CN104672172A - Production process of rubber accelerator DCBS - Google Patents

Production process of rubber accelerator DCBS Download PDF

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Publication number
CN104672172A
CN104672172A CN201310643913.0A CN201310643913A CN104672172A CN 104672172 A CN104672172 A CN 104672172A CN 201310643913 A CN201310643913 A CN 201310643913A CN 104672172 A CN104672172 A CN 104672172A
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China
Prior art keywords
sodium
temperature
chlorine
water
time
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Pending
Application number
CN201310643913.0A
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Chinese (zh)
Inventor
张维仁
陶巧华
岳姝雅
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TIANJIN YIHUA CHEMICAL CO Ltd
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TIANJIN YIHUA CHEMICAL CO Ltd
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Priority to CN201310643913.0A priority Critical patent/CN104672172A/en
Publication of CN104672172A publication Critical patent/CN104672172A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D277/00Heterocyclic compounds containing 1,3-thiazole or hydrogenated 1,3-thiazole rings
    • C07D277/60Heterocyclic compounds containing 1,3-thiazole or hydrogenated 1,3-thiazole rings condensed with carbocyclic rings or ring systems
    • C07D277/62Benzothiazoles
    • C07D277/68Benzothiazoles with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached in position 2
    • C07D277/70Sulfur atoms
    • C07D277/76Sulfur atoms attached to a second hetero atom
    • C07D277/80Sulfur atoms attached to a second hetero atom to a nitrogen atom

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)

Abstract

The invention discloses a production process of a rubber accelerator DCBS. The process comprises the following steps: performing reaction on liquid alkali and chlorine to generate sodium hypochlorite; sequentially adding quantitative isopropanol, water, sodium bicarbonate, dicyclohexylamine and a proper amount of sulfuric acid into an oxidization reaction kettle; adding M sodium salt, sodium hypochlorite and sulfuric acid to perform oxidization reaction to obtain a finished product DCBS; filtering and washing the finished product to obtain the product. The production process has the beneficial effects that the yield and the purity of the accelerate DCBS can be improved, the yield and the quality of the product are improved, and the production cost is reduced; the rubber product which is manufactured by the accelerator prepared by using the method has low content of impurities and is long in service life.

