113562A CN103923062B CN 103923062 B CN103923062 B CN 103923062B CN 201410113562 A CN201410113562 A CN 201410113562A CN 103923062 B CN103923062 B CN 103923062B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D341/00—Heterocyclic compounds containing rings having three or more sulfur atoms as the only ring hetero atoms
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Abstract
The invention discloses the precision processing technique of high pressure sulfide isobutene, comprise the following steps: extraction agent No. 6 industrial napthas and thick product high pressure sulfide isobutene are uniformly mixed according to volume ratio 0.5 ~ 2: 3 by (1); (2) be 0.5 ~ 3: 3 according to clear water and thick product high pressure sulfide isobutene volume ratio, add clear water, keep temperature to be 20 ~ 30 DEG C, agitator treating 10 ~ 40 minutes, point water-yielding stratum; (3) adding concentration is 3% ~ 15% superoxol, and keep temperature to be 20 ~ 30 DEG C, agitator treating 10 ~ 40 minutes, separates inorganic phase; (4) (2) operation is repeated; (5) be warming up to 100 DEG C, underpressure distillation goes out No. 6 industrial napthas and moisture; (6) keep temperature to be 40 ~ 80 DEG C, in product, pass into nitrogen carry out stripping in 1 ~ 3 hour, after filtration, obtain finished product high pressure sulfide isobutene.The high pressure sulfide isobutene product odour that the present invention produces is light, and of light color, storage time is long.
Description
Technical field
The present invention relates to the technical field of sulfide of acyclic unsaturated carbon skeleton, particularly relate to a kind of precision processing technique of high pressure sulfide isobutene.
Background technology
Sulfide isobutene is a kind of excellent lubricating grease extreme-pressure anti-friction additive, because it has higher sulphur content, extreme pressure anti-wear is strong, oil soluble good, copper corrosion performance is little, toxicity is low, consumption is few, on producing, particularly adjust the sulphur index of vulcanizing agent, the sulfide isobutene product of different sulphur content and different activities can be produced, therefore being widely used in gear oil, metalworking fluid and lubricating grease, is the main product of sulphur agent in current extreme pressure anti-wear additives.
In domestic sulfide isobutene traditional processing technology, typical conventional two-step synthesis technique is summarized as follows: iso-butylene and sulfur dichloride are at normal pressure, temperature is at 45 ~ 55 DEG C, addition reaction is carried out with catalyst action, generate sulphur chlorination isobutene adducts, discharge is containing the waste gas of HCl simultaneously, and catalyzer is lower alcohol, Lewis acid, iodine etc.Addition product obtains crude product sulfide isobutene with sodium sulphite or sodium polysulphide generation dechlorination reaction in the solubility promoter be made up of Virahol, the trimethyl carbinol and propyl carbinol (or other low-carbon alcohol), then with No. 120 industrial naptha extractions, washing, obtains finished product through diatomite filtration.
Technique comparatively advanced is at present high-pressure process, and domestic existing producer builds up the industrialized unit of the high-pressure process production sulfide isobutene of Production Equipment of 2000 t Capacity Per.This technique adopts SULPHUR POWDER, iso-butylene is raw material, take ammonia soln as catalyzer, directly carries out high-pressure synthesis reaction and prepares sulfide isobutene.This technique is comparatively simple relative to two-step synthesis method, and production cost is also cheaper, and product is little with traditional sulfide isobutene phase specific viscosity, and heat-resistant quality, oil soluble, extreme pressure anti-wear and copper corrosion performance are on close level.Main deficiency is that the precision processing technique in later stage is only add No. 120 industrial naptha extractions, and final high temperature distilling off solvent, causes the finished product smell weight, and color is dark, and storage time is long and occur precipitation.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of precision processing technique of high pressure sulfide isobutene.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is: the precision processing technique of high pressure sulfide isobutene, comprises the following steps:
(1) extraction agent No. 6 industrial napthas and thick product high pressure sulfide isobutene are uniformly mixed according to volume ratio 0.5 ~ 2: 3;
(2) be 0.5 ~ 3: 3 according to clear water and thick product high pressure sulfide isobutene volume ratio, add clear water, keep temperature to be 20 ~ 30 DEG C, agitator treating 10 ~ 40 minutes, point water-yielding stratum;
(3) be 0.5 ~ 2: 3 according to superoxol and crude product high pressure sulfide isobutene volume ratio, adding concentration is 3% ~ 15% superoxol, and keep temperature to be 20 ~ 30 DEG C, agitator treating 10 ~ 40 minutes, separates inorganic phase;
(4) be 0.5 ~ 3: 3 according to clear water and crude product high pressure sulfide isobutene volume ratio, add clear water, keep temperature 20 ~ 30 DEG C, agitator treating 10 ~ 40 minutes, point water-yielding stratum;
(5) be warming up to 100 DEG C, underpressure distillation goes out No. 6 industrial napthas and moisture;
(6) keep temperature to be 40 ~ 80 DEG C, in product, pass into nitrogen carry out stripping in 1 ~ 3 hour, after filtration, obtain finished product high pressure sulfide isobutene.
