CN107629024A - A kind of continuous synthesizer of rubber vulcanization accelerator M and its production technology - Google Patents
A kind of continuous synthesizer of rubber vulcanization accelerator M and its production technology Download PDFInfo
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- CN107629024A CN107629024A CN201710952464.6A CN201710952464A CN107629024A CN 107629024 A CN107629024 A CN 107629024A CN 201710952464 A CN201710952464 A CN 201710952464A CN 107629024 A CN107629024 A CN 107629024A
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- aniline
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- preheater
- vulcanization accelerator
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Abstract
The invention belongs to field of chemical equipment, the continuous synthesizer of more particularly to a kind of rubber vulcanization accelerator M and its production technology.Autoclaves for synthesis and a discharging kettle, a knockout drum including no less than two；The Autoclaves for synthesis, discharging kettle, knockout drum pass sequentially through discharge nozzle series connection；The Autoclaves for synthesis, discharging kettle upper end are connected by pressure-equalizing pipe；The Autoclaves for synthesis is connected to aniline preheater, molten sulphur liquid preheater by pipeline, and aniline preheater is connected with aniline measuring pump, and molten sulphur liquid preheater is connected with molten sulphur liquid measuring pump.The present invention realizes the continuous synthesis of rubber vulcanization accelerator M, realizes continuous operation, and automatic and mechanical degree is high, effectively raises the stability of product quality.The production capacity and production efficiency of product are improved, reduces production cost, meets the demand for development of chemical process automation production.
Description
（One）Technical field
The invention belongs to field of chemical equipment, the continuous synthesizer of more particularly to a kind of rubber vulcanization accelerator M and its production work
Skill.
（Two）Background technology
Rubber vulcanization accelerator M, full name are rubber vulcanization accelerant 2-mercaptobenzothiazole, are universal accelerator, extensively should
For various rubber, in natural gum and general rubber polymer, there is short vulcanization facilitation, in addition also have necessarily
Plasticity and anti-old property, can make delayer in neoprene.Captax or other rubber accelerators such as CZ, NS, DZ,
DM synthesis material, the market demand are bigger.
Synthetic rubber accelerator M method includes at present：Aniline process, o-nitrochlorobenzene method, nitrobenzene and nitrosobenzene
Method and benzothiazole method.Wherein aniline process is the widely used synthetic method of domestic and international manufacturer.Synthetic rubber vulcanization promotees
The prior art device for entering agent M uses intermittent high-pressure synthesis reactor more, to improve reaction mass transfer heat transfer efficiency, often takes band and stirs
The Autoclaves for synthesis mixed, but all produced for intermittently operated, quantum of output is limited by single inventory, the stability of product quality
Difference, equipment capacity is than relatively limited.And it is larger labor intensity to be present, the drawback such as operating environment difference.Therefore need to building-up process
Serialization transformation is carried out with equipment.
（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 continuous synthesizer of rubber vulcanization accelerator M and its life
Production. art.
The present invention is achieved through the following technical solutions：
A kind of continuous synthesizer of rubber vulcanization accelerator M, it is characterised in that：Autoclaves for synthesis including no less than two and one
Individual discharging kettle, a knockout drum；The Autoclaves for synthesis, discharging kettle, knockout drum pass sequentially through discharge nozzle series connection；Institute
State Autoclaves for synthesis, discharging kettle upper end is connected by pressure-equalizing pipe；The Autoclaves for synthesis is connected to benzene by pipeline
Amine preheater, molten sulphur liquid preheater, aniline preheater are connected with aniline measuring pump, and molten sulphur liquid preheater is connected with molten sulphur liquid metering
Pump.Turned on each bottom portion discharge nozzle into next procedure, peak is turned on each bottom portion discharge nozzle and is located at respective kettle height
Between 50-80%.
Wherein, the Autoclaves for synthesis, discharging kettle and knockout drum are respectively equipped with temperature and pressure control system.
Wherein, the Autoclaves for synthesis is provided with heating system.
Wherein, the heating system that the Autoclaves for synthesis is provided with is infrared heating, oil bath heating, one kind of salt bath heating
It is or several.
Wherein, discharging kettle enters knockout drum using the direct bottom discharge of bottom discharge pipe.