Description

The production technique of a kind of rubber accelerator DCBS
(1) technical field
The present invention relates to a kind of rubber accelerator production technique, particularly relate to the production technique of a kind of rubber accelerator DCBS.
(2) background technology
At present, rubber accelerator DCBS is the delayed action accelerator of natural rubber, styrene-butadiene rubber(SBR), cis-1,4-polybutadiene rubber etc., and good dispersion property in rubber, is applicable to high reactivity strengthening agent, large usage quantity.Also being applicable to polybutadiene rubber or reclaimed rubber is main sizing material.The cross-linked rubber mechanical property produced with this promotor, especially dynamic property is relatively good, elasticity and tensile modulus high, can be used for manufacturing the extension gum material etc. of tire, adhesive tape, damping products and retreading.But present rubber accelerator DCBS is due to the impact of production technique, productive rate generally maintains about 95%, and purity is about 96%, causes the rubber product foreign matter content produced with this promotor more, and impact uses.Productive rate and purity can be improved on the market, improve output and quality product, reduce production cost, and the production technique of rubber accelerator DCBS that the rubber product foreign matter content that the promotor that this method of use is made is produced is low, work-ing life extends is not also found, and awaits exploitation.
(3) summary of the invention
In order to overcome the weak point of existing rubber accelerator production technique, the invention provides the production technique of a kind of rubber accelerator DCBS.
Technical scheme of the present invention realizes like this.
The production technique of a kind of rubber accelerator DCBS of this programme, concrete steps are as follows:
(1) clorox operation
Be that the alkali lye of 20g/100ml puts into sodium hypochlorite reaction still after metering by concentration, unlatching cools, and temperature is down to 15 DEG C, starts logical chlorine.Open the recycle pump of vaporizer, its water temperature 35 DEG C simultaneously;
Reaction process observes temperature variation at any time, and reaction controlling is below 30 DEG C, if temperature stops chlorine close to when 30 DEG C, after temperature lowers, continues reaction;
According to the logical amount of chlorine of estimation, lead to chlorine speed when closing on terminal and want slow and shift to an earlier date sampling analysis, until reach effective chlorine density 15.8g/100ml, logical chlorine is stopped during free alkali concentration 1.1g/100ml, logical chlorine end of operation, treats that temperature is down in 15 DEG C, stops stirring and cooling;
(2) oxidation operation
Close stills for air blowing discharging section door, after 25% dilute sulphuric acid of the aqueous isopropanol of 1200 parts of 0.64kg/L, 220 parts of water, 6 parts of sodium bicarbonates, 293 parts of dicyclohexyl amines and 280L is dropped into successively, open and stir, open simultaneously and survey pH value and to circulate little pump, drip the clorox that the M sodium salt of 55.5kg/L and step () are synthesized in proportion simultaneously, the flow control of M sodium salt at 238L/h, by clorox flow control at 702L/h; Within first 30 minutes, sodium salt is 1:3 with the actual charging capacity volume of time sodium, and then secondary sodium volumetric flow rate reduces, and is 1:2, finally adds simultaneously at the volume of remaining 2 hours M sodium salts and time sodium.In reaction process, detect the pH value of material at any time, with sulfuric acid strictly control PH9.7, by the cold control temperature of reaction of chuck 38 DEG C, end of operation is cooled to 30 DEG C, is gone out by material to water washing tank, stops high temperature discharging;
(3) alcohol wash, washing, drying operation
First the mother liquor of water washing tank material is pumped, material is made to become dry powder, then add 350L alcohol and carry out alcohol wash, washing time 15 minutes, wash and alcohol is pumped, the complete 380L of the adding water of alcohol wash is washed, each washing time 20 minutes, washes 3 times, washing is stopped to water lotion pH value≤7.5, wash and complete material is put into drier, the material of drier is wanted evenly, and material can not exceed 2/3rds of rotary drum, get rid of to drier outlet be as the criterion without water droplet, after drier stops, by the material collection after drying, namely obtain finished product.
Usefulness of the present invention is: the method can improve productive rate and the purity of vulkacit D CBS, improves output and quality product, reduces production cost, and the rubber product foreign matter content that the promotor that this method of use is made is produced is low, prolongation in work-ing life.
(4) embodiment
Embodiment 1
