CN107602748A - A kind of preparation method of 2 mercaptobenzothiazoler scarvenger - Google Patents
A kind of preparation method of 2 mercaptobenzothiazoler scarvenger Download PDFInfo
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- CN107602748A CN107602748A CN201710377919.6A CN201710377919A CN107602748A CN 107602748 A CN107602748 A CN 107602748A CN 201710377919 A CN201710377919 A CN 201710377919A CN 107602748 A CN107602748 A CN 107602748A
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- mercaptobenzothiazole
- scarvenger
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- mercaptobenzothiazoler
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- Thiazole And Isothizaole Compounds (AREA)
Abstract
The invention provides a kind of preparation method of 2 mercaptobenzothiazoler scarvenger：A certain amount of styrene is distributed in water, is proportionally added into dicyclopentadienyl, trimethoxy pentamethylcyclopentadiene base titanium, potassium peroxydisulfate and neopelex, 1, the alkene of 5,7 three azabicyclo [4.4.0] last of the ten Heavenly stems 5, benzyl vinyl ether, heating, reacted under preference temperature pressure, after reaction terminates, product filtering, drying, that is, obtain 2 mercaptobenzothiazoler purification adsorbents.
Description
Technical field
The present invention relates to a kind of purification process of 2-mercaptobenzothiazole, especially a kind of 2-mercaptobenzothiazole scarvenger
Preparation method.
Background technology
2-mercaptobenzothiazole is mainly used as the vulcanization accelerator of rubber（Captax）, agriculture chemicals fungicide is also served as, claims hydrogen
Sulphur agent or M agent.It can be used as corrosion inhibitor again.Sterling also serves as metal special reagent.Can by aniline, carbon disulfide and Sulfur,
Or carbon disulfide and rhenocure CA, or o-nitrochlorobenzene, NaHS and carbon disulfide synthesis.
CN1300123 discloses a kind of extracting process of 2-mercaptobenzothiazole, belongs to a kind of extraction process.The present invention
The technical issues that need to address are to provide a kind of extracting process of 2-mercaptobenzothiazole, its 2-mercaptobenzothiazole extracted
Purity is high and cost is low.The technical scheme is that a kind of extracting process of 2-mercaptobenzothiazole, (1) is by 1 part (weight)
2-mercaptobenzothiazole and 1-5 part toluene solutions are put into extraction kettle and stirred, until 2-mercaptobenzothiazole outer surface free from admixture
Untill, above-mentioned mixed liquor is put into suction filtration tank and filtered by (2), obtains filtrate and filter cake, and (3) obtain above-mentioned operation (2)
Filter cake is put into bipyramid rotary dryer, is dried under the conditions of vacuum is 0.02-0.08mpa and 80-120 DEG C, until filter cake
Heating loss it is qualified untill, that is, qualified 2-mercaptobenzothiazole product is made.
CN105061357A discloses a kind of process for purification of 2-mercaptobenzothiazole.2- sulfydryls benzene provided by the invention
And the process for purification of thiazole, 2-mercaptobenzothiazole is tied again with acetone using double solvents toluene and isopropanol or toluene
Crystalline substance purification, prepares 2-mercaptobenzothiazole highly finished product.
Existing 2-mercaptobenzothiazole purifies exquisite method a complex manufacturing mostly, to environment in production process
Caused by pollution it is big, the shortcomings that 2-mercaptobenzothiazole product purity is not high enough.
The content of the invention
The purpose of the present invention is：A kind of preparation method of 2-mercaptobenzothiazole scarvenger is provided, it can apply to 2-
In mercaptobenzothiazoler production, using this adsorbent, the 2-mercaptobenzothiazole product purity produced is high, and flow is simple, raw
It is few that waste is produced during production, is influenceed to caused by environment smaller.It is characterized in that preparation process includes：
A certain amount of styrene is distributed in water, dicyclopentadienyl, trimethoxy pentamethyl ring penta 2 are added in following ratios
Alkenyl titanium, potassium peroxydisulfate and neopelex, vinyl propionate, benzyl vinyl ether, heating, at 70-100 DEG C,
React 8-12 hours, product filtering, drying, that is, obtain 2-mercaptobenzothiazole scarvenger.
Ingredients weight parts
Styrene 100
Dicyclopentadienyl 1-5
Trimethoxy pentamethylcyclopentadiene base titanium 0.5-1.5
Potassium peroxydisulfate 0.5-1
Neopelex 0.5-1.5
The azabicyclos of 1,5,7- tri- [4.4.0] decyl- 5- alkene 0.5-2
Benzyl vinyl ether 0.5-1.5
Water 1000
Dicyclopentadienyl is commercially available prod, the product produced such as Zhangjiagang meter Xi Si photoelectric materials Co., Ltd；Trimethoxy five
Methyl cyclopentadienyl titanium is commercially available prod, the product produced such as Hubei Ju Sheng Co., Ltds；Neopelex is city
Product is sold, the product produced such as Shanghai Yan Sheng bio tech ltd；The azabicyclos of 1,5,7- tri- [4.4.0] decyl- 5- alkene is
Commercially available prod, the product produced such as Hubei Ju Sheng Co., Ltds；Benzyl vinyl ether is commercially available prod, as Hubei Holy Ghost's science and technology has
The product of limit company production.