The production technology that rubber vulcanization accelerator M continuously synthesizes is as follows：
Aniline is squeezed into aniline preheater by aniline measuring pump to be preheated, molten sulphur liquid squeezed into by molten sulphur liquid measuring pump molten
Sulphur liquid preheater is preheated, it is preheated after aniline and molten sulphur liquid be continuously driven into the Autoclaves for synthesis of series connection carry out it is anti-
Should, end reaction material is drained into knockout drum and carries out continuous separation extraction by the kettle that discharged after reaction, and the gas of extraction is carried out
Gas treatment, liquid carry out purification processes.
Wherein, the molten sulphur liquid is that sulphur is dissolved in mixed liquor in carbon disulfide, and the mass ratio of sulphur and carbon disulfide is
1：2.1-2.4.
Wherein, the aniline, carbon disulfide, sulphur mol ratio are：1：1.0-1.2：1.0-1.3.
Wherein, synthesis temperature is 160-280 DEG C, synthesis pressure 5.0-10MPa, when reaction mass stops in synthesis reactor
For 2.0-4.5 hours.
The recyclable sulphur of extraction gas treatment prepares sulfuric acid or prepares NaHS with Alkali absorption.Produce liquid purification processes
Acid-base method and solvent method can be used.
The beneficial effects of the invention are as follows：1st, the continuous synthesis of rubber vulcanization accelerator M is realized, realizes serialization behaviour
Make, automatic and mechanical degree is high, effectively raises the stability of product quality.Improve production capacity and the production of product
Efficiency, production cost is reduced, meet the demand for development of chemical process automation production.2nd, the synthesis work that the present invention is connected using autoclave
Skill, being sufficiently mixed for reaction mass is realized, reaction temperature and pressure are relatively low, make the captax content of high pressure product
It is higher than traditional handicraft.
（Four）Brief description of the drawings
The present invention is further illustrated below in conjunction with the accompanying drawings.
Fig. 1 is the structural representation of the present invention；
In figure, 1- aniline measuring pumps, the molten sulphur liquid measuring pumps of 2-, 3- aniline preheaters, the molten sulphur liquid preheaters of 4-, 5- high-pressure synthesis
Kettle, 6- bottom discharge pipes, 7- pressure-equalizing pipes, 8- discharging kettles, 9- discharge nozzles, 10- knockout drums.
（Five）Embodiment
Embodiment 1
Accompanying drawing is a kind of specific embodiment of the invention.The embodiment includes being no less than the Autoclaves for synthesis 5 of two and one goes out
Expect 8, knockout drums 10 of kettle；The Autoclaves for synthesis 5, discharging kettle 8, knockout drum 10 pass sequentially through discharge nozzle 9 and gone here and there
Connection；The Autoclaves for synthesis 5, the discharging upper end of kettle 8 are connected by pressure-equalizing pipe 7；The Autoclaves for synthesis 5 is distinguished by pipeline
Aniline preheater 3, molten sulphur liquid preheater 4 are connected with, aniline preheater 3 is connected with aniline measuring pump 1, and molten sulphur liquid preheater 4 connects
It is connected to molten sulphur liquid measuring pump 2.Turned on each bottom portion discharge nozzle 96 into next procedure, peak is turned on each bottom portion discharge nozzle 96
Between the 50-80% of respective kettle height.
Wherein, the Autoclaves for synthesis 5, discharging kettle 8 and knockout drum 10 are respectively equipped with temperature and pressure control system.
Wherein, the Autoclaves for synthesis 5 is provided with heating system.
Wherein, the heating system that the Autoclaves for synthesis 5 is provided with is infrared heating, oil bath heating, the one of salt bath heating
Kind is several.
Wherein, the kettle 8 that discharges enters knockout drum 10 using 96 direct bottom discharge of bottom discharge pipe.
Embodiment 2
Using the device of embodiment 1, continuous synthetic rubber accelerator M：
Starting aniline measuring pump 1 makes aniline flow be 186g/h, is continuously pumped into aniline preheater 3, is drained into after being preheating to 200 DEG C
Autoclaves for synthesis 5.Starting molten sulphur liquid measuring pump 2 makes molten sulphur flow quantity be 230g/h, is continuously pumped into molten sulphur liquid preheater 4, preheating
Autoclaves for synthesis 5 is drained into after to 200 DEG C to be reacted.The heating system affiliated by autoclave is adjusted, controls Autoclaves for synthesis 5
Temperature is 220 DEG C, controls synthesis pressure 8.5MPa by the control pressurer system of discharging kettle 8, residence time of material 3 hours, is discharged into
To knockout drum 10, gas prepares NaHS by absorbing by liquid caustic soda, and liquid purifies through soda acid, obtains product thiofide
M.High pressure product M contents 94%, 172.0 DEG C of captax just fusing point after purification.