A production technique of rubber accelerator DCBS, is characterized in that:
Concrete steps are as follows:
(1) clorox operation
Be that the alkali lye of 20g/100ml puts into sodium hypochlorite reaction still after metering by concentration, unlatching cools, and temperature is down to 15 DEG C, starts logical chlorine.Open the recycle pump of vaporizer, its water temperature 35 DEG C simultaneously;
Reaction process observes temperature variation at any time, and reaction controlling is below 30 DEG C, if temperature stops chlorine close to when 30 DEG C, after temperature lowers, continues reaction;
According to the logical amount of chlorine of estimation, lead to chlorine speed when closing on terminal and want slow and shift to an earlier date sampling analysis, until reach effective chlorine density 15.8g/100ml, logical chlorine is stopped during free alkali concentration 1.1g/100ml, logical chlorine end of operation, treats that temperature is down in 15 DEG C, stops stirring and cooling;
(2) oxidation operation
Close stills for air blowing discharging section door, after 25% dilute sulphuric acid of the aqueous isopropanol of 1200L0.64kg/L, 220L water, 6kg sodium bicarbonate, 293kg dicyclohexyl amine and 280L is dropped into successively, open and stir, open simultaneously and survey pH value and to circulate little pump, drip the clorox that the M sodium salt of 55.5kg/L and step () are synthesized in proportion simultaneously, the flow control of M sodium salt at 238L/h, by clorox flow control at 702L/h; Within first 30 minutes, sodium salt is 1:3 with the actual charging capacity volume of time sodium, and then secondary sodium volumetric flow rate reduces, and is 1:2, finally adds simultaneously at the volume of remaining 2 hours M sodium salts and time sodium.In reaction process, detect the pH value of material at any time, with sulfuric acid strictly control PH9.7, by the cold control temperature of reaction of chuck 38 DEG C, end of operation is cooled to 30 DEG C, is gone out by material to water washing tank, stops high temperature discharging;
(3) alcohol wash, washing, drying operation
First the mother liquor of water washing tank material is pumped, material is made to become dry powder, then add 350L alcohol and carry out alcohol wash, washing time 15 minutes, washes and is pumped by alcohol, and the complete 380L of the adding water of alcohol wash is washed, each washing time 20 minutes, wash 3 times, to water lotion pH value≤7.5, stop washing, wash and complete material is put into drier, the material of drier is wanted evenly, material can not exceed 2/3rds of rotary drum, get rid of to drier outlet be as the criterion without water droplet, until drier stopping after, by the material collection after drying, namely finished product is obtained, productive rate 96% as calculated, purity 99%.
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 technique of rubber accelerator DCBS, is characterized in that:
Concrete steps are as follows:
(1) clorox operation
Be that the alkali lye of 19.5-21g/100ml puts into sodium hypochlorite reaction still after metering by concentration, unlatching cools, and temperature is down to less than 20 DEG C, starts logical chlorine.Open the recycle pump of vaporizer, its water temperature≤45 DEG C simultaneously;
Reaction process observes temperature variation at any time, and reaction controlling is below 30 DEG C, if temperature stops chlorine close to when 30 DEG C, after temperature lowers, continues reaction;
According to the logical amount of chlorine of estimation, lead to chlorine speed when closing on terminal and want slow and shift to an earlier date sampling analysis, until reach effective chlorine density 15-16g/100ml, logical chlorine is stopped during free alkali concentration 0.9-1.2g/100ml, logical chlorine end of operation, treats that temperature is down in about 15 DEG C, stops stirring and cooling;
(2) oxidation operation
Close stills for air blowing discharging section door, after 25% dilute sulphuric acid of the aqueous isopropanol of 1200 parts of 0.64kg/L, 220 parts of water, 6 parts of sodium bicarbonates, 293 parts of dicyclohexyl amines and 280L is dropped into successively, open and stir, open simultaneously and survey pH value and to circulate little pump, drip the clorox that the M sodium salt of 55.5kg/L and step () are synthesized in proportion simultaneously, the flow control of M sodium salt at 200-300L/h, by clorox flow control at 650-750L/h.Within first 30 minutes, sodium salt is 1:3 with the actual charging capacity volume of time sodium, and then secondary sodium volumetric flow rate reduces, and is 1:2, finally adds simultaneously at the volume of remaining 2 hours M sodium salts and time sodium.In reaction process, detect the pH value of material at any time, with sulfuric acid strictly control PH9.6-10, with the cold control temperature of reaction 30-50 DEG C of chuck, end of operation is cooled to 30 DEG C, is gone out by material to water washing tank, stops high temperature discharging;
