CN104672172A - Production process of rubber accelerator DCBS - Google Patents
Production process of rubber accelerator DCBS Download PDFInfo
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- 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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- CN
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- Prior art keywords
- sodium
- temperature
- chlorine
- water
- time
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 229920001971 elastomer Polymers 0.000 title claims abstract description 22
- 239000005060 rubber Substances 0.000 title claims abstract description 22
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 18
- CMAUJSNXENPPOF-UHFFFAOYSA-N n-(1,3-benzothiazol-2-ylsulfanyl)-n-cyclohexylcyclohexanamine Chemical compound C1CCCCC1N(C1CCCCC1)SC1=NC2=CC=CC=C2S1 CMAUJSNXENPPOF-UHFFFAOYSA-N 0.000 title claims abstract description 14
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000000460 chlorine Substances 0.000 claims abstract description 29
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000006243 chemical reaction Methods 0.000 claims abstract description 25
- 238000005406 washing Methods 0.000 claims abstract description 25
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims abstract description 18
- 159000000000 sodium salts Chemical class 0.000 claims abstract description 17
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 16
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000003513 alkali Substances 0.000 claims abstract description 9
- 239000005708 Sodium hypochlorite Substances 0.000 claims abstract description 6
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 6
- 239000000463 material Substances 0.000 claims description 34
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 12
- 239000011734 sodium Substances 0.000 claims description 12
- 229910052708 sodium Inorganic materials 0.000 claims description 12
- 238000007599 discharging Methods 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 238000004458 analytical method Methods 0.000 claims description 4
- 238000007664 blowing Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 238000010981 drying operation Methods 0.000 claims description 4
- 239000006210 lotion Substances 0.000 claims description 4
- 239000012452 mother liquor Substances 0.000 claims description 4
- 230000003647 oxidation Effects 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- 238000005070 sampling Methods 0.000 claims description 4
- 235000011149 sulphuric acid Nutrition 0.000 claims description 4
- 239000001117 sulphuric acid Substances 0.000 claims description 4
- 239000006200 vaporizer Substances 0.000 claims description 4
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical class [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 3
- 150000001412 amines Chemical class 0.000 claims description 3
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 3
- XBPCUCUWBYBCDP-UHFFFAOYSA-N Dicyclohexylamine Chemical compound C1CCCCC1NC1CCCCC1 XBPCUCUWBYBCDP-UHFFFAOYSA-N 0.000 abstract description 2
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 abstract description 2
- 230000009286 beneficial effect Effects 0.000 abstract 1
- 238000001914 filtration Methods 0.000 abstract 1
- 239000012535 impurity Substances 0.000 abstract 1
- 239000007788 liquid Substances 0.000 abstract 1
- 230000003245 working effect Effects 0.000 description 2
- OWRCNXZUPFZXOS-UHFFFAOYSA-N 1,3-diphenylguanidine Chemical compound C=1C=CC=CC=1NC(=N)NC1=CC=CC=C1 OWRCNXZUPFZXOS-UHFFFAOYSA-N 0.000 description 1
- 244000043261 Hevea brasiliensis Species 0.000 description 1
- 239000002390 adhesive tape Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229920003193 cis-1,4-polybutadiene polymer Polymers 0.000 description 1
- 238000013016 damping Methods 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229920003052 natural elastomer Polymers 0.000 description 1
- 229920001194 natural rubber Polymers 0.000 description 1
- 229920002857 polybutadiene Polymers 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 229920003048 styrene butadiene rubber Polymers 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D277/00—Heterocyclic compounds containing 1,3-thiazole or hydrogenated 1,3-thiazole rings
- C07D277/60—Heterocyclic compounds containing 1,3-thiazole or hydrogenated 1,3-thiazole rings condensed with carbocyclic rings or ring systems
- C07D277/62—Benzothiazoles
- C07D277/68—Benzothiazoles 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
- C07D277/70—Sulfur atoms
- C07D277/76—Sulfur atoms attached to a second hetero atom
- C07D277/80—Sulfur atoms attached to a second hetero atom to a nitrogen atom
Landscapes
- 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
(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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310643913.0A CN104672172A (en) | 2013-12-03 | 2013-12-03 | Production process of rubber accelerator DCBS |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310643913.0A CN104672172A (en) | 2013-12-03 | 2013-12-03 | Production process of rubber accelerator DCBS |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104672172A true CN104672172A (en) | 2015-06-03 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310643913.0A Pending CN104672172A (en) | 2013-12-03 | 2013-12-03 | Production process of rubber accelerator DCBS |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104672172A (en) |
Cited By (2)
| 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 |
-
2013
- 2013-12-03 CN CN201310643913.0A patent/CN104672172A/en active Pending
Cited By (3)
| 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 |