CN114516978A - Method for mechanically applying vulcanization accelerator DZ mother liquor for rubber and application thereof - Google Patents
Method for mechanically applying vulcanization accelerator DZ mother liquor for rubber and application thereof Download PDFInfo
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- CN114516978A CN114516978A CN202210197476.3A CN202210197476A CN114516978A CN 114516978 A CN114516978 A CN 114516978A CN 202210197476 A CN202210197476 A CN 202210197476A CN 114516978 A CN114516978 A CN 114516978A
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- Prior art keywords
- mother liquor
- vulcanization accelerator
- rubber
- accelerator
- upper layer
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- 239000012452 mother liquor Substances 0.000 title claims abstract description 60
- 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 45
- 238000000034 method Methods 0.000 title claims abstract description 44
- 238000004073 vulcanization Methods 0.000 title claims abstract description 21
- 229920001971 elastomer Polymers 0.000 title claims abstract description 20
- 239000005060 rubber Substances 0.000 title claims abstract description 20
- XBPCUCUWBYBCDP-UHFFFAOYSA-N Dicyclohexylamine Chemical compound C1CCCCC1NC1CCCCC1 XBPCUCUWBYBCDP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000007788 liquid Substances 0.000 claims abstract description 19
- YXIWHUQXZSMYRE-UHFFFAOYSA-N 1,3-benzothiazole-2-thiol Chemical compound C1=CC=C2SC(S)=NC2=C1 YXIWHUQXZSMYRE-UHFFFAOYSA-N 0.000 claims abstract description 14
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 37
- 239000000243 solution Substances 0.000 claims description 19
- 238000006243 chemical reaction Methods 0.000 claims description 18
- 238000013040 rubber vulcanization Methods 0.000 claims description 12
- 239000005708 Sodium hypochlorite Substances 0.000 claims description 11
- 238000001914 filtration Methods 0.000 claims description 11
- 239000000047 product Substances 0.000 claims description 11
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 10
- 239000002904 solvent Substances 0.000 claims description 9
- 238000005273 aeration Methods 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 6
- 239000012535 impurity Substances 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 4
- 229920003051 synthetic elastomer Polymers 0.000 claims description 4
- 239000005061 synthetic rubber Substances 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 239000000706 filtrate Substances 0.000 claims description 3
- 239000010413 mother solution Substances 0.000 claims description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 2
- 239000000460 chlorine Substances 0.000 claims description 2
- 229910052801 chlorine Inorganic materials 0.000 claims description 2
- 239000012295 chemical reaction liquid Substances 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 4
- 239000002699 waste material Substances 0.000 abstract description 3
- 150000003839 salts Chemical class 0.000 abstract 1
- 239000002351 wastewater Substances 0.000 abstract 1
- 239000011347 resin Substances 0.000 description 11
- 229920005989 resin Polymers 0.000 description 11
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 10
- 239000012071 phase Substances 0.000 description 7
- 238000004064 recycling Methods 0.000 description 5
- 238000007664 blowing Methods 0.000 description 4
- 238000004811 liquid chromatography Methods 0.000 description 4
- 230000002194 synthesizing effect Effects 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000003513 alkali Substances 0.000 description 2
- 239000008346 aqueous phase Substances 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 239000003995 emulsifying agent Substances 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 230000002572 peristaltic effect Effects 0.000 description 2
- XTUSEBKMEQERQV-UHFFFAOYSA-N propan-2-ol;hydrate Chemical compound O.CC(C)O XTUSEBKMEQERQV-UHFFFAOYSA-N 0.000 description 2
- 238000004537 pulping Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 230000001133 acceleration Effects 0.000 description 1
- 238000005276 aerator Methods 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000010815 organic waste Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/36—Sulfur-, selenium-, or tellurium-containing compounds
- C08K5/45—Heterocyclic compounds having sulfur in the ring
- C08K5/46—Heterocyclic compounds having sulfur in the ring with oxygen or nitrogen in the ring
- C08K5/47—Thiazoles
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/17—Amines; Quaternary ammonium compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L21/00—Compositions of unspecified rubbers
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/62—Plastics recycling; Rubber recycling
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for mechanically applying a vulcanization accelerator DZ mother liquor for rubber and application thereof. The method has the advantages of simple process, reduction of the generation amount of salt-containing organic wastewater, reduction of the pollution of waste liquid discharge to the environment, full utilization of the raw materials of dicyclohexylamine and the accelerator M, and high purity, high yield and good quality of the synthesized accelerator DZ.