As preferably, in the hydrogen peroxide washes in step (3) and step (4) washes hybrid modulation concentration lower than 2% superoxol be recycling in the washing process of step (2).
As preferred further, the agitator treating time in step (2), (3), (4) is 30 minutes.
The invention has the beneficial effects as follows:
1. the high pressure sulfide isobutene product after this art breading is substantially without ammonia and thiol smell;
2. extraction agent adopts No. 6 industrial napthas, low compared with No. 120 industrial naptha recovered temperatures, and the time is short;
3. product colour is compared with more shallow before precision processing;
4. product places 10 months still clears, without precipitation.
Embodiment
Embodiment 1
(1) in reactor, elemental sulfur 20.4Kg is added, massfraction is the ammoniacal liquor 34Kg of 20%, be warming up to 200 DEG C, intermittent type slowly adds iso-butylene 25.5Kg, pressure controls all the time at below 4.5MPa, add rear continuation reaction 3 hours, be then cooled to 60 DEG C, utilize overbottom pressure that mixture is extruded reactor.Stratification, separates lower floor's inorganic phase, obtains high pressure sulfide isobutene crude product.
(2) get high pressure sulfide isobutene crude product 60L, add No. 6 industrial naptha 10L, be uniformly mixed, add clear water 20L, keep temperature 20 ~ 30 DEG C, agitator treating 30 minutes, point water-yielding stratum; Add concentration 15% superoxol 30L, keep temperature 20 ~ 30 DEG C, agitator treating 30 minutes, separates lower floor's inorganic phase; Add clear water 20L, keep temperature 20 ~ 30 DEG C, continue agitator treating 30 minutes, point water-yielding stratum; Be warming up to 100 DEG C, underpressure distillation goes out No. 6 industrial napthas and moisture; Keep temperature 60 C, in product, pass into nitrogen 2 hours.Product high pressure sulfide isobutene is obtained after filtration.
Embodiment 2
(1) with the step (1) of embodiment 1.
(2) get high pressure sulfide isobutene crude product 60L, add No. 6 industrial naptha 20L, be uniformly mixed, add clear water 30L, keep temperature 20 ~ 30 DEG C, agitator treating 30 minutes, point water-yielding stratum; Add concentration 10% superoxol 30L, keep temperature 20 ~ 30 DEG C, agitator treating 30 minutes, separates lower floor's inorganic phase; Add clear water 30L, keep temperature 20 ~ 30 DEG C, continue agitator treating 30 minutes, point water-yielding stratum; Be warming up to 100 DEG C, underpressure distillation goes out No. 6 industrial napthas and moisture; Keep temperature 40 DEG C, in product, pass into nitrogen 3 hours.Product high pressure sulfide isobutene is obtained after filtration.
Embodiment 3
(1) with the step (1) of embodiment 1.
(2) get high pressure sulfide isobutene crude product 60L, add No. 6 industrial naptha 30L, be uniformly mixed, add clear water 40L, keep temperature 20 ~ 30 DEG C, agitator treating 30 minutes, point water-yielding stratum; Add concentration 3% superoxol 20L, keep temperature 20 ~ 30 DEG C, agitator treating 30 minutes, separates lower floor's inorganic phase; Add clear water 40L, keep temperature 20 ~ 30 DEG C, continue agitator treating 30 minutes, point water-yielding stratum; Be warming up to 100 DEG C, underpressure distillation goes out No. 6 industrial napthas and moisture; Keep temperature 80 DEG C, in product, pass into nitrogen 1 hour.Product high pressure sulfide isobutene is obtained after filtration.
