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Method for producing refining M by calcium salt method

A production method, the technology of calcium salt method, is applied in the refining field of crude rubber vulcanization accelerator M (2-mercaptobenzothiazole), which can solve the problems of high COD, corrosion equipment, and low purity of M, so as to reduce pollution and Good corrosion and separation selectivity

Active Publication Date: 2014-09-03
SHANDONG SUNSINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The present invention uses cheap and easy-to-obtain calcium oxide or its hydroxide or a mixture of the two as a separating agent instead of high-concentration liquid caustic soda as a raw material, and overcomes the low purity of M, low yield, corrosion of equipment, large amount of waste water, and high COD Shortcomings

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  • Method for producing refining M by calcium salt method

Examples

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Comparison scheme
Effect test

Embodiment 1

[0025] Example 1: Take 63 grams of high-pressure synthetic crude product M, crush it, and the M content is 93%; the separating agent is 18 grams of calcium hydroxide, the main content (calcium hydroxide purity) is 90.5%, add 80 ml of water, and heat to 80-- React at 100°C for 1-2 hours, add 2000 ml of water to dilute and blast for about 1-2 hours; after solid-liquid separation, add 5--25% (wt.) hydrochloric acid to the clear liquid for full reaction, and control the end point to PH5-6; M was subjected to solid-liquid separation, washed with water and dried to obtain 58.2 g of M. The yield of crude product M is 92.38%.

Embodiment 2

[0026] Example 2: Take 63 grams of high-pressure synthetic crude product M, pulverize it, wherein the M content is 93%; take 15 grams of calcium hydroxide as the separating agent, the main content (calcium hydroxide purity) is 90.5%, add 80 milliliters of water, and heat up to 80-- React at 100°C for 1-2 hours, add 2000 ml of water to dilute and blast for about 1-2 hours; after solid-liquid separation, add 5--25% (wt.) hydrochloric acid to the clear liquid for full reaction, and control the end point to PH5-6; M was subjected to solid-liquid separation, washed with water, and dried to obtain 56.8 grams of M. The yield of crude product M is 90.16%.

Embodiment 3

[0027] Example 3: Take 63 grams of high-pressure synthetic crude product M, crush it, and the M content is 93%; take 14 grams of calcium oxide as the separating agent, the main content (calcium oxide purity) is 95.5%, add 90 ml of water, and heat to 80--100 ° C React for 1-2 hours, add 2000 ml of water to dilute and blast for about 1-2 hours; after solid-liquid separation, add 5--25% (wt.) hydrochloric acid to the clear liquid for full reaction, and control the end point pH5-6; Solid-liquid separation, washing with water, and drying gave 57.9 g of M. The yield of crude product M was 91.9%.

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Abstract

The invention provides a method for producing refining M by calcium salt method. The method includes that calcium oxides or calcium hydroxides or a mixture of the calcium oxides and the calcium hydroxides are used as water mixed emulsions of a separation agent and added into a crude product M, the molar ratio between the crude product M and the separation agent is 1 : (0.5-1.5), the mixture is subjected to reaction for 1-2 hours at the temperature between 40 DEG C and 100 DEG C and water is added for dilution; then, by means of blast air, calcium salts in impurities which are close to the properties of M in the crude product M are enabled preferentially to react with carbon dioxide in the blast air to produce calcium carbonate particles the impurities are free from the calcium salts, and under the action of air floatation of the blast air, the calcium carbonate particles and the free impurities are subjected to adsorption and aggregation and further to separation and purification; and a M calcium salt solution is subjected to still standing and then removed, a M calcium salt is neutralized by means of acidification, and dehydration and drying are performed to obtain the refining M. According to the production method of the refining M by the calcium salt method, the cheap and easily obtained calcium oxides or the calcium hydroxides or the mixture of the calcium oxides and the other hydroxides are used as the separation agent to substitute high concentration liquid caustic soda to serve as raw materials, so that the defects of device eroding and being low in purity of the M, low in yield, large in amount of waste water and high in chemical oxygen demand (COD) are overcome.

Description

technical field [0001] The invention relates to a rubber vulcanization accelerator, in particular to a method for refining a crude rubber vulcanization accelerator M (2-mercaptobenzothiazole). Background technique [0002] Rubber vulcanization accelerator M (2-mercaptobenzothiazole) is an important old variety of thiazole accelerators, and it is also the parent material for the synthesis of most sulfenamide accelerators, and its output occupies the first place among various rubber additives. Another use of M in the rubber industry is as a peptizer. Adding a small amount of M in the plasticizing process of natural rubber can greatly increase the plasticizing speed of raw rubber, and can also effectively prevent copper corrosion. It can also be used as a mineral Flotation agent, carrier resin, can also be used for the modification of epoxy resin, the pure product can be used as metal special reagent, and has a wide range of uses. However, the problem of "three wastes" of acce...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D277/72
Inventor 徐承秋刘经福赵峰苗静郭国强
Owner SHANDONG SUNSINE CHEM
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