CN106905259A - The method that rubber accelerator M is prepared using micro passage reaction - Google Patents
The method that rubber accelerator M is prepared using micro passage reaction Download PDFInfo
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- CN106905259A CN106905259A CN201710130513.8A CN201710130513A CN106905259A CN 106905259 A CN106905259 A CN 106905259A CN 201710130513 A CN201710130513 A CN 201710130513A CN 106905259 A CN106905259 A CN 106905259A
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- reaction
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- microreactor
- micro passage
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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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- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to chemical industry synthesis field, a kind of method that utilization micro passage reaction prepares rubber accelerator M is particularly disclosed.This prepares the method for rubber accelerator M using micro passage reaction, including the micro passage reaction being formed by connecting by micro-mixer and microreactor, it is characterised in that：Cosan is dissolved in solution is formed in carbon disulfide, and aniline is pumped into micro-mixer by metering and mixed, and is then fed into being reacted in microreactor, microreactor end is provided with counterbalance valve and gas collector；Reaction is purified after terminating, suction filtration, filter cake are washed, drying, finally obtains captax.Course of reaction of the present invention is simple, safety, and it is successive reaction to react, and security is higher compared with prior art, can effectively improve the yield and purity of captax, improve product quality, it is ensured that the stability of product quality, it is easy to operate.
Description
（One）Technical field
The present invention relates to chemical industry synthesis field, the method that more particularly to a kind of utilization micro passage reaction prepares rubber accelerator M.
（Two）Background technology
Captax, chemical name is 2- benzothiazolyl mercaptans, molecular formula C7H5NS2, relative molecular mass is 167.26, is also cried
Accelerant MBT, product appearance has micro- smelly and bitter taste, relative density 1.42 for yellowish powder.170~181 DEG C of fusing point.It is dissolved in third
The alkaline solution such as ketone, ethyl acetate, dichloromethane, ethanol and NaOH and sodium carbonate.It is slightly soluble in benzene, water insoluble and vapour
Oil.Flammable, during in dust, LEL is 21g/m3。
The structural formula of captax is shown below：
。
Captax is universal accelerator, is widely used in various rubber, is had to natural gum and general sulfur cross-linking rubber polymer
Effect is rapidly promoted, glue burning event is short, vulcanizes flat molded breadth.Easily disperse in rubber, do not pollute, but contacted with its vulcanizate
Article tend to have bitter taste.Mainly for the manufacture of tire, the inner tube of a tyre, adhesive tape, rubber overshoes and industrial product.
The synthetic method of rubber accelerator M is mainly the completion in autoclave, and it is high to there is high temperature in production process
Pressure, the features such as side reaction is more, potential safety hazard is larger.In the last few years, because micro passage reaction is equipped in other chemical industry
In successful Application and cause and pay close attention to more and more widely.Micro passage reaction is different from batch reactor, and microchannel plate should
Utensil has that mixing rate is fast, heat and mass transfer performance is good, contact between homogeneous response condition, molecule, it is safe the features such as.It is micro- logical
Road reactor uses continuous flowing reactive, therefore the chemical quantity for stopping in the reactor is always little, even if just in case losing
Control, the extent of injury is also very limited.Micro passage reaction heat exchange efficiency is additionally, since high, even if release is a large amount of suddenly for reaction
Heat, it is also possible to derived rapidly, so as to ensure the stabilization of reaction temperature, reduces generation security incident and quality accident occurs
Possibility.
（Three）The content of the invention
The present invention is in order to make up the deficiencies in the prior art, there is provided a kind of course of reaction is simple, safety, and the utilization of high conversion rate is micro-
The method that channel reactor prepares rubber accelerator M.
The present invention is achieved through the following technical solutions：
A kind of method that utilization micro passage reaction prepares rubber accelerator M, including by micro-mixer and microreactor connection
Into micro passage reaction, it is characterised in that：Cosan is dissolved in solution is formed in carbon disulfide, and aniline is pumped by measuring
Enter mixing in micro-mixer, be then fed into being reacted in microreactor, microreactor end is provided with counterbalance valve and gas is received
Acquisition means；Reaction is purified after terminating, suction filtration, filter cake are washed, drying, finally obtains captax.
The characteristics of present invention is using micro passage reaction, is applied in the production of captax, by its HTHP
Severe production conditions are improved, and the very exothermic overcome in conventional high-tension reactor course of reaction causes poor product quality
Problem, easily meets technological requirement, realizes that highly effective and safe is produced.
More excellent technical scheme of the invention is：
The mol ratio of the aniline, carbon disulfide and sulphur is 1:1-1.2:1-1.1.
In the microreactor, reaction temperature is 180-300 DEG C, preferably 240-290 DEG C；Reaction pressure is 6.0-
12.0MPa, preferably 8.0-10.0MPa；Residence time is 0.5-30min, preferably 8-10min.More optimizedly, reaction temperature is
260 DEG C, reaction pressure is 10.0MPa, and the residence time is 10min.
1-3 material inlet, the reactor effluent stream of micro-mixer are connected with by connecting tube on the charging aperture of the micro-mixer
Speed is 0.04-5mL/min, preferably 0.5mL/min；The pressure regulation spectrum of counterbalance valve is 0-15MPa.
