CN104672119A - Production method of rubber accelerator TMTD (tetramethyl thiuram disulfide) - Google Patents

Abstract

The invention relates to a production method of a rubber accelerator TMTD (tetramethyl thiuram disulfide), which comprises the following steps: carrying out condensation reaction on dimethylamine, sodium hydroxide and carbon bisulfide, oxidizing with chlorine to obtain the TMTD, washing with water, dewatering, and drying. The method can effectively enhance the yield and purity of the accelerator TMTD and improve the quality of product, so that the quality of the rubber product produced by the accelerator is enhanced.

Description

The production method of a kind of rubber accelerator TMTD

(1) technical field

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

(2) background technology

At present, rubber accelerator TMTD is excellent the second promotor of thiazole accelerator, also can do the promotor of endless vulcanization micelle with other accelerator combinations, usually also can with accelerant MBT (M) and use, the sulfuration basic simlarity of its situation and butyl rubber.This promotor, mainly for the manufacture of tire, the inner tube of a tyre, rubber overshoes, medical treatment product, cable, industrial rubber articles etc., being agriculturally used as sterilant and sterilant, also can be used as lubricating oil additive.But present Vulcanization accelerator TMTD production technique Shortcomings, output generally rests on about 89%, purity about 95%, has had influence on the rubber product quality using this promotor to produce.Effectively can improve productive rate and the purity of Vulcanization accelerator TMTD 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 the production method of a kind of rubber accelerator TMTD.

Technical scheme of the present invention realizes like this.

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

(1) condensation operation

Close condensation tank coxopodite door, 3500L water is added in condensation tank, open and stir, open water coolant section door, drop into the dimethylamine 500L of 40%, start 98% dithiocarbonic anhydride slowly adding 264L, control charging reaction time 0.5 hours, control temperature of reaction 10 ~ 30 DEG C simultaneously, close water coolant section door, continue stirring and slowly add sodium hydroxide 159kg again in 0.5 hour, control temperature of reaction 20 ~ 40 DEG C, 1 hour reaction times, stop stirring and leave standstill, after being separated dithiocarbonic anhydride raffinate, continue to stir, after carrying out adding alkali debugging pH to 8.8 ~ 9.0 again, open the cooling of water coolant section door, when temperature is down to 30 DEG C, stop stirring, close water coolant section door and carry out standing material, open at the bottom of still and divide carbon section door, after CS2 raffinate is separated, close and finish a point carbon section door, open blowing pipeline section door, material is put into Sodium Dimethyldithiocarbamate suction filtration tank, slurry tank is squeezed into after suction filtration,

(2) oxidation operation

Close oxidation tank coxopodite door, 1500 ~ 2500L Sodium Dimethyldithiocarbamate that step one is obtained is squeezed in oxidizing reactor, open and stir and roots blower, start to pass into chlorine 69 ~ 115kg, open the insulation water of chlorine cylinder, its water temperature is 30 ~ 40 DEG C simultaneously, and logical chlorine speed is 50 ~ 65m3/h, control temperature of reaction below 50 DEG C, control of reaction end point PH=4 ~ 2;

(3) washing dries operation

Open oxidation tank coxopodite door, open dnockout pump, material is squeezed in water washing tank and passes through filter cloth, mother liquor leaches naturally, and close tank coxopodite door, add water washing, open to stir and fully washed by material, wash water leaches naturally, stops washing during pH=7, after washing, drying cloth bag is evenly taped against in drier rotary drum, opens drier, material is evenly put into drier, charge amount is 2/3 of rotary drum thickness, strengthens washing test simultaneously, stops washing after drying draining PH=7;

(4) drying process

Start housing power supply and instrument display instrument switch;

Start induced draft fan, open air door, start sieving machine and air compressor blowback pulse control instrument, open heater steam section door, be automatic system by dry import temperature controller by manual switch, inlet temperature arranges 100 ~ 120 DEG C, start discharging Sealer, discharging stirring and feeder, adjustment feed rate, and control temperature out 55 ~ 80 DEG C, induced draft fan blast: 7500Pa, cloth bag import blast: 6000Pa, cyclonic separator blast: 4000Pa, import blast: 1400Pa;

First stop heating during parking, steam off section door, and by instrument by being automatically converted to manually, going out only until material in system, material collection can be obtained product.

