CN104672173A - Production method of rubber accelerator TBBS (N-tert-butyl-2-benzothiazolesulfenamide) - Google Patents

Abstract

The invention relates to a production method of a rubber accelerator TBBS (N-tert-butyl-2-benzothiazolesulfenamide), which comprises the following steps: reacting liquid caustic soda and chlorine to generate sodium hypochlorite, injecting a prepared MBT (2-mercaptobenzthiazole) slurry into an oxidizing reaction kettle, starting stirring, adding tert-butylamine and sulfuric acid, stirring for 10 minutes, dropwisely adding sodium hypophosphite until the reaction end point, recovering the mother solution and water washing solution, and carrying out flash drying on the material to obtain the accelerator TBBS. The method can effectively enhance the yield and purity of the accelerator TBBS and improve the quality of product, so that the quality of the rubber product produced by the accelerator is enhanced.

Description

A kind of production method of rubber accelerator TBBS

(1) technical field

The present invention relates to a kind of rubber accelerator production method, particularly relate to a kind of production method of rubber accelerator TBBS.

(2) background technology

At present, rubber accelerator TBBS is universal promotor, is widely used in various Rubber & Rubber Products, especially for the processing of radial, has advantages such as " imitating late at a high speed ".。But present accelerator TBBS production technique Shortcomings, output generally rests on about 93%, purity about 92%, has had influence on the rubber product quality using this promotor to produce.Effectively can improve productive rate and the purity of accelerator TBBS on the market, improve the quality of products, thus the rubber accelerator production method that the rubber product quality that this promotor of use is produced rises also is not found, and awaits exploitation.

(3) summary of the invention

In order to overcome the weak point of existing rubber accelerator working method, the invention provides a kind of production method of rubber accelerator TBBS.

Technical scheme of the present invention realizes like this.

The production method of a kind of rubber accelerator TBBS of this programme, concrete steps are as follows:

(1) clorox operation

Close sodium hypochlorite reaction still blowing section door, the alkali lye alkali of alkalinity 24.5 ~ 25.5g/100ml is put into sodium hypochlorite reaction still, open and stir, open the cold cooling of chuck, reaction process observes temperature variation at any time, control temperature of reaction 0 ~ 30 DEG C, chlorine is closed immediately close to 30 DEG C, logical chlorine is continued after temperature lowers, according to the logical chlorine dose of estimation, slowly chlorine will be led to when closing on terminal, and sampling analysis in advance, until reach available chlorine content 18.3 ~ 18.8g/100ml in chlorine bleach liquor, after free alkali content 0.9 ~ 1.2g/100ml, stop passing into chlorine, stop stirring and cooling,

(2) oxidation operation

The MBT slurry got ready is squeezed into stills for air blowing and opened stirring, closes stills for air blowing section door, add 25% sulfuric acid of 590kg TERTIARY BUTYL AMINE and 120L to reactor;

Clorox step one configured is shown by header tank liquidometer and flow control, adds speed control at 800-900L/h, and add 1050L is 300-400L/h later, and begin to cool down after still temperature rise to 40 DEG C, temperature controls at 35-50 DEG C;

Clorox consumption to continuing during 1050L to drip clorox, and starts to use ammonium sulfate, potassiumiodide, starch mixed solution to survey terminal, stops adding clorox after reaching home, and continues stirring and rechecks confirmation terminal again after 5 minutes;

Add the 10% S-WAT terminator of 10L after confirming terminal, stir 30% sodium hydroxide adding 60L after 5 minutes and continue stirring ten minutes, temperature is down to 40 DEG C of dischargings, material is transferred to transfer tank;

(3) washing dries operation

First transfer tank material is squeezed into horizontal type scraper centrifuger to be purified by mother liquor, then add water and wash, water lotion pH value is 1 ~ 7.5, and in whizzer, material is wanted evenly, observes visor and is as the criterion without water droplet, to be drained off complete after, the material after drying is put into wet feed groove;

(4) air stream drying operation

Blow in machine; Open air compressor machine and dedusting blowback; Open steam, computer heating control inlet temperature 90-100 DEG C, drive glassware into and modulate suitable rotating speed, when moisture is down to 1 ~ 3%, open front warehouse discharging; Open rear warehouse discharging, collection can obtain product.