The micro-mixer is Y types, T-shaped or J-type blender, and microreactor is tubular microreactors, and internal diameter is 0.5-
3.0mm, preferably 1mm；Length is 0.5-20m.
Reaction equation of the invention is as follows：
。
Course of reaction of the present invention is simple, safety, and it is successive reaction to react, and security is higher compared with prior art, can
The effective yield and purity for improving captax, improve product quality, it is ensured that the stability of product quality, it is easy to operate.
（Four）Brief description of the drawings
The present invention is further illustrated below in conjunction with the accompanying drawings.
Fig. 1 is preparation flow schematic diagram of the invention.
（Five）Specific embodiment
According to following embodiments, the present invention may be better understood.However, as it will be easily appreciated by one skilled in the art that embodiment
Described content is merely to illustrate the present invention, without should also without limitation on this hair described in detail in claims
It is bright.
Embodiment 1：
Weighing 60g sulphur adds the carbon disulfide of 160g to stir and be deployed into solution, then takes the aniline of 84g, by measuring pump
Two phase liquid is driven to enter by Y blenders in the reactor of coil pipe footpath 1mm, the flow velocity of microreactor is 1mL/min, reaction solution
The residence time is 5min in reactor, and reaction temperature is 260 DEG C, and setting counterbalance valve is 8MPa.Start to collect after a cycle
Reaction solution.By purification, the product filter, being dried to obtain determines that yield is 90.9% after testing, and 171.2 DEG C of fusing point, outward appearance is light
Yellow powder.
Embodiment 2：
Weighing 60g sulphur adds the carbon disulfide of 160g to stir and be deployed into solution, then takes the aniline of 84g, by measuring pump
Two phase liquid is driven to enter by Y blenders in the reactor of coil pipe footpath 1mm, the flow velocity of microreactor is 0.5mL/min, reaction
Liquid residence time in reactor is 10min, and reaction temperature is 260 DEG C, and it is 8MPa to set by pressure valve.Start to receive after a cycle
Collection reaction solution.By purification, the product filter, being dried to obtain determines that yield is 91.3% after testing, 171.6 DEG C of fusing point, and outward appearance is
Pale yellow powder.
Embodiment 3：
Weighing 60g sulphur adds the carbon disulfide of 160g to stir and be deployed into solution, then takes the aniline of 84g, by measuring pump
Two phase liquid is driven to enter by Y blenders in the reactor of coil pipe footpath 1mm, the flow velocity of microreactor is 0.25mL/min, instead
It is 20min to answer liquid residence time in reactor, and reaction temperature is 260 DEG C, and it is 8MPa to set by pressure valve.Start after a cycle
Collect reaction solution.By purification, the product filter, being dried to obtain determines that yield is 90.5%, 171.3 DEG C of fusing point, outward appearance after testing
It is pale yellow powder.
Embodiment 4：
Weighing 60g sulphur adds the carbon disulfide of 160g to stir and be deployed into solution, then takes the aniline of 84g, by measuring pump
Two phase liquid is driven to enter by Y blenders in the reactor of coil pipe footpath 1mm, the flow velocity of microreactor is 0.5mL/min, reaction
Liquid residence time in reactor is 10min, and reaction temperature is 240 DEG C, and it is 8MPa to set by pressure valve.Start to receive after a cycle
Collection reaction solution.By purification, the product filter, being dried to obtain determines that yield is 89.6% after testing, 171.8 DEG C of fusing point, and outward appearance is
Pale yellow powder.
Embodiment 5：
Weighing 60g sulphur adds the carbon disulfide of 160g to stir and be deployed into solution, then takes the aniline of 84g, by measuring pump
Two phase liquid is driven to enter by Y blenders in the reactor of coil pipe footpath 1mm, the flow velocity of microreactor is 0.5mL/min, reaction
Liquid residence time in reactor is 10min, and reaction temperature is 280 DEG C, and it is 8MPa to set by pressure valve.Start to receive after a cycle
Collection reaction solution.By purification, the product filter, being dried to obtain determines that yield is 90.1% after testing, 171.5 DEG C of fusing point, and outward appearance is
Pale yellow powder.
Claims (7)
1. a kind of method that utilization micro passage reaction prepares rubber accelerator M, including connected by micro-mixer and microreactor
Micro passage reaction, it is characterised in that：Cosan is dissolved in solution is formed in carbon disulfide, and aniline passes through measuring pump
Mix in feeding micro-mixer, be then fed into being reacted in microreactor, microreactor end is provided with counterbalance valve and gas
Collection device；Reaction is purified after terminating, suction filtration, filter cake are washed, drying, finally obtains captax.