The product of the present invention has the advantages that：
Introduce dicyclopentadienyl, trimethoxy pentamethylcyclopentadiene base titanium, 1,5,7- tri- azabicyclo [4.4.0] decyl- 5-
As polymerized monomer, the chemical stability and heat endurance for making adsorbent product greatly enhance alkene, this adsorbent product absorption speed
Degree is fast, and adsorbing contaminant amount is big, and the waste water waste material caused by 2-mercaptobenzothiazole that puts into production is few, the 2- sulfydryl benzo thiophenes of output
Azoles product purity is high.
Embodiment
Following instance is only to further illustrate the present invention, is not limitation the scope of protection of the invention.
Embodiment 1
1000Kg water, 100Kg styrene, 3Kg dicyclopentadienyls, 1Kg trimethoxy pentamethyl rings are added in 2000L reactors
Pentadienyl titanium, 0.8Kg potassium peroxydisulfates, 1Kg neopelexes, 1.5Kg1,5,7- tri- azabicyclo [4.4.0] decyl-s
5- alkene, 1Kg benzyl vinyl ethers, 80 DEG C are warming up to, react 10h, product filtering, drying, that is, obtain 2-mercaptobenzothiazole and carry
It is pure to use adsorbent.
Embodiment 2
1000Kg water, 100Kg styrene, 1Kg dicyclopentadienyls, 0.5Kg trimethoxy pentamethyls are added in 2000L reactors
Cyclopentadienyltitanium, 0.5Kg potassium peroxydisulfates, 0.5Kg neopelexes, 0.5Kg1,5,7- tri- azabicyclos [4.4.0]
Decyl- 5- alkene, 0.5Kg benzyl vinyl ethers, 70 DEG C are warming up to, react 8h, product filtering, drying, that is, obtain 2- sulfydryl benzo thiophenes
Azoles scarvenger.
Embodiment 3
1000Kg water, 100Kg styrene, 5Kg dicyclopentadienyls, 1.5Kg trimethoxy pentamethyls are added in 2000L reactors
Cyclopentadienyltitanium, 1Kg potassium peroxydisulfates, 1.5Kg neopelexes, 2Kg1,5,7- tri- azabicyclo [4.4.0] decyl-s
5- alkene, 1.5Kg benzyl vinyl ethers, 100 DEG C are warming up to, react 12h, product filtering, drying, that is, obtain 2-mercaptobenzothiazole
Scarvenger.
Comparative example 1
Dicyclopentadienyl is added without, other conditions are the same as embodiment 1.
Comparative example 2
Trimethoxy pentamethylcyclopentadiene base titanium is added without, other conditions are the same as embodiment 1.
Comparative example 3
1,5,7- tri- azabicyclo [4.4.0] decyl- 5- alkene are added without, other conditions are the same as embodiment 1.
Comparative example 4
Benzyl vinyl ether is added without, other conditions are the same as embodiment 1.
Embodiment 4
The 2-mercaptobenzothiazole crude product of weight/mass percentage composition 97% or so is passed through equipped with this patent embodiment 1-3 and right
2-mercaptobenzothiazole scarvenger 500g prepared by ratio 1-4 1000ml exchange columns, temperature 60 C, flow velocity 0.5BV/h, use gas
Phase chromatogram detects the weight/mass percentage composition of efflux, is shown in Table 1.
Table 1：The purity of 2-mercaptobenzothiazole product after the adsorbent absorption purification that different process is produced.
Claims (3)
- A kind of 1. preparation method of 2-mercaptobenzothiazole scarvenger, it is characterised in that it is raw materials used including：Ingredients weight partsStyrene 100Dicyclopentadienyl 1-5Trimethoxy pentamethylcyclopentadiene base titanium 0.5-1.5Potassium peroxydisulfate 0.5-1Neopelex 0.5-1.5The azabicyclos of 1,5,7- tri- [4.4.0] decyl- 5- alkene 0.5-2Benzyl vinyl ether 0.5-1.5Water 1000.
- A kind of 2. preparation method of 2-mercaptobenzothiazole scarvenger according to claim 1, it is characterised in that preparation side The reaction temperature of method is：70-100℃.
- A kind of 3. preparation method of 2-mercaptobenzothiazole scarvenger according to claim 1, it is characterised in that preparation side The reaction time of method is 8-12 hours.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106188373A (en) * | 2016-08-21 | 2016-12-07 | 王金桢 | A kind of preparation method of 2 mercaptobenzothiazoler purification adsorbents |
| CN106220773A (en) * | 2016-08-21 | 2016-12-14 | 王金桢 | A kind of preparation method of L tryptophan purification adsorbent |
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2017
- 2017-05-25 CN CN201710377919.6A patent/CN107602748A/en not_active Withdrawn
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106188373A (en) * | 2016-08-21 | 2016-12-07 | 王金桢 | A kind of preparation method of 2 mercaptobenzothiazoler purification adsorbents |
| CN106220773A (en) * | 2016-08-21 | 2016-12-14 | 王金桢 | A kind of preparation method of L tryptophan purification adsorbent |
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Application publication date: 20180119 |