Description
Technical Field
The invention relates to a method for mechanically applying a vulcanization accelerator DZ mother liquor for rubber, and also relates to a method for mechanically applying the mother liquor to synthesize the vulcanization accelerator DZ for rubber, belonging to the technical field of rubber auxiliary agent preparation.
Background
The rubber accelerator DZ is a sulfimide accelerator with long scorching time, has the functions of vulcanization acceleration and adhesion, and is very suitable for radial tire production. The production of the accelerant DZ can generate a large amount of organic waste liquid, so that a mother liquor recycling process is developed. CN103524451A introduces a method for synthesizing a rubber accelerator DZ by mother liquor mechanically, which comprises the steps of adding the mother liquor, isopropanol and dicyclohexylamine into a reaction kettle, and then dropwise adding M-Na into the reaction kettle to synthesize the accelerator DZ; CN101899020A introduces a method for producing accelerator DZ by using sodium hypochlorite as an oxidant and using mother liquor and isopropanol as solvents of dicyclohexylamine, and then synthesizing the accelerator DZ by three drops. As is known to all, because the purity of the accelerator M is not 100%, impurities such as resin in the accelerator M are enriched after mother liquor is reused, particularly after the mother liquor is reused for many times, and are finally remained in an accelerator DZ product, so that the appearance color and the purity of the product are seriously influenced. Mother liquor introduced in Qi Rong Wei Master thesis of Qingdao university of science and technology is used mechanically by distilling mother liquor to recover isopropanol, adjusting pH of residue in kettle to about 7, filtering, adding a small amount of toluene into waste residue (containing resin, unreacted raw material accelerator M and byproduct accelerator DM), stirring to dissolve part of impurities such as resin, filtering, adding a large amount of recovered isopropanol into filter residue, stirring to dissolve, filtering insoluble substances, and using filtrate solution in synthesis experiment. The process is very complex and high in energy consumption, and only unreacted raw material accelerator M and byproduct accelerator DM are utilized without utilizing the raw material dicyclohexylamine in the mother liquor.
Disclosure of Invention
Aiming at the defects of the existing mother liquor applying process, the invention provides an applying method of a vulcanization accelerator DZ mother liquor for rubber.
The specific technical scheme of the invention is as follows:
a method for mechanically applying a vulcanization accelerator DZ mother solution for rubber comprises the following steps: standing and layering the rubber vulcanization accelerator DZ mother liquor, taking the upper layer liquid, adjusting the pH of the upper layer liquid to be alkaline, then carrying out aeration treatment, filtering the upper layer liquid after the aeration treatment to remove impurities, and using the obtained filtrate as a solvent in the production process of the rubber vulcanization accelerator DZ for indiscriminately.
Furthermore, in the applying method, the pH value of the upper layer liquid is adjusted to 8.0-9.0, and then aeration treatment is carried out, so that resin impurities can be better separated out.
Further, in the above application method, the upper layer liquid aeration treatment mode is as follows: introducing air into the upper layer liquid at the speed of 2-5 cubic decimeters per minute for about 0.5-1 hour.
Further, in the above-mentioned method for applying mechanically, the said vulcanization accelerator DZ mother liquor for rubber refers to the liquor remaining after the vulcanization accelerator DZ for rubber is separated from the reaction liquor of the vulcanization accelerator DZ for rubber.
The invention also provides a method for synthesizing the vulcanization accelerator DZ for rubber by using the mother liquor mechanically, which comprises the following steps: the mother liquor of the vulcanization accelerator DZ for rubber is treated according to the mechanically applying method and then used as a solvent sleeve for synthesizing the vulcanization accelerator DZ for rubber.
Further, the vulcanization accelerator DZ for synthetic rubber comprises the following steps:
(1) adding the treated mother liquor and dicyclohexylamine into a reaction kettle, and stirring for dissolving;
(2) heating the reaction kettle to the reaction temperature, simultaneously dripping an isopropanol solution and a sodium hypochlorite aqueous solution of the accelerant M into the reaction kettle while stirring, keeping the pH of the system to be 9-11 in the dripping process, and continuing the reaction after dripping is finished;
(3) after the reaction, separating the rubber vulcanization accelerator DZ from the reaction solution, washing and drying to obtain a rubber vulcanization accelerator DZ product, and treating the residual mother liquor by the method for mechanically applying the rubber vulcanization accelerator DZ mother liquor to serve as a solvent for preparing the next batch of products.
