CN104592158A - Preparation method of rubber promoter N-cyclohexyl-2-benzothiazole sulfonamide - Google Patents
Preparation method of rubber promoter N-cyclohexyl-2-benzothiazole sulfonamide Download PDFInfo
- Publication number
- CN104592158A CN104592158A CN201310520640.0A CN201310520640A CN104592158A CN 104592158 A CN104592158 A CN 104592158A CN 201310520640 A CN201310520640 A CN 201310520640A CN 104592158 A CN104592158 A CN 104592158A
- Authority
- CN
- China
- Prior art keywords
- cyclohexyl
- preparation
- mercaptobenzothiazole
- benzothiazole sulfonamide
- cyclohexylamine
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
- C07D277/76—Sulfur atoms attached to a second hetero atom
- C07D277/80—Sulfur atoms attached to a second hetero atom to a nitrogen atom
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Thiazole And Isothizaole Compounds (AREA)
Abstract
The invention discloses a preparation method of rubber promoter N-cyclohexyl-2-benzothiazole sulfonamide. The preparation method comprises following steps: step 1, crude 2-mercaptobenzothiazole and cyclohexylamine with a mass concentration of 25% are delivered into a reaction kettle at a mass ratio of 1:2.5, an obtained mixture is stirred and heated until complete dissolving is realized, and is cooled to 45 DEG C, and sodium hypochlorite is added dropwise for 1.5h; and step 2, an obtained mixed material is subjected to cooling, and pump filtration, impurities are removed via washing with cyclohexylamine aqueous solution, an obtained product is washed with water, and obtained filter cake is dried so as to obtain N-cyclohexyl-2-benzothiazole sulfonamide. According to the preparation method of rubber promoter N-cyclohexyl-2-benzothiazole sulfonamide, technology is simple, refining of crude 2-mercaptobenzothiazole is avoided, production cost is reduced greatly, and sewage discharge is reduced.
Description
Technical field
The present invention relates to a kind of preparation method of rubber accelerator, be specifically related to a kind of preparation method of N cyclohexyl 2 benzothiazole sulfenamide.
Background technology
N cyclohexyl 2 benzothiazole sulfenamide is a kind of conventional delayed action accelerator, has scorching quality good, and vulcanization rate is fast, process safety, the advantages such as curing time is short, is mainly used in making tire, rubber overshoes, sebific duct, adhesive tape etc.The smart 2-mercaptobenzothiazole of industrial main employing and hexahydroaniline oxidative condensation produce N cyclohexyl 2 benzothiazole sulfenamide, but the operation environmental pollution producing smart 2-mercaptobenzothiazole is serious, and production cost is high; The selectivity that extraction process produces smart 2-mercaptobenzothiazole is low, and the residue reclaimed after toluene contains relatively large 2-mercaptobenzothiazole, and energy consumption is large, complex procedures.
Summary of the invention
The object of the invention is to, provide a kind of preparation method of rubber accelerator N cyclohexyl 2 benzothiazole sulfenamide, technique is simple, and product yield is high, reduces production cost, reduces sewage discharge.
The preparation method of described rubber accelerator N cyclohexyl 2 benzothiazole sulfenamide, it comprises the following steps:
One, to be the thick 2-mercaptobenzothiazole of 1:2.5 and massfraction by mass ratio be 25% hexahydroaniline drop in reactor, stir and be warming up to whole dissolving, be cooled to 45 DEG C, drip clorox, 1.5h dropwises;
Two, cool, suction filtration also washes away impurity with Aqueous Solution of Cyclohexylamine, and wash with water, namely dry cake obtains N cyclohexyl 2 benzothiazole sulfenamide.
The preparation method of rubber accelerator N cyclohexyl 2 benzothiazole sulfenamide provided by the invention, its beneficial effect is, technique is simple, eliminates the refining step of thick 2-mercaptobenzothiazole, significantly reduces production cost, decrease sewage discharge.
Embodiment
Below in conjunction with an embodiment, the preparation method of rubber accelerator N cyclohexyl 2 benzothiazole sulfenamide provided by the invention is described in detail.
Embodiment
One, to be the thick 2-mercaptobenzothiazole of 1:2.5 and massfraction by mass ratio be 25% hexahydroaniline drop in reactor, stir and be warming up to whole dissolving, be cooled to 45 DEG C, drip clorox, 1.5h dropwises;
Two, cool, suction filtration also washes away impurity with Aqueous Solution of Cyclohexylamine, and wash with water, namely dry cake obtains N cyclohexyl 2 benzothiazole sulfenamide.
