CN104151263A - Anhydrous preparation technology for vulcanization promoter M - Google Patents
Anhydrous preparation technology for vulcanization promoter M Download PDFInfo
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- CN104151263A CN104151263A CN201410386763.4A CN201410386763A CN104151263A CN 104151263 A CN104151263 A CN 104151263A CN 201410386763 A CN201410386763 A CN 201410386763A CN 104151263 A CN104151263 A CN 104151263A
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- solvent
- preparation technology
- anhydrous preparation
- crude product
- mbt
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D277/00—Heterocyclic compounds containing 1,3-thiazole or hydrogenated 1,3-thiazole rings
- C07D277/60—Heterocyclic compounds containing 1,3-thiazole or hydrogenated 1,3-thiazole rings condensed with carbocyclic rings or ring systems
- C07D277/62—Benzothiazoles
- C07D277/68—Benzothiazoles with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached in position 2
- C07D277/70—Sulfur atoms
- C07D277/72—2-Mercaptobenzothiazole
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses an anhydrous preparation technology for a vulcanization promoter M. the anhydrous preparation technology is characterized in that aniline, sulfur and carbon disulfide are thrown into a high-pressure autoclave to synthesize a crude product M; the crude product M is thrown into a solvent kettle and completely dissolved in the solvent kettle and subject to first hot filtration through a hot filter to remove insoluble matters and enter an adsorbing kettle containing an adsorbent for absorbing impurities, is subject to second hot filtration through another hot filter; a filtered crude product M solution is transmitted to a crystallizing tank for cooling so as to separate out products; a solvent and a product M solution are pressed into a dryer to filter out the solvent and obtain the solvent through heating, pressure reducing, drying and recycling; the promoter M is packaged after cooled through the dryer; the technology is operated in a completely closed condition. According to the invention, the anhydrous preparation technology is energy-saving, pollution-free, short in production cycle and high in safety, water is not needed, and waste water is not produced; pressure filtration and suction filtration are conducted in inert gas under the closed condition, so that the quality of products is high, and the yield is high.
Description
Technical field
The present invention relates to chemical rubber vulcanization accelerator technical field, be specifically related to a kind of anhydrous preparation technology of 2 Mercaptobenzothiazole (MBT).
Background technology
At present, main two kinds of the refining existing technique of captax: (1) water method: height is pressed into rear discharging and generates M sodium salt in the molten still of alkali, entering the oxidation of oxidation axe thin up, impurity is proposed, in being filled into and in still and acid adding, close dehydration, dry packing.This technique is maximum technique of producing now use, 170 ℃-171 ℃ of product fusing points. 20 tons of one ton of product waters of every production, contains sodium sulfate in waste water, cannot process pollution.(2) broken following the example of: height is pressed into rear discharging and cools to below 30 ℃ in toluene tank.With the impurity in toluene stripping M, toluene is filtered out with inhaling worry groove.Generalized case one batch of material will be got three times with toluene is broken. and be dried, pack, this technique is that toluene an ancient egg-shaped, holed wind instrument consumption is large.80-120 kilogram of product consumption per ton, the toluene volatilizing is harmful.Dangerous quality product is low, and fusing point is domestic with regard to several families 168 ℃ of these techniques, because of the defective sale of product bad.
Summary of the invention
Object of the present invention is exactly the defect existing for prior art, the anhydrous preparation technology who provides a kind of 2 Mercaptobenzothiazole (MBT) to purify.