Usefulness of the present invention is: present method effectively can improve productive rate and the purity of accelerator TBBS, improves the quality of products, thus the rubber product quality that this promotor of use is produced rises.

(4) embodiment

Embodiment 1

(1) clorox operation

Close sodium hypochlorite reaction still blowing section door, the alkali lye alkali of alkalinity 249g/100ml is put into sodium hypochlorite reaction still, open and stir, open the cold cooling of chuck, reaction process observes temperature variation at any time, control temperature of reaction 25 DEG C, chlorine is closed immediately close to 30 DEG C, after temperature lowers, continue logical chlorine, according to the logical chlorine dose of estimation, when closing on terminal, slowly will lead to chlorine, and sampling analysis in advance, until after reaching available chlorine content 18.5g/100ml in chlorine bleach liquor, free alkali content 1.1g/100ml, stop passing into chlorine, stop stirring and cooling;

(2) oxidation operation

The MBT slurry got ready is squeezed into stills for air blowing and opened stirring, closes stills for air blowing section door, add 25% sulfuric acid of 590kg TERTIARY BUTYL AMINE and 120L to reactor;

Clorox step one configured is shown by header tank liquidometer and flow control, adds speed control at 880L/h, and add 1050L is 350L/h later, and begin to cool down after still temperature rise to 40 DEG C, temperature controls at 40 DEG C;

Clorox consumption to continuing during 1050L to drip clorox, and starts to use ammonium sulfate, potassiumiodide, starch mixed solution to survey terminal, stops adding clorox after reaching home, and continues stirring and rechecks confirmation terminal again after 5 minutes;

Add the 10% S-WAT terminator of 10L after confirming terminal, stir 30% sodium hydroxide adding 60L after 5 minutes and continue stirring ten minutes, temperature is down to 40 DEG C of dischargings, material is transferred to transfer tank;

(3) washing dries operation

First transfer tank material is squeezed into horizontal type scraper centrifuger to be purified by mother liquor, then add water and wash, water lotion pH value is 7, and in whizzer, material is wanted evenly, observes visor and is as the criterion without water droplet, to be drained off complete after, the material after drying is put into wet feed groove;

(4) air stream drying operation

Blow in machine; Open air compressor machine and dedusting blowback; Open steam, computer heating control inlet temperature 95 DEG C, drive glassware into and modulate suitable rotating speed, when moisture is down to 3%, open front warehouse discharging; Open rear warehouse discharging, collection can obtain product.

The accelerator TBBS purity 98% that this method is made, output 97%, effective productive rate and the purity improving accelerant MBT S, improves the quality of products, thus the rubber product quality that this promotor of use is produced rises.

Above one embodiment of the present of invention have been described in detail, but described content being only preferred embodiment of the present invention, can not being considered to for limiting practical range of the present invention.All equalizations done according to the present patent application scope change and improve, and all should still belong within patent covering scope of the present invention.

Claims (2)

1. a production method for rubber accelerator TBBS, is characterized in that: concrete steps are as follows:

(1) clorox operation

Close sodium hypochlorite reaction still blowing section door, the alkali lye alkali of alkalinity 24.5 ~ 25.5g/100ml is put into sodium hypochlorite reaction still, open and stir, open the cold cooling of chuck, reaction process observes temperature variation at any time, control temperature of reaction 0 ~ 30 DEG C, chlorine is closed immediately close to 30 DEG C, logical chlorine is continued after temperature lowers, according to the logical chlorine dose of estimation, slowly chlorine will be led to when closing on terminal, and sampling analysis in advance, until reach available chlorine content 18.3 ~ 18.8g/100ml in chlorine bleach liquor, after free alkali content 0.9 ~ 1.2g/100ml, stop passing into chlorine, stop stirring and cooling,

