CN117551054A - Method for improving yield of synthesized sulfenamide accelerator by pulping isopropanol - Google Patents
Method for improving yield of synthesized sulfenamide accelerator by pulping isopropanol Download PDFInfo
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- CN117551054A CN117551054A CN202410039541.9A CN202410039541A CN117551054A CN 117551054 A CN117551054 A CN 117551054A CN 202410039541 A CN202410039541 A CN 202410039541A CN 117551054 A CN117551054 A CN 117551054A
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- isopropanol
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- mbt
- material amine
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- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 title claims abstract description 101
- 238000000034 method Methods 0.000 title claims abstract description 25
- QAZLUNIWYYOJPC-UHFFFAOYSA-M sulfenamide Chemical compound [Cl-].COC1=C(C)C=[N+]2C3=NC4=CC=C(OC)C=C4N3SCC2=C1C QAZLUNIWYYOJPC-UHFFFAOYSA-M 0.000 title claims abstract description 20
- 238000004537 pulping Methods 0.000 title claims abstract description 18
- 150000001412 amines Chemical class 0.000 claims abstract description 59
- 239000002994 raw material Substances 0.000 claims abstract description 49
- 238000006243 chemical reaction Methods 0.000 claims abstract description 39
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000007800 oxidant agent Substances 0.000 claims abstract description 20
- 230000003647 oxidation Effects 0.000 claims abstract description 20
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 20
- 230000001590 oxidative effect Effects 0.000 claims abstract description 20
- 239000005708 Sodium hypochlorite Substances 0.000 claims abstract description 16
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims abstract description 16
- XTUSEBKMEQERQV-UHFFFAOYSA-N propan-2-ol;