Its technical scheme is: the anhydrous preparation technology of 2 Mercaptobenzothiazole (MBT), is characterized in that: aniline, sulphur, dithiocarbonic anhydride are squeezed in autoclave, and under 265 ℃-270 ℃ of temperature, pressure 9.5-9.7MPA, height is pressed into crude product M, crude product M is all driven in solvent still, and 85 ℃-95 ℃ of temperature, pressure 0.1-0.3MPA is dissolved in the solvent in solvent still completely, temperature is 85 ℃-95 ℃ again, pressure is that 0.09-0.15MPA carries out heat filtering for the first time by heat filter, after removing insolubles, enter suck up impurity in the absorption still that is added with sorbent material, then by another heat filter, carry out heat filtering for the second time, through the crude product M lysate filtering, being transported to crystallizer is cooled to below 30 ℃, solvent is comprised to product M lysate is pressed onto in moisture eliminator together, by rare gas element, be press-filtered out solvent and heat drying under reduced pressure recovery solvent, discharging wrapped product captax after the cooling of drying device, above-mentioned technique is under sealing, to carry out completely.
Wherein, the mol ratio of described aniline, sulphur, dithiocarbonic anhydride is 0.9-1.1:1-1.06:1.1-1.2.The mol ratio of described aniline, sulphur, dithiocarbonic anhydride the best is 1:1.03:1.15.Described sorbent material is silicon dioxide activity charcoal.Described rare gas element is nitrogen.
The present invention compared with prior art, has the following advantages: energy-conservation, not water, pollution-free without waste water, solvent load is few, with short production cycle, safe.Hermetic type is produced press filtration suction filtration under rare gas element, and the high yield of quality product is high.
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet of an embodiment of the present invention.
Embodiment
Embodiment 1
With reference to Fig. 1, a kind of anhydrous preparation technology of 2 Mercaptobenzothiazole (MBT), the aniline that is 0.9:1:1.2 by mol ratio, sulphur, dithiocarbonic anhydride are squeezed in autoclave, and under 260 ℃, pressure 8MPA, height is pressed into crude product M, crude product M is all driven in solvent still, and 85 ℃ of temperature, pressure 0.1MPA is dissolved in the solvent in solvent still completely, by heat filter, carry out heat filtering for the first time again, remove after insolubles and enter and be added with suck up impurity in the absorption still that sorbent material is silicon dioxide activity charcoal, then by another heat filter, carry out heat filtering for the second time, through the crude product M lysate filtering, be transported to crystallizer and be cooled to 40 ℃, enter in the cryogenic tank that is added with solvent and separate out, solvent is comprised to crude product M lysate is pressed onto in moisture eliminator together, by inert nitrogen gas, carrying out safety is press-filtered out solvent and heats drying under reduced pressure recovery solvent, discharging wrapped product captax after the cooling of drying device.
Embodiment 2
With reference to Fig. 1, a kind of anhydrous preparation technology of 2 Mercaptobenzothiazole (MBT), the aniline that is 1:1.03:1.15 by mol ratio, sulphur, dithiocarbonic anhydride are squeezed in autoclave, and under 270 ℃, pressure 10MPA, height is pressed into crude product M; Crude product M is all driven in solvent still, and be dissolved in completely in the solvent in solvent still at 90 ℃ of temperature, pressure 0.2MPA, by heat filter, carry out heat filtering for the first time again, remove and enter that to be added with sorbent material be silicon-dioxide after insolubles, in the absorption still of gac, suck up impurity reaches purification requirement, then by another heat filter, carry out heat filtering for the second time, through the crude product M lysate filtering, be transported to crystallizer and be cooled to 30 ℃ and separate out below product, solvent is comprised
product M lysatebe pressed onto together in moisture eliminator, by inert nitrogen gas, undertaken that safety is press-filtered out solvent and the drying under reduced pressure of heating reclaims solvent, discharging wrapped product promotor product M after the cooling of drying device.
Technique of the present invention is under sealing, to carry out completely, with rare gas element press filtration, the solvent-free volatilization of safety, without waste water.Product fusing point is more than 175 ℃.(national top grade product are 173 ℃)
The present invention is energy-conservation, water,, solvent pollution-free without waste water can not be repeatedly used without distilation, so that consumption is few, with short production cycle, hermetic type is produced under rare gas element press filtration suction filtration is safe, the high yield of quality product is high.