Claims (1)
1. a preparation method for rubber accelerator N cyclohexyl 2 benzothiazole sulfenamide, is characterized in that: it comprises the following steps:
One, to be the thick 2-mercaptobenzothiazole of 1:2.5 and massfraction by mass ratio be 25% hexahydroaniline drop in reactor, stir and be warming up to whole dissolving, be cooled to 45 DEG C, drip clorox, 1.5h dropwises;
Two, cool, suction filtration also washes away impurity with Aqueous Solution of Cyclohexylamine, and wash with water, namely dry cake obtains N cyclohexyl 2 benzothiazole sulfenamide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310520640.0A CN104592158A (en) | 2013-10-30 | 2013-10-30 | Preparation method of rubber promoter N-cyclohexyl-2-benzothiazole sulfonamide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310520640.0A CN104592158A (en) | 2013-10-30 | 2013-10-30 | Preparation method of rubber promoter N-cyclohexyl-2-benzothiazole sulfonamide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104592158A true CN104592158A (en) | 2015-05-06 |
Family
ID=53118262
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310520640.0A Pending CN104592158A (en) | 2013-10-30 | 2013-10-30 | Preparation method of rubber promoter N-cyclohexyl-2-benzothiazole sulfonamide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104592158A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106800540A (en) * | 2017-03-30 | 2017-06-06 | 山东斯递尔化工科技有限公司 | A kind of method that utilization micro passage reaction prepares rubber vulcanizing accelerator CBS |
| CN108727301A (en) * | 2017-10-23 | 2018-11-02 | 科迈化工股份有限公司 | A kind of synthesis technology of vulcanization accelerator N cyclohexyl 2 benzothiazole sulfenamide |
| CN110305075A (en) * | 2019-07-11 | 2019-10-08 | 聊城大学 | A kind of method of Co catalysts oxygen method synthesis N cyclohexyl 2 benzothiazole sulfenamide |
-
2013
- 2013-10-30 CN CN201310520640.0A patent/CN104592158A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106800540A (en) * | 2017-03-30 | 2017-06-06 | 山东斯递尔化工科技有限公司 | A kind of method that utilization micro passage reaction prepares rubber vulcanizing accelerator CBS |
| CN108727301A (en) * | 2017-10-23 | 2018-11-02 | 科迈化工股份有限公司 | A kind of synthesis technology of vulcanization accelerator N cyclohexyl 2 benzothiazole sulfenamide |
| CN110305075A (en) * | 2019-07-11 | 2019-10-08 | 聊城大学 | A kind of method of Co catalysts oxygen method synthesis N cyclohexyl 2 benzothiazole sulfenamide |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105524014B (en) | Purification method of rubber vulcanization accelerator 2-mercaptobenzothiazole | |
| CN102863567B (en) | Preparation method of polyvinyl alcohol through low-alkali method | |
| CN101891683B (en) | Aminopyrine production method | |
| CN103849017B (en) | A kind of preparation method of whole-tyre reclaim | |
| CN101108834A (en) | Method of refining rubber vulcanization accelerant MBT | |
| CN104592158A (en) | Preparation method of rubber promoter N-cyclohexyl-2-benzothiazole sulfonamide | |
| CN104262200A (en) | Production method for preparing N,N'-dicyclohexylcarbodiimide (DCC) by recycling wastewater | |
| CN103058899B (en) | Synthetic method for methyl-sulfuryl benzaldehyde | |
| CN103102326A (en) | Preparation method of rubber accelerator NOBS (N-(oxidiethylene)-2-benzothiazolyl sulfenamide) | |
| CN102838562A (en) | Method for synthesizing rubber vulcanization accelerator NS (N-tertiary butyl-2-benzothiazole sulfenamide) through two-step method by taking hydrogen peroxide as oxidant | |
| CN103524450A (en) | Synthetic method for accelerator DZ by using methanol as solvent | |
| CN102850294A (en) | Method for synthesizing rubber vulcanizing promoter CZ (N-cyclohexylbenzothiazole-2-sulphenamide) via two-step process by using hydrogen peroxide as oxidant | |
| CN102775443B (en) | The synthetic method of Chlorpyrifos 94 | |
| CN102838561A (en) | Production method of rubber vulcanization accelerator NS (N-tertiary butyl-2-benzothiazole sulfenamide) | |
| CN104311506A (en) | Synthetic process of rubber vulcanization accelerator CBS | |
| CN104592040A (en) | Preparation method of rubber antioxidant p-phenylenediamine | |
| CN101899020A (en) | DZ synthesized by mixing mother solution | |
| CN103539757A (en) | Method for synthesizing rubber vulcanization accelerator CZ | |
| CN103508977A (en) | Method for producing rubber vulcanization accelerator CZ by adopting double-dripping method using hydrogen peroxide as oxidizing agent | |
| CN103508978A (en) | Method for producing rubber vulcanization accelerator CZ with two-dropping method | |
| CN101475168B (en) | Method for washing active carbon | |
| CN102952074A (en) | Method of recycling dextromethorphan from crystallization mother liquor | |
| CN105622481A (en) | Process for efficient synthesis of 5-bromoindole | |
| WO2014183381A1 (en) | Method for caustic purification of silicon carbide filter cake | |
| CN104592155A (en) | Preparation method of rubber promoter 2,2'-dithiobis(benzothiazole) |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20150506 |