Embodiment 3
Using the device of embodiment 1, continuous synthetic rubber accelerator M：
Starting aniline measuring pump 1 makes aniline flow be 465g/h, is continuously pumped into aniline preheater 3, is drained into after being preheating to 200 DEG C
Autoclaves for synthesis 5.Starting molten sulphur liquid measuring pump 2 makes molten sulphur flow quantity be 580g/h, is continuously pumped into molten sulphur liquid preheater 4, preheating
Autoclaves for synthesis 5 is drained into after to 240 DEG C to be reacted.The heating system affiliated by autoclave is adjusted, controls Autoclaves for synthesis 5
Temperature is 240 DEG C, and synthesis pressure 9.0MPa, residence time of material 2.5 hours, row are controlled by the control pressurer system of discharging kettle 8
Entering to knockout drum 10, gas has absorbing by liquid caustic soda to prepare NaHS, and liquid purifies through toluene, obtains product vulcanization of rubber promotion
Agent M.High pressure product M contents 95.2%, 171.3 DEG C of purification captax just fusing point.
Embodiment 4
Using the device of embodiment 1, continuous synthetic rubber accelerator M：
Starting aniline measuring pump 1 makes aniline flow be 465g/h, is continuously pumped into aniline preheater 3, is drained into after being preheating to 200 DEG C
Autoclaves for synthesis 5.Starting molten sulphur liquid measuring pump 2 makes molten sulphur flow quantity be 580g/h, is continuously pumped into molten sulphur liquid preheater 4, preheating
Autoclaves for synthesis 5 is drained into after to 240 DEG C to be reacted.The heating system affiliated by autoclave is adjusted, controls Autoclaves for synthesis 5
Temperature is 240 DEG C, and synthesis pressure 9.0MPa, residence time of material 3.0 hours, row are controlled by the control pressurer system of discharging kettle 8
Entering to knockout drum 10, gas has absorbing by liquid caustic soda to prepare NaHS, and liquid purifies through soda acid, obtains product vulcanization of rubber promotion
Agent M.High pressure product M contents 93.0%, 172.3 DEG C of captax just fusing point after purification.
Embodiment 5
Using the device of embodiment 1, continuous synthetic rubber accelerator M：
Adjustment aniline measuring pump 1 makes aniline flow be 370L/h, is continuously pumped into aniline preheater 3, is drained into after being preheating to 200 DEG C
Autoclaves for synthesis 5.Adjusting molten sulphur liquid measuring pump 2 makes molten sulphur flow quantity be 382g/h, is continuously pumped into molten sulphur liquid preheater 4, preheating
Autoclaves for synthesis 5 is drained into after to 210 DEG C to be reacted.The heating system affiliated by autoclave is adjusted, controls Autoclaves for synthesis 5
Temperature is 250 DEG C, and synthesis pressure 9.0MPa, residence time of material 4.0 hours, row are controlled by the control pressurer system of discharging kettle 8
Enter to knockout drum 10, gas and purified by advanced claus oven Recovered sulphur, liquid through soda acid, obtain product vulcanization of rubber rush
Enter agent M.High pressure product M contents 92.4%, 171.0 DEG C of captax just fusing point after purification.
Embodiment 6
Using the device of embodiment 1, continuous synthetic rubber accelerator M：
Adjustment aniline measuring pump 1 makes aniline flow be 400L/h, is continuously pumped into aniline preheater 3, is drained into after being preheating to 260 DEG C
Autoclaves for synthesis 5.Adjusting molten sulphur liquid measuring pump 2 makes molten sulphur flow quantity be 410g/h, is continuously pumped into molten sulphur liquid preheater 4, preheating
Autoclaves for synthesis 5 is drained into after to 260 DEG C to be reacted.The heating system affiliated by autoclave is adjusted, controls Autoclaves for synthesis 5
Temperature is 260 DEG C, and synthesis pressure 9.5MPa, residence time of material 3.5 hours, row are controlled by the control pressurer system of discharging kettle 8
Enter to knockout drum 10, gas and purified by advanced claus oven Recovered sulphur, liquid through soda acid, obtain product vulcanization of rubber rush
Enter agent M.High pressure product M contents 92.2%, 172.0 DEG C of captax just fusing point after purification.