Claims (5)
1. the anhydrous preparation technology of 2 Mercaptobenzothiazole (MBT), is characterized in that: aniline, sulphur, dithiocarbonic anhydride are squeezed in autoclave, and under 265 ℃-270 ℃ of temperature, pressure 9.5-9.7MPA, height is pressed into crude product M, crude product M is all driven in solvent still, and 85 ℃-95 ℃ of temperature, pressure 0.1-0.3MPA is dissolved in the solvent in solvent still completely, in temperature, it is 85 ℃-95 ℃, pressure is that 0.09-0.15MPA carries out heat filtering for the first time by heat filter, after removing insolubles, enter suck up impurity in the absorption still that is added with sorbent material, then by another heat filter, carry out heat filtering for the second time, through the crude product M lysate filtering, being transported to crystallizer is cooled to below 30 ℃, enter in the cryogenic tank that is added with solvent and separate out, solvent is comprised to product M lysate is pressed onto in moisture eliminator together, by rare gas element, be press-filtered out solvent and heat drying under reduced pressure recovery solvent, discharging wrapped product captax after the cooling of drying device, above-mentioned technique is under sealing, to carry out completely.
2. the anhydrous preparation technology of 2 Mercaptobenzothiazole (MBT) according to claim 1, is characterized in that: the mol ratio of described aniline, sulphur, dithiocarbonic anhydride is 0.9-1.1:1-1.06:1.1-1.2.
3. the anhydrous preparation technology of 2 Mercaptobenzothiazole (MBT) according to claim 1 and 2, is characterized in that: the mol ratio of described aniline, sulphur, dithiocarbonic anhydride the best is 1:1.03:1.15.
4. the anhydrous preparation technology of 2 Mercaptobenzothiazole (MBT) according to claim 1, is characterized in that: described sorbent material is silicon dioxide activity charcoal.
5. the anhydrous preparation technology of 2 Mercaptobenzothiazole (MBT) according to claim 1, is characterized in that: described rare gas element is nitrogen.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410386763.4A CN104151263B (en) | 2014-08-08 | 2014-08-08 | The anhydrous preparation technology of 2 Mercaptobenzothiazole (MBT) |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410386763.4A CN104151263B (en) | 2014-08-08 | 2014-08-08 | The anhydrous preparation technology of 2 Mercaptobenzothiazole (MBT) |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104151263A true CN104151263A (en) | 2014-11-19 |
| CN104151263B CN104151263B (en) | 2016-03-16 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410386763.4A Expired - Fee Related CN104151263B (en) | 2014-08-08 | 2014-08-08 | The anhydrous preparation technology of 2 Mercaptobenzothiazole (MBT) |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107629024A (en) * | 2017-10-13 | 2018-01-26 | 山东尚舜化工有限公司 | A kind of continuous synthesizer of rubber vulcanization accelerator M and its production technology |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101759659A (en) * | 2009-11-16 | 2010-06-30 | 天津市科迈化工有限公司 | Method for synthesizing thiofide MBT by liquid sulphur |
| CN103965137A (en) * | 2014-05-07 | 2014-08-06 | 镇江苏秦环保科技有限公司 | Method for refining accelerant M(2-mercaptobenzothiazole) by using non-aqueous polarity method |
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2014
- 2014-08-08 CN CN201410386763.4A patent/CN104151263B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101759659A (en) * | 2009-11-16 | 2010-06-30 | 天津市科迈化工有限公司 | Method for synthesizing thiofide MBT by liquid sulphur |
| CN103965137A (en) * | 2014-05-07 | 2014-08-06 | 镇江苏秦环保科技有限公司 | Method for refining accelerant M(2-mercaptobenzothiazole) by using non-aqueous polarity method |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107629024A (en) * | 2017-10-13 | 2018-01-26 | 山东尚舜化工有限公司 | A kind of continuous synthesizer of rubber vulcanization accelerator M and its production technology |
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| CN104151263B (en) | 2016-03-16 |
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Granted publication date: 20160316 Termination date: 20200808 |