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

(4) embodiment

Embodiment 1

(1) condensation operation

Close condensation tank coxopodite door, 3500L water is added in condensation tank, open and stir, open water coolant section door, drop into the dimethylamine 500L of 40%, start 98% dithiocarbonic anhydride slowly adding 264L, control charging reaction time 0.5 hours, control temperature of reaction 25 DEG C simultaneously, close water coolant section door, continue stirring and slowly add sodium hydroxide 159kg again in 0.5 hour, control temperature of reaction 30 DEG C, 1 hour reaction times, stop stirring and leave standstill, after being separated dithiocarbonic anhydride raffinate, continue to stir, after carrying out adding alkali debugging pH to 8.9 again, open the cooling of water coolant section door, when temperature is down to 30 DEG C, stop stirring, close water coolant section door and carry out standing material, open at the bottom of still and divide carbon section door, after CS2 raffinate is separated, close and finish a point carbon section door, open blowing pipeline section door, material is put into Sodium Dimethyldithiocarbamate suction filtration tank, slurry tank is squeezed into after suction filtration,

(2) oxidation operation

Close oxidation tank coxopodite door, the 2000L Sodium Dimethyldithiocarbamate that step one is obtained is squeezed in oxidizing reactor, open and stir and roots blower, start to pass into chlorine 110kg, open the insulation water of chlorine cylinder, its water temperature is 35 DEG C simultaneously, and logical chlorine speed is 57m3/h, control temperature of reaction below 50 DEG C, control of reaction end point PH=3;

(3) washing dries operation

Open oxidation tank coxopodite door, open dnockout pump, material is squeezed in water washing tank and passes through filter cloth, mother liquor leaches naturally, and close tank coxopodite door, add water washing, open to stir and fully washed by material, wash water leaches naturally, stops washing during pH=7, after washing, drying cloth bag is evenly taped against in drier rotary drum, opens drier, material is evenly put into drier, charge amount is 2/3 of rotary drum thickness, strengthens washing test simultaneously, stops washing after drying draining PH=7;

(4) drying process

Start housing power supply and instrument display instrument switch;

Start induced draft fan, open air door, start sieving machine and air compressor blowback pulse control instrument, open heater steam section door, be automatic system by dry import temperature controller by manual switch, inlet temperature arranges 110 DEG C, start discharging Sealer, discharging stirring and feeder, adjustment feed rate, and control temperature out 70 DEG C, induced draft fan blast: 7500Pa, cloth bag import blast: 6000Pa, cyclonic separator blast: 4000Pa, import blast: 1400Pa;

First stop heating during parking, steam off section door, and by instrument by being automatically converted to manually, going out only until material in system, material collection can be obtained product.

The Vulcanization accelerator TMTD purity 99% that this method is made, output 94%, 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 of rubber accelerator TMTD, is characterized in that: concrete steps are as follows:

(1) condensation operation

Close condensation tank coxopodite door, 3500L water is added in condensation tank, open and stir, open water coolant section door, drop into the dimethylamine 500L of 40%, start 98% dithiocarbonic anhydride slowly adding 264L, control charging reaction time 0.5 hours, control temperature of reaction 10 ~ 30 DEG C simultaneously, close water coolant section door, continue stirring and slowly add sodium hydroxide 159kg again in 0.5 hour, control temperature of reaction 20 ~ 40 DEG C, 1 hour reaction times, stop stirring and leave standstill, after being separated dithiocarbonic anhydride raffinate, continue to stir, after carrying out adding alkali debugging pH to 8.8 ~ 9.0 again, open the cooling of water coolant section door, when temperature is down to 30 DEG C, stop stirring, close water coolant section door and carry out standing material, open at the bottom of still and divide carbon section door, after CS2 raffinate is separated, close and finish a point carbon section door, open blowing pipeline section door, material is put into Sodium Dimethyldithiocarbamate suction filtration tank, slurry tank is squeezed into after suction filtration,