2. the method that utilization micro passage reaction according to claim 1 prepares rubber accelerator M, it is characterised in that：Institute
The mol ratio for stating aniline, carbon disulfide and sulphur is 1:1-1.2:1-1.1.
3. the method that utilization micro passage reaction according to claim 1 prepares rubber accelerator M, it is characterised in that：Institute
State in microreactor, reaction temperature is 180-300 DEG C, and reaction pressure is 6.0-12.0MPa, and the residence time is 0.5-30min.
4. the method that utilization micro passage reaction according to claim 1 prepares rubber accelerator M, it is characterised in that：Institute
State and 1-3 material inlet is connected with by connecting tube on the charging aperture of micro-mixer, the tapping flowrate of micro-mixer is 0.04-
5mL/min；The pressure regulation spectrum of counterbalance valve is 0-15MPa.
5. the method that utilization micro passage reaction according to claim 1 prepares rubber accelerator M, it is characterised in that：Institute
Micro-mixer is stated for Y types, T-shaped or J-type blender, microreactor is tubular microreactors, and internal diameter is 0.5-3.0mm, and length is
0.5-20m。
6. the method that utilization micro passage reaction according to claim 3 prepares rubber accelerator M, it is characterised in that：Institute
State in microreactor, reaction temperature is 240-290 DEG C, and reaction pressure is 8.0-10.0MPa, and the residence time is 8-10min.
7. the utilization micro passage reaction according to claim 4,5 or 6 prepares the method for being added captax, and its feature exists
In：In the microreactor, reaction temperature is 260 DEG C, and reaction pressure is 10.0MPa, and the residence time is 10min；Micro-mixer
Tapping flowrate be 0.5mL/min；The internal diameter of microreactor is 1mm.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108855055A (en) * | 2018-05-31 | 2018-11-23 | 南京东焱氢能源科技有限公司 | A kind of preparation method of the high activity hydroxide palladium carbon based on microreactor |
| CN109810074A (en) * | 2019-02-19 | 2019-05-28 | 蔚林新材料科技股份有限公司 | A kind of reaction unit of continuous synthesis 2-mercaptobenzothiazole |
| CN111423392A (en) * | 2020-06-15 | 2020-07-17 | 湖南速博生物技术有限公司 | Synthesis method of 2-mercapto-6-chlorobenzoxazole |
| CN114213297A (en) * | 2021-12-01 | 2022-03-22 | 蔚林新材料科技股份有限公司 | Method for continuously synthesizing rubber vulcanization accelerator EZ |
| CN115160255A (en) * | 2022-09-06 | 2022-10-11 | 科迈化工股份有限公司 | Method and system device for continuously producing 2-mercaptobenzothiazole |
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| CS197513B1 (en) * | 1977-08-25 | 1980-05-30 | Stanislav Kacani | Method for the continuous preparation of 2-mercaptobenzthiazole |
| SK53793A3 (en) * | 1993-05-26 | 1995-02-08 | Istrochem S P | Method of continual production of 2-mercaptobenzothiazole |
| RU2404171C2 (en) * | 2008-12-16 | 2010-11-20 | Алексей Андреевич Брункин | Method for continuous synthesis of 2-mercaptobenzothiazole in tube reactor and device for realising said method |
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2017
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| CS197513B1 (en) * | 1977-08-25 | 1980-05-30 | Stanislav Kacani | Method for the continuous preparation of 2-mercaptobenzthiazole |
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| RU2404171C2 (en) * | 2008-12-16 | 2010-11-20 | Алексей Андреевич Брункин | Method for continuous synthesis of 2-mercaptobenzothiazole in tube reactor and device for realising said method |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108855055A (en) * | 2018-05-31 | 2018-11-23 | 南京东焱氢能源科技有限公司 | A kind of preparation method of the high activity hydroxide palladium carbon based on microreactor |
| CN109810074A (en) * | 2019-02-19 | 2019-05-28 | 蔚林新材料科技股份有限公司 | A kind of reaction unit of continuous synthesis 2-mercaptobenzothiazole |
| CN109810074B (en) * | 2019-02-19 | 2023-02-10 | 蔚林新材料科技股份有限公司 | Reaction device for continuously synthesizing 2-mercaptobenzothiazole |
| CN111423392A (en) * | 2020-06-15 | 2020-07-17 | 湖南速博生物技术有限公司 | Synthesis method of 2-mercapto-6-chlorobenzoxazole |
| CN111423392B (en) * | 2020-06-15 | 2020-09-08 | 湖南速博生物技术有限公司 | Synthesis method of 2-mercapto-6-chlorobenzoxazole |
| CN114213297A (en) * | 2021-12-01 | 2022-03-22 | 蔚林新材料科技股份有限公司 | Method for continuously synthesizing rubber vulcanization accelerator EZ |
| CN115160255A (en) * | 2022-09-06 | 2022-10-11 | 科迈化工股份有限公司 | Method and system device for continuously producing 2-mercaptobenzothiazole |
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