(2) oxidation operation

The MBT slurry got ready is squeezed into stills for air blowing and opened stirring, closes stills for air blowing section door, add 25% sulfuric acid of 590kg TERTIARY BUTYL AMINE and 120L to reactor;

Clorox step one configured is shown by header tank liquidometer and flow control, adds speed control at 800-900L/h, and add 1050L is 300-400L/h later, and begin to cool down after still temperature rise to 40 DEG C, temperature controls at 35-50 DEG C;

Clorox consumption to continuing during 1050L to drip clorox, and starts to use ammonium sulfate, potassiumiodide, starch mixed solution to survey terminal, stops adding clorox after reaching home, and continues stirring and rechecks confirmation terminal again after 5 minutes;

Add the 10% S-WAT terminator of 10L after confirming terminal, stir 30% sodium hydroxide adding 60L after 5 minutes and continue stirring ten minutes, temperature is down to 40 DEG C of dischargings, material is transferred to transfer tank;

(3) washing dries operation

First transfer tank material is squeezed into horizontal type scraper centrifuger to be purified by mother liquor, then add water and wash, water lotion pH value is 1 ~ 7.5, and in whizzer, material is wanted evenly, observes visor and is as the criterion without water droplet, to be drained off complete after, the material after drying is put into wet feed groove;

(4) air stream drying operation

Blow in machine; Open air compressor machine and dedusting blowback; Open steam, computer heating control inlet temperature 90-100 DEG C, drive glassware into and modulate suitable rotating speed, when moisture is down to 1 ~ 3%, open front warehouse discharging; Open rear warehouse discharging, collection can obtain product.

2. the production method of a kind of rubber accelerator TBBS according to claim 1, is characterized in that: concrete steps are as follows:

(1) clorox operation

Close sodium hypochlorite reaction still blowing section door, the alkali lye alkali of alkalinity 249g/100ml is put into sodium hypochlorite reaction still, open and stir, open the cold cooling of chuck, reaction process observes temperature variation at any time, control temperature of reaction 25 DEG C, chlorine is closed immediately close to 30 DEG C, after temperature lowers, continue logical chlorine, according to the logical chlorine dose of estimation, when closing on terminal, slowly will lead to chlorine, and sampling analysis in advance, until after reaching available chlorine content 18.5g/100ml in chlorine bleach liquor, free alkali content 1.1g/100ml, stop passing into chlorine, stop stirring and cooling;

(2) oxidation operation

The MBT slurry got ready is squeezed into stills for air blowing and opened stirring, closes stills for air blowing section door, add 25% sulfuric acid of 590kg TERTIARY BUTYL AMINE and 120L to reactor;

Clorox step one configured is shown by header tank liquidometer and flow control, adds speed control at 880L/h, and add 1050L is 350L/h later, and begin to cool down after still temperature rise to 40 DEG C, temperature controls at 40 DEG C;

Clorox consumption to continuing during 1050L to drip clorox, and starts to use ammonium sulfate, potassiumiodide, starch mixed solution to survey terminal, stops adding clorox after reaching home, and continues stirring and rechecks confirmation terminal again after 5 minutes;

Add the 10% S-WAT terminator of 10L after confirming terminal, stir 30% sodium hydroxide adding 60L after 5 minutes and continue stirring ten minutes, temperature is down to 40 DEG C of dischargings, material is transferred to transfer tank;

(3) washing dries operation

First transfer tank material is squeezed into horizontal type scraper centrifuger to be purified by mother liquor, then add water and wash, water lotion pH value is 7, and in whizzer, material is wanted evenly, observes visor and is as the criterion without water droplet, to be drained off complete after, the material after drying is put into wet feed groove;

(4) air stream drying operation

Blow in machine; Open air compressor machine and dedusting blowback; Open steam, computer heating control inlet temperature 95 DEG C, drive glassware into and modulate suitable rotating speed, when moisture is down to 3%, open front warehouse discharging; Open rear warehouse discharging, collection can obtain product.