Further, sodium hypochlorite: accelerator M: the molar ratio of dicyclohexylamine is 1.0-1.6: 1.0-1.2: 1.
Furthermore, in the isopropanol solution of the accelerator M, the mass ratio of the accelerator M to the isopropanol is 1: 3.5-4.0.
Furthermore, the effective chlorine concentration in the sodium hypochlorite water solution is 14.5-19.0 g/100 ml.
Further, the mass ratio of dicyclohexylamine to the treated mother liquor is 1: 2.5 to 4.5.
Further, in the step (2), the reaction temperature is 35.0-55.0 ℃, the stirring speed is 350-500 r/min, the dropping time is 2.0-3.0 hours, and the temperature is kept for 0.5-1 hour after the dropping is finished.
The method treats the synthetic mother liquor of the promoter DZ and then applies the synthetic mother liquor, removes the impurities such as resin and the like which easily influence the appearance, color and purity of the promoter DZ in the mother liquor, and avoids the influence of the mother liquor application on the quality of the promoter DZ. The treatment method has the advantages of simple operation, low cost, good environmental protection, no generation of new pollution, no need of recovering isopropanol by evaporation, and reduced energy consumption and cost. The treated mother liquor is used as a solvent for recycling, residual dicyclohexylamine, the accelerator M and derivatives thereof in the mother liquor are fully utilized, the appearance and the purity of the obtained accelerator DZ are similar to those of a fresh solvent, the purity of the accelerator DZ is over 99.0 percent, and the yield can reach 98.8 percent. And the recycling of the mother liquor also reduces the pollution of the discharge of the waste liquid to the environment, and meets the requirement of environmental protection.
Detailed Description
The invention is further illustrated and described below by means of specific examples, which are given by way of illustration only and do not limit the scope of protection.
Example 1
1. Adding 52 g of 98.8wt% of accelerator M into a beaker containing 200 g of isopropanol, and pulping for 10 minutes by using a high-shear emulsifier for later use;
2. weighing 200 g of sodium hypochlorite aqueous solution with the mass concentration of 15wt% in a brown bottle for later use;
3. adding 135 g of 40wt% isopropanol aqueous solution into a four-neck flask, adding 47 g of dicyclohexylamine, stirring and heating, when the temperature in the four-neck flask is heated to 45 ℃, respectively dropwise adding a sodium hypochlorite solution and an accelerator M solution into the four-neck flask by using a peristaltic pump, completing dropwise adding within 2.5 hours, maintaining the pH value to be 9-11 by using dilute sulfuric acid or dilute alkali solution in the dropwise adding process, preserving the temperature at 45-50 ℃ for 30 minutes after completing dropwise adding, filtering, washing with water, and drying to obtain 84.4 g of an accelerator DZ product, wherein the yield is 93.9% (calculated by dicyclohexylamine), the liquid chromatogram purity is 99.5%, and the appearance is bright yellowish.
Pouring the filtered mother liquor into a pear-shaped separating funnel to stand for 1 hour, then removing the lower water phase, transferring the upper oil phase into a three-neck flask, adjusting the pH to 8.5 by using 15wt% dilute sulfuric acid, then blowing air into the flask for 1 hour by using a miniature air blower at the air blowing speed of 5 cubic decimeters per minute (under the standard atmospheric pressure, at 25 ℃), then filtering to remove the precipitated black solid resin, wherein the weight of the dried resin is about 0.65g, and the filtered mother liquor is reserved.
The mother liquor replaces isopropanol water solution for recycling, and the method comprises the following steps: promoter DZ was prepared using steps 1, 2 and 3 above, except that 135 grams of a 40wt% aqueous isopropanol solution from step 2 was replaced with a mother liquor treated in the manner described above. The mother liquor is continuously recycled according to the method, the mother liquor is treated in the method and then recycled, and when the mother liquor is continuously recycled for 5 times, the yield of the obtained promoter DZ product is 98.6% (calculated by dicyclohexylamine), the liquid chromatography purity is 99.2%, and the appearance is still bright and yellowish.
Example 2
The mother liquor obtained by filtration in the above example 1 was poured into a pear-shaped separatory funnel and allowed to stand for 1 hour, then the lower aqueous phase was discarded, the upper oil phase was transferred to a three-necked flask, the pH was adjusted to 8.0 with 15wt% dilute sulfuric acid, and then the flask was aerated with a micro-aerator at an aeration rate of 5 cubic decimeters per minute (25 ℃ C. under standard atmospheric pressure) for 0.5 hour, and then the precipitated black solid resin was removed by filtration, the weight of the resin was about 0.72 g after drying, and the filtered mother liquor was ready for use.