(2) oxidation operation

Close oxidation tank coxopodite door, 1500 ~ 2500L Sodium Dimethyldithiocarbamate that step one is obtained is squeezed in oxidizing reactor, open and stir and roots blower, start to pass into chlorine 69 ~ 115kg, open the insulation water of chlorine cylinder, its water temperature is 30 ~ 40 DEG C simultaneously, and logical chlorine speed is 50 ~ 65m3/h, control temperature of reaction below 50 DEG C, control of reaction end point PH=4 ~ 2;

(3) washing dries operation

Open oxidation tank coxopodite door, open dnockout pump, material is squeezed in water washing tank and passes through filter cloth, mother liquor leaches naturally, and close tank coxopodite door, add water washing, open to stir and fully washed by material, wash water leaches naturally, stops washing during pH=7, after washing, drying cloth bag is evenly taped against in drier rotary drum, opens drier, material is evenly put into drier, charge amount is 2/3 of rotary drum thickness, strengthens washing test simultaneously, stops washing after drying draining PH=7;

(4) drying process

Start housing power supply and instrument display instrument switch;

Start induced draft fan, open air door, start sieving machine and air compressor blowback pulse control instrument, open heater steam section door, be automatic system by dry import temperature controller by manual switch, inlet temperature arranges 100 ~ 120 DEG C, start discharging Sealer, discharging stirring and feeder, adjustment feed rate, and control temperature out 55 ~ 80 DEG C, induced draft fan blast: 7500Pa, cloth bag import blast: 6000Pa, cyclonic separator blast: 4000Pa, import blast: 1400Pa;

First stop heating during parking, steam off section door, and by instrument by being automatically converted to manually, going out only until material in system, material collection can be obtained product.

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

(1) condensation operation

Close condensation tank coxopodite door, 3500L water is added in condensation tank, open and stir, open water coolant section door, drop into the dimethylamine 500L of 40%, start 98% dithiocarbonic anhydride slowly adding 264L, control charging reaction time 0.5 hours, control temperature of reaction 25 DEG C simultaneously, close water coolant section door, continue stirring and slowly add sodium hydroxide 159kg again in 0.5 hour, control temperature of reaction 30 DEG C, 1 hour reaction times, stop stirring and leave standstill, after being separated dithiocarbonic anhydride raffinate, continue to stir, after carrying out adding alkali debugging pH to 8.9 again, open the cooling of water coolant section door, when temperature is down to 30 DEG C, stop stirring, close water coolant section door and carry out standing material, open at the bottom of still and divide carbon section door, after CS2 raffinate is separated, close and finish a point carbon section door, open blowing pipeline section door, material is put into Sodium Dimethyldithiocarbamate suction filtration tank, slurry tank is squeezed into after suction filtration,

(2) oxidation operation

Close oxidation tank coxopodite door, the 2000L Sodium Dimethyldithiocarbamate that step one is obtained is squeezed in oxidizing reactor, open and stir and roots blower, start to pass into chlorine 110kg, open the insulation water of chlorine cylinder, its water temperature is 35 DEG C simultaneously, and logical chlorine speed is 57m3/h, control temperature of reaction below 50 DEG C, control of reaction end point PH=3;

(3) washing dries operation

Open oxidation tank coxopodite door, open dnockout pump, material is squeezed in water washing tank and passes through filter cloth, mother liquor leaches naturally, and close tank coxopodite door, add water washing, open to stir and fully washed by material, wash water leaches naturally, stops washing during pH=7, after washing, drying cloth bag is evenly taped against in drier rotary drum, opens drier, material is evenly put into drier, charge amount is 2/3 of rotary drum thickness, strengthens washing test simultaneously, stops washing after drying draining PH=7;

(4) drying process

Start housing power supply and instrument display instrument switch;

Start induced draft fan, open air door, start sieving machine and air compressor blowback pulse control instrument, open heater steam section door, be automatic system by dry import temperature controller by manual switch, inlet temperature arranges 110 DEG C, start discharging Sealer, discharging stirring and feeder, adjustment feed rate, and control temperature out 70 DEG C, induced draft fan blast: 7500Pa, cloth bag import blast: 6000Pa, cyclonic separator blast: 4000Pa, import blast: 1400Pa;

First stop heating during parking, steam off section door, and by instrument by being automatically converted to manually, going out only until material in system, material collection can be obtained product.