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Method for preparing high-purity accelerant CZ through purification, and application of high-purity accelerant CZ

A kind of accelerator, high-purity technology, applied in the field of purifying and preparing high-purity accelerator CZ, high-purity and chromatographic-grade purity accelerator CZ, can solve the problems of residue, the structure is not particularly stable, the solubility is general, etc., and the purification process is fast. , Conducive to drying, high purity effect

Active Publication Date: 2021-06-25
BEIJING RED AVENUE INNOVA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are following deficiencies in this method: 1, select toluene as solvent for use, and add gac adsorption impurity
On the one hand, this step artificially introduces activated carbon, which brings new risks of impurities; on the other hand, the solvent of impurities in the hot toluene solution is very good, and the effect of filtration and crystallization is not good, and the effect of removing by-products is not achieved.
2. The solubility of toluene crystals in hot methanol is average, so the effect of recrystallization using methanol temperature difference is also average, and it cannot achieve better results
3. The structure of the accelerator CZ itself is not particularly stable, and it is easy to partially decompose in an organic solvent at a temperature of 50°C for a long time to form the accelerator DM. In addition, due to the high boiling point of toluene solvent, drying at low temperature will cause damage to the product. There are remnants

Method used

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  • Method for preparing high-purity accelerant CZ through purification, and application of high-purity accelerant CZ
  • Method for preparing high-purity accelerant CZ through purification, and application of high-purity accelerant CZ
  • Method for preparing high-purity accelerant CZ through purification, and application of high-purity accelerant CZ

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] At normal temperature, add 150g slightly light yellow commercially available CZ (manufactured by Kemai, with a purity of 98.4%), 50g tetrahydrofuran, and 2g cyclohexylamine into a 500ml reaction flask equipped with a stirring device, a thermometer and a reflux condenser, and stir for 10min. Rapidly raise the temperature to 50°C, until all impurities visible to the naked eye are dissolved in tetrahydrofuran, and some CZ are not completely dissolved. Quickly cool down to 5°C in the ice-water mixture, add 70g of absolute ethanol, stir for 1min, transfer the mixture to a sand core funnel, filter with suction, and dry in vacuum at 35°C for 5h to obtain 115g of CZ in the form of white crystals. The product is chromatographed by HPLC Test, the area normalization method peak area is 99.49%.

[0056] Take 100g of CZ purified once, and purify once again according to the above-mentioned material addition ratio and operation steps to obtain 75g of purified CZ. The product is tested...

Embodiment 2

[0058] At normal temperature, 150g slightly light yellow commercially available CZ (manufactured by Kemai, with a purity of 98.4%), 35g tetrahydrofuran, and 0.8g cyclohexylamine were added to a 500ml reaction flask equipped with a stirring device, a thermometer and a reflux condenser, and stirred Rapidly raise the temperature to 55°C within 10 minutes until all impurities visible to the naked eye are dissolved in tetrahydrofuran, and part of CZ is not completely dissolved. Quickly cool down to 5°C in the ice-water mixture, add 80g of absolute ethanol, stir for 1min, transfer the mixture to a sand core funnel, filter it with suction, and dry it in vacuum at 35°C for 5h to obtain 120g of CZ in the form of white crystals. The product was analyzed by HPLC Chromatography test, the area normalization method peak area is 99.40%, almost does not contain DM peak in the product.

Embodiment 3

[0060] Step 1: Preparation of accelerator CZ (water phase method)

[0061] Add 83.5g (0.5mol) of accelerator M, 178g (1.8mol) of cyclohexylamine, 0.6g of copper sulfate, and 500g of distilled water into a 1000ml reaction flask equipped with a stirring device, a thermometer and a reflux condenser, and stir evenly; 68g (0.6mol) of 30% hydrogen peroxide, reaction temperature 40°C; hydrogen peroxide was added dropwise for 90 minutes, cooled to 20°C after the reaction, settled, filtered, and dried at 40°C for 12 hours to obtain 117g of dark yellow CZ crude product, which was chromatographed by HPLC According to the curve test, the purity is 92.7%.

[0062] Step 2: Purification of Accelerator CZ

[0063] At room temperature, take 100g of CZ made in step 1, 50g of tetrahydrofuran, and 1.2g of cyclohexylamine into a 500ml reaction bottle equipped with a stirring device, a thermometer and a reflux condenser, and rapidly raise the temperature to 45°C within 10 minutes under stirring, u...

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Abstract

The invention discloses a method for preparing a high-purity accelerant CZ through purification, and application of the high-purity accelerant CZ. The method for preparing the high-purity accelerant CZ through purification uses tetrahydrofuran and absolute ethyl alcohol as solvents and cyclohexylamine as an inhibitor for resisting decomposition of the accelerant CZ. The method comprises the following steps: 1) mixing the coarse accelerant CZ, the tetrahydrofuran and the cyclohexylamine at normal temperature, rapidly heating a formed system in a stirring state to enable the system to be in a completely or partially dissolved state, and then rapidly cooling the system; and 2) keeping a cooling temperature, adding absolute ethyl alcohol, carrying out suction filtration, and conducting drying to obtain the high-purity accelerant CZ. According to the method, an accelerator CZ product with high-grade purity can be obtained through one-time purification, technological operation is simple and rapid, new impurities cannot be introduced, and purification effect is good.

Description

technical field [0001] The present invention relates to the purification process field of rubber accelerators, in particular, it relates to a method for purifying and preparing high-purity accelerator CZ and its application, utilizing the solubility difference of accelerator CZ at different temperatures and in different solvents to quickly Purify to obtain high-purity and chromatographic-grade purity accelerator CZ. Background technique [0002] N-cyclohexyl-2-benzothiazole sulfenamide (accelerator CBS or CZ), the English name is N-Cyclohexyl-2-Benzothiazole Sulphenamide, which is a kind of sulfenamide latex widely used at home and abroad with excellent comprehensive performance. Effective rubber vulcanization accelerator, mainly used in the manufacture of industrial rubber products such as tires, rubber hoses, rubber shoes, and wires. [0003] Usually, the accelerator CZ is prepared by reacting the accelerator M (2-mercaptobenzothiazole) with 2 to 4 molar equivalents of cy...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D277/80
CPCC07D277/80
Inventor 张洁阮振刚胡小娜张成董栋张宁
Owner BEIJING RED AVENUE INNOVA
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