Embodiment 4
(1) with the step (1) of embodiment 1.
(2) get high pressure sulfide isobutene crude product 60L, add No. 6 industrial naptha 40L, be uniformly mixed, add clear water 60L, keep temperature 20 ~ 30 DEG C, agitator treating 30 minutes, point water-yielding stratum; Add concentration 5% superoxol 10L, keep temperature 20 ~ 30 DEG C, agitator treating 30 minutes, separates lower floor's inorganic phase; Add clear water 60L, keep temperature 20 ~ 30 DEG C, continue agitator treating 30 minutes, point water-yielding stratum; Be warming up to 100 DEG C, underpressure distillation goes out No. 6 industrial napthas and moisture; Keep temperature 60 C, in product, pass into nitrogen 2 hours.Product high pressure sulfide isobutene is obtained after filtration.
Above-described embodiment of the present invention, does not form limiting the scope of the present invention.Any amendment done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within claims of the present invention.
Claims (3)
1. the precision processing technique of high pressure sulfide isobutene, is characterized in that comprising the following steps:
(1) extraction agent No. 6 industrial napthas and thick product high pressure sulfide isobutene are uniformly mixed according to volume ratio 0.5 ~ 2: 3;
(2) be 0.5 ~ 3: 3 according to clear water and thick product high pressure sulfide isobutene volume ratio, add clear water, keep temperature to be 20 ~ 30 DEG C, agitator treating 10 ~ 40 minutes, point water-yielding stratum;
(3) be 0.5 ~ 2: 3 according to superoxol and crude product high pressure sulfide isobutene volume ratio, adding concentration is 3% ~ 15% superoxol, and keep temperature to be 20 ~ 30 DEG C, agitator treating 10 ~ 40 minutes, separates inorganic phase;
(4) be 0.5 ~ 3: 3 according to clear water and crude product high pressure sulfide isobutene volume ratio, add clear water, keep temperature 20 ~ 30 DEG C, agitator treating 10 ~ 40 minutes, point water-yielding stratum;
(5) be warming up to 100 DEG C, underpressure distillation goes out No. 6 industrial napthas and moisture;
(6) keep temperature to be 40 ~ 80 DEG C, in product, pass into nitrogen carry out stripping in 1 ~ 3 hour, after filtration, obtain finished product high pressure sulfide isobutene.
2. the precision processing technique of high pressure sulfide isobutene according to claim 1, is characterized in that: in the hydrogen peroxide washes in described step (3) and step (4) washes hybrid modulation concentration lower than 2% superoxol be recycling in the washing process of step (2).
3. the precision processing technique of high pressure sulfide isobutene according to claim 1, is characterized in that: the agitator treating time in described step (2), (3), (4) is 30 minutes.
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| US4119550A (en) * | 1975-03-21 | 1978-10-10 | The Lubrizol Corporation | Sulfurized compositions |
| EP0032281B1 (en) * | 1980-01-15 | 1984-04-04 | Edwin Cooper Inc. | A process for making an extreme pressure lubricating oil additive |
| CN101070296B (en) * | 2006-05-09 | 2012-12-05 | 东丽精密化学株式会社 | Preparation method of dicyclohexyldisulfide |
| CN1872837B (en) * | 2006-06-27 | 2011-04-13 | 山东联合化工股份有限公司 | Technique for extracting and washing sulfurized isobutene |
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Inventor after: Pan Wensheng Inventor after: Wu Xuhu Inventor after: Li Ping Inventor before: Wu Xuhu Inventor before: Song Xiaofei Inventor before: Wu Xuhu, Song Xiaofei, Wang Yuehu |
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Effective date of registration: 20151008 Address after: 233200, Anhui County, Chuzhou province Dingyuan County town salt chemical industry park Applicant after: DINGYUAN COUNTY YUNSEN TECHNOLOGY CO., LTD. Address before: 230000 No. 1, No. 264, No. 109 Changjiang East Road, Yaohai District, Anhui, Hefei Applicant before: Wu Xuhu |
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