CN102285939A - Method for preparing accelerator TBBS (N-tert-butylbenzothiazole-2-sulphenamide) - Google Patents

Abstract

The invention relates to a method for preparing accelerator TBBS (N-tert-butylbenzothiazole-2-sulphenamide). The method comprises the following steps of: adding an accelerator M of 32.5 to water of 100ml, adding a peregal dispersing agent of 2ml and concentration of 7%, supplementing the water or a mother solution to be total 125ml to prepare accelerator M slurry, and placing in a vessel for later use; putting sodium hypochlorite of 100ml including available chlorine of 18.4-18.6g/100ml and free alkali of 0.8-1g/100ml into the vessel for later use; adding tertbutylamine into a 300ml reaction vessel, wherein the mole ratio of tertbutylamine total amount to accelerator total amount is 1.06:1; stirring till the temperature is increased to 43-45 DEG C; and adding the accelerator M of 5ml as a base material, and dropwise adding the accelerator M slurry in the step (1) and the sodium hypochlorite in the step (2) based on volume ratio of 5:3, wherein the dropwire adding needs to be finished within 45-55min, and the temperature during dropwise adding can not be higher than 45 DEG C. According to the method disclosed by the invention, the recovery and the distillation of the mother liquid are not needed, thus the amount of drained waste water is reduced, the cost is reduced, economical and environment-friendly properties are owned, and each technical index of products matches the national standard.

Description

The production method of accelerator N-tertiary butyl-2-[4-morpholinodithio sulphenamide

Technical field

The invention relates to the novel method of accelerator NS (N tert butyl benzothiazole 2 sulfenamide) (english abbreviation is TBBS) explained hereafter, belong to the rubber accelerator production technical field.

Background technology

Accelerator NS (TBBS) is a kind of safe accelerator, is applicable to natural rubber, cis-1,4-polybutadiene rubber, different the eleventh of the twelve Earthly Branches rubber, styrene-butadiene rubber(SBR) and natural rubber reclaimed rubber, and is as safe as a house under service temperature.Domestic main production method has hypochlorite oxidation method and hydrogen peroxide oxidation method at present, two kinds of methods all adopt the excessive additive process of TERTIARY BUTYL AMINE, being about to quantitative captax (2-thiol benzothiazole) and excessive TERTIARY BUTYL AMINE drops in the reactor, under the effect of oxygenant, generate accelerator NS, the mol ratio of captax and TERTIARY BUTYL AMINE is general to adopt 1: 2.7～3, because TERTIARY BUTYL AMINE is excessive more, when aftertreatment, need the mother liquor recovery is distilled, promptly increase wastewater flow rate and increased production cost again.

Summary of the invention

In order to solve prior art problems, we have carried out research experiment, and proposed new accelerator NS production method: technical scheme of the present invention is as follows:

The production method of a kind of accelerator N-tertiary butyl-2-[4-morpholinodithio sulphenamide, step is as follows:

1) the 32.5g captax is added in the 100ml water, adding 2 ml concns again is that 7% peregal dispersion agent amounts to 125ml, and make up water or mother liquor are made the captax slurry to 125ml, the containers for future use of packing into;

2) the clorox 100ml of available chlorine 18.4-18.6g/100ml, free alkali 0.8-1g/100ml is packed into container is standby;

3) TERTIARY BUTYL AMINE is dropped in the reaction vessel of 300ml, the mol ratio of TERTIARY BUTYL AMINE total amount and captax total amount is 1.06: 1, stirs and is warming up to 43-45 ℃;

4) the captax slurry that adds 5ml is as bed material, again with the captax slurry and the step 2 of step 1)) clorox be to drip at 5: 3 by volume, need between 45-55 minute, dropwise, temperature can not be higher than 45 ℃ in the dropping process.

Wherein the dropwise operation of step 4) is as follows:

M slurry (ml)	5	10	20	30	40	50	60	70	80	90	100	110	120
														Clorox (ml)	0	6	12	18	24	30	36	42	48	54	60	66	72
The dropping time (min)		7	6	3	3	3	3	3	3	3	3	6	7

Described dispersion agent is peregal or peregal 0.

Above in 1,2,3 raw-material ratio increase accordingly.Temperature-resistant, charging time was controlled between 1.5-2 hour.

The present invention does not need mother liquor to reclaim and distillation.Owing to there is not mother liquor to reclaim distillation, reduce discharge of wastewater, reduced cost, not only economy but also environmental protection, the every technical indicator of product all meets national standard.

Embodiment

Embodiment:

1, the 32.5g captax is added in the 100ml water, adding 2ml concentration again is that 7% peregal amounts to 125ml, mends when volume is not enough to 125ml (first water is supplied, and replaces water to supply with mother liquor later on), and packing into has the containers for future use of volume markings.

2, with available chlorine 18.4-18.6g/100ml, the clorox 100ml of the free alkali 0.8-1g/100ml container that has volume markings of packing into is standby.

3, at first the TERTIARY BUTYL AMINE of 15g (21.7ml) is dropped in the reaction vessel of 300ml, stir, be warming up to 43-45 ℃, the captax slurry that adds 5ml then is as bed material, be to drip at 5: 3 more by volume with captax slurry and clorox, need to dropwise between 45-55 minute, temperature can not be higher than 45 ℃ in the dropping process.

Add the 15g TERTIARY BUTYL AMINE in the reactor that stirring, thermometer are housed, stir and heat up, when treating that temperature rises to 45 ℃, add 5ml captax slurry and continue to stir, according to the form below is operated then:

In dripping the process of clorox, be in line with two slow in the middle of fast principle, and strict control reaction temperature must not be above 45 ℃.The captax slurry drips the back and continues to drip clorox, when dripping to about 80ml, survey its terminal point with end point indicator, stop to drip clorox if reach home, if continue to drip less than terminal point, till terminal point, be cooled to 35 ℃ then with bottom discharge, (retained part mother liquor be used for captax making beating), washing after filtration, dry finished product 43.4g, the product fusing point is more than 106 ℃.

Claims (3)

1. the production method of accelerator N-tertiary butyl-2-[4-morpholinodithio sulphenamide is characterized in that step is as follows:

1) the 32.5g captax is added in the 100ml water, adding 2 ml concns again is that 7% peregal dispersion agent amounts to 125ml, and make up water or mother liquor are made the captax slurry to 125ml, the containers for future use of packing into;

2) the clorox 100ml of available chlorine 18.4-18.6g/100ml, free alkali 0.8-1g/100ml is packed into container is standby;

3) TERTIARY BUTYL AMINE is dropped in the reaction vessel of 300ml, the mol ratio of TERTIARY BUTYL AMINE total amount and captax total amount is 1.06: 1, stirs and is warming up to 43-45 ℃;

4) the captax slurry that adds 5ml is as bed material, again with the captax slurry and the step 2 of step 1)) clorox be to drip at 5: 3 by volume, need between 45-55 minute, dropwise, temperature can not be higher than 45 ℃ in the dropping process.

2. production method as claimed in claim 1 is characterized in that the dropwise operation of step 4) is as follows:

M slurry (ml) 5 10 20 30 40 50 60 70 80 90 100 110 120 Clorox (ml) 0 6 12 18 24 30 36 42 48 54 60 66 72 The dropping time (min) 7 6 3 3 3 3 3 3 3 3 6 7

3. the method for claim 1, it is characterized in that: described dispersion agent is peregal or peregal 0.