(3) alcohol wash, washing, drying operation
First the mother liquor of water washing tank material is pumped, material is made to become dry powder, then add 350L alcohol and carry out alcohol wash, washing time is no less than 10 minutes, wash and alcohol is pumped, the water of complete about the 300-400L of adding of alcohol wash is washed, and each washing time is no less than 10 minutes, washes 2-3 time, washing is stopped to water lotion pH value≤7.5, wash and complete material is put into drier, the material of drier is wanted evenly, and material can not exceed 2/3rds of rotary drum, get rid of to drier outlet be as the criterion without water droplet, after drier stops, by the material collection after drying, namely obtain finished product.
2. the production technique of a kind of rubber accelerator DCBS according to claim 1, is characterized in that:
Concrete steps are as follows:
(1) clorox operation
Be that the alkali lye of 20g/100ml puts into sodium hypochlorite reaction still after metering by concentration, unlatching cools, and temperature is down to 15 DEG C, starts logical chlorine.Open the recycle pump of vaporizer, its water temperature 35 DEG C simultaneously;
Reaction process observes temperature variation at any time, and reaction controlling is below 30 DEG C, if temperature stops chlorine close to when 30 DEG C, after temperature lowers, continues reaction;
According to the logical amount of chlorine of estimation, lead to chlorine speed when closing on terminal and want slow and shift to an earlier date sampling analysis, until reach effective chlorine density 15.8g/100ml, logical chlorine is stopped during free alkali concentration 1.1g/100ml, logical chlorine end of operation, treats that temperature is down in 15 DEG C, stops stirring and cooling;
(2) oxidation operation
Close stills for air blowing discharging section door, after 25% dilute sulphuric acid of the aqueous isopropanol of 1200 parts of 0.64kg/L, 220 parts of water, 6 parts of sodium bicarbonates, 293 parts of dicyclohexyl amines and 280L is dropped into successively, open and stir, open simultaneously and survey pH value and to circulate little pump, drip the clorox that the M sodium salt of 55.5kg/L and step () are synthesized in proportion simultaneously, the flow control of M sodium salt at 238L/h, by clorox flow control at 702L/h; Within first 30 minutes, sodium salt is 1:3 with the actual charging capacity volume of time sodium, and then secondary sodium volumetric flow rate reduces, and is 1:2, finally adds simultaneously at the volume of remaining 2 hours M sodium salts and time sodium.In reaction process, detect the pH value of material at any time, with sulfuric acid strictly control PH9.7, by the cold control temperature of reaction of chuck 38 DEG C, end of operation is cooled to 30 DEG C, is gone out by material to water washing tank, stops high temperature discharging;
(3) alcohol wash, washing, drying operation
First the mother liquor of water washing tank material is pumped, material is made to become dry powder, then add 350L alcohol and carry out alcohol wash, washing time 15 minutes, wash and alcohol is pumped, the complete 380L of the adding water of alcohol wash is washed, each washing time 20 minutes, washes 3 times, washing is stopped to water lotion pH value≤7.5, wash and complete material is put into drier, the material of drier is wanted evenly, and material can not exceed 2/3rds of rotary drum, get rid of to drier outlet be as the criterion without water droplet, after drier stops, by the material collection after drying, namely obtain finished product.
CN201310643913.0A 2013-12-03 2013-12-03 Production process of rubber accelerator DCBS Pending CN104672172A (en)

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Application Number Priority Date Filing Date Title
CN201310643913.0A CN104672172A (en) 2013-12-03 2013-12-03 Production process of rubber accelerator DCBS

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CN104672172A true CN104672172A (en) 2015-06-03

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105037295A (en) * 2015-07-22 2015-11-11 聊城金歌合成材料有限公司 Method for producing sulfenamide rubber vulcanization accelerator
CN117551054A (en) * 2024-01-11 2024-02-13 科迈化工股份有限公司 Method for improving the yield of synthetic sulfenamide accelerators using isopropyl alcohol

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105037295A (en) * 2015-07-22 2015-11-11 聊城金歌合成材料有限公司 Method for producing sulfenamide rubber vulcanization accelerator
CN105037295B (en) * 2015-07-22 2018-06-22 聊城金歌合成材料有限公司 A kind of method for producing sulfenamide thiofide
CN117551054A (en) * 2024-01-11 2024-02-13 科迈化工股份有限公司 Method for improving the yield of synthetic sulfenamide accelerators using isopropyl alcohol

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Application publication date: 20150603