The present invention is described by way of example above, but the invention is not restricted to above-mentioned specific embodiment, it is all to be based on
Any changes or modifications that the present invention is done belong to the scope of protection of present invention.
Claims (8)
- A kind of 1. continuous synthesizer of rubber vulcanization accelerator M, it is characterised in that：Autoclaves for synthesis including no less than two and One discharging kettle, a knockout drum；The Autoclaves for synthesis, discharging kettle, knockout drum pass sequentially through discharge nozzle series connection； The Autoclaves for synthesis, discharging kettle upper end are connected by pressure-equalizing pipe；The Autoclaves for synthesis is connected to by pipeline Aniline preheater, molten sulphur liquid preheater, aniline preheater are connected with aniline measuring pump, and molten sulphur liquid preheater is connected with molten sulphur liquid meter Measure pump.
- 2. the continuous synthesizer of rubber vulcanization accelerator M according to claim 1, it is characterised in that：The high-pressure synthesis Kettle, discharging kettle and knockout drum are respectively equipped with temperature and pressure control system.
- 3. the continuous synthesizer of rubber vulcanization accelerator M according to claim 1, it is characterised in that：The high-pressure synthesis Kettle is provided with heating system.
- 4. the continuous synthesizer of rubber vulcanization accelerator M according to claim 3, it is characterised in that：The high-pressure synthesis The heating system that kettle is provided with is infrared heating, oil bath heating, the one or more of salt bath heating.
- 5. the production technology that rubber vulcanization accelerator M according to claim 1 continuously synthesizes, it is characterised in that：By aniline Aniline preheater is squeezed into by aniline measuring pump to be preheated, and molten sulphur liquid is squeezed into molten sulphur liquid preheater by molten sulphur liquid measuring pump Preheated, it is preheated after aniline and molten sulphur liquid be continuously driven into the Autoclaves for synthesis of series connection and reacted, go out after reaction End reaction material is drained into knockout drum and carries out continuous separation extraction by material kettle, and the gas of extraction carries out gas treatment, liquid Body carries out purification processes.
- 6. the continuous synthesizer of rubber vulcanization accelerator M according to claim 5 and its production technology, it is characterised in that： The molten sulphur liquid is that sulphur is dissolved in mixed liquor in carbon disulfide, and the mass ratio of sulphur and carbon disulfide is 1：2.1-2.4.
- 7. the continuous synthesizer of rubber vulcanization accelerator M according to claim 5 and its production technology, it is characterised in that： The aniline, carbon disulfide, sulphur mol ratio are：1：1.0-1.2：1.0-1.3.
- 8. the continuous synthesizer of rubber vulcanization accelerator M according to claim 5 and its production technology, it is characterised in that： Synthesis temperature is 160-280 DEG C, synthesis pressure 5.0-10MPa, small for 2.0-4.5 when reaction mass stops in synthesis reactor When.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108315552A (en) * | 2018-03-16 | 2018-07-24 | 中国恩菲工程技术有限公司 | Pressure leaching device |
| 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 |
| CN110862360A (en) * | 2019-10-18 | 2020-03-06 | 蔚林新材料科技股份有限公司 | Reaction system and method for continuously synthesizing rubber vulcanization accelerator dibenzothiazyl disulfide |
| CN112645899A (en) * | 2020-12-25 | 2021-04-13 | 蔚林新材料科技股份有限公司 | Green and clean process for continuously synthesizing 2-mercaptobenzothiazole |
| CN112920094A (en) * | 2021-01-29 | 2021-06-08 | 江苏奥洁生物科技有限公司 | Method for adjusting production load and improving yield of N-methyl sodium taurate |
| 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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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108315552A (en) * | 2018-03-16 | 2018-07-24 | 中国恩菲工程技术有限公司 | Pressure leaching device |
| 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 |
| CN110862360A (en) * | 2019-10-18 | 2020-03-06 | 蔚林新材料科技股份有限公司 | Reaction system and method for continuously synthesizing rubber vulcanization accelerator dibenzothiazyl disulfide |
| CN112645899A (en) * | 2020-12-25 | 2021-04-13 | 蔚林新材料科技股份有限公司 | Green and clean process for continuously synthesizing 2-mercaptobenzothiazole |
| CN112920094A (en) * | 2021-01-29 | 2021-06-08 | 江苏奥洁生物科技有限公司 | Method for adjusting production load and improving yield of N-methyl sodium taurate |
| 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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Application publication date: 20180126 |