Accelerator DZ was prepared by the method of steps 1, 2 and 3 in example 1, substituting the treated mother liquor for the aqueous isopropanol solution in step 2 in example 1. The mother liquor obtained each time is mechanically applied in the manner, and after the mother liquor is continuously applied for 5 times, the yield of the obtained promoter DZ product is 98.8% (calculated by dicyclohexylamine), the liquid chromatography purity is 99.0%, and the appearance is still bright and yellowish.
Example 3
1. Adding 52 g of 98.8 wt% of accelerator M into a beaker filled with 200 g of isopropanol, and pulping for 10 minutes by using a high-shear emulsifier for later use;
2. weighing 200 g of sodium hypochlorite aqueous solution with the mass concentration of 15wt% in a brown bottle for later use;
3. adding 200 g of 40wt% isopropanol aqueous solution into a four-neck flask, adding 47 g of dicyclohexylamine, stirring and heating, when the temperature in the four-neck flask is heated to 35 ℃, respectively dropwise adding sodium hypochlorite solution and accelerator M solution into the four-neck flask by using a peristaltic pump, completing dropwise adding within 3.0 hours, maintaining the pH value to be 9-11 by using dilute sulfuric acid or dilute liquid alkali in the dropwise adding process, keeping the temperature at 50-55 ℃ for 60 minutes after completing dropwise adding, and then filtering, washing and drying to obtain 84.7 g of an accelerator DZ product, wherein the yield is 94.3% (calculated by dicyclohexylamine), the liquid chromatogram purity is 99.3%, and the appearance is bright yellowish.
Pouring the filtered mother liquor into a pear-shaped separating funnel, standing for 1 hour, removing a lower water phase, transferring an upper oil phase into a three-neck flask, adjusting the pH to 9.0 by using 15wt% dilute sulfuric acid, then blowing air into the flask for 1 hour by using a miniature air blower at the air blowing speed of 2.5 cubic decimeters per minute (under the standard atmospheric pressure, at 25 ℃), filtering to remove precipitated black solid resin, wherein the weight of the resin is about 0.85 g after drying, and reserving the filtered mother liquor for later use.
The mother liquor replaces isopropanol water solution for recycling, and the method comprises the following steps: promoter DZ was prepared using steps 1, 2 and 3 above, except that 200 grams of a 40wt% aqueous isopropanol solution from step 2 was replaced with a mother liquor treated in the manner described above. The mother liquor is continuously recycled according to the method, the mother liquor is treated in the method and then recycled, and when the mother liquor is continuously recycled for 5 times, the yield of the obtained promoter DZ product is 98.5 percent (calculated by dicyclohexylamine), the liquid chromatography purity is 99.1 percent, and the appearance is still bright and yellowish.
Comparative example 1
Pouring the mother liquor obtained in the example 1 into a pear-shaped separating funnel to stand for 1 hour, then discarding the lower aqueous phase, and transferring the upper oil phase into a three-neck flask for later use;
accelerator DZ was prepared using steps 1, 2, 3 of example 1, except that: 135 grams of 40wt% aqueous isopropanol solution was replaced with untreated mother liquor of the upper oil phase. The resultant DZ promoter was 85.1 g, a yield of 94.7% (based on dicyclohexylamine), a liquid chromatography purity of 98.2%, and a gray-black appearance.
Claims (10)
1. A method for mechanically applying vulcanization accelerator DZ mother liquor for rubber is characterized by comprising the following steps: standing and layering the rubber vulcanization accelerator DZ mother liquor, taking the upper layer liquid, adjusting the pH of the upper layer liquid to be alkaline, then carrying out aeration treatment, filtering the upper layer liquid after the aeration treatment to remove impurities, and using the obtained filtrate as a solvent in the production process of the rubber vulcanization accelerator DZ for indiscriminately.
2. The method of claim 1, wherein: adjusting the pH value of the upper layer liquid to 8.0-9.0.
3. The method of using of claim 1 or 2, wherein: the upper layer liquid aeration treatment mode is as follows: and introducing air into the upper layer liquid at the speed of 2-5 cubic decimeters per minute for treatment for 0.5-1 hour.
4. The method of claim 1, wherein: the rubber vulcanization accelerator DZ mother liquor refers to the liquid remained after the rubber vulcanization accelerator DZ reaction liquid is separated.
5. A method for mechanically applying a vulcanization accelerator DZ for synthetic rubber to mother liquor is characterized by comprising the following steps: the rubber vulcanization accelerator DZ mother liquor is treated according to the method for applying the rubber vulcanization accelerator DZ mother liquor of any one of claims 1 to 4 and then used as a solvent to be applied to the synthetic rubber vulcanization accelerator DZ.
6. The method of claim 5, wherein: the vulcanization accelerator DZ for synthetic rubber comprises the following steps:
(1) adding the treated mother liquor and dicyclohexylamine into a reaction kettle, and stirring for dissolving;
(2) heating the reaction kettle to the reaction temperature, simultaneously dripping an isopropanol solution of an accelerant M and a sodium hypochlorite aqueous solution into the reaction kettle while stirring, keeping the pH of the system at 9-11 in the dripping process, and continuing to react after dripping is finished;
(3) After the reaction, separating the vulcanization accelerator DZ for rubber from the reaction solution, washing and drying to obtain a vulcanization accelerator DZ product for rubber, wherein the residual mother solution is used as a solvent for preparing the next product after being treated according to the method for mechanically applying the vulcanization accelerator DZ mother solution for rubber as described in any one of claims 1 to 4.
7. The method of claim 6, wherein: sodium hypochlorite: accelerator M: the molar ratio of dicyclohexylamine is 1.0-1.6: 1.0-1.2: 1.
8. The method of claim 6, wherein: in the promoter M isopropanol solution, the mass ratio of the promoter M to the isopropanol is 1: 3.5-4.0, and the effective chlorine concentration in the sodium hypochlorite aqueous solution is 14.5-19.0 g/100 ml.
9. The method of claim 6, wherein: the mass ratio of dicyclohexylamine to the treated mother liquor is 1: 2.5 to 4.5.
10. The method of claim 6, wherein: in the step (2), the reaction temperature is 35.0-55.0 ℃, the stirring speed is 350-500 r/min, the dripping time is 2.0-3.0 hours, and the temperature is kept for 0.5-1 hour after dripping.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210197476.3A CN114516978A (en) | 2022-03-02 | 2022-03-02 | Method for mechanically applying vulcanization accelerator DZ mother liquor for rubber and application thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210197476.3A CN114516978A (en) | 2022-03-02 | 2022-03-02 | Method for mechanically applying vulcanization accelerator DZ mother liquor for rubber and application thereof |
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| CN114516978A true CN114516978A (en) | 2022-05-20 |
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| CN202210197476.3A Pending CN114516978A (en) | 2022-03-02 | 2022-03-02 | Method for mechanically applying vulcanization accelerator DZ mother liquor for rubber and application thereof |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102432136A (en) * | 2011-09-20 | 2012-05-02 | 科迈化工股份有限公司 | Method for treating wastewater of rubber vulcanization accelerator N-cyclohexyl-2-benzothiazole sulfonamide |
| CN103539755A (en) * | 2013-08-15 | 2014-01-29 | 山东邹平开元化工石材有限公司 | Production method of accelerator MBT (Mercaptobenzothiazole) |
| CN104672169A (en) * | 2013-12-03 | 2015-06-03 | 天津一化化工有限公司 | Production method of rubber accelerator MBT |
| 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 |
| CN105217870A (en) * | 2015-11-04 | 2016-01-06 | 南京环保产业创新中心有限公司 | Reinforcing rubber promotor wastewater preprocessing process |
-
2022
- 2022-03-02 CN CN202210197476.3A patent/CN114516978A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102432136A (en) * | 2011-09-20 | 2012-05-02 | 科迈化工股份有限公司 | Method for treating wastewater of rubber vulcanization accelerator N-cyclohexyl-2-benzothiazole sulfonamide |
| CN103539755A (en) * | 2013-08-15 | 2014-01-29 | 山东邹平开元化工石材有限公司 | Production method of accelerator MBT (Mercaptobenzothiazole) |
| CN104672169A (en) * | 2013-12-03 | 2015-06-03 | 天津一化化工有限公司 | Production method of rubber accelerator MBT |
| 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 |
| CN105217870A (en) * | 2015-11-04 | 2016-01-06 | 南京环保产业创新中心有限公司 | Reinforcing rubber promotor wastewater preprocessing process |
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Application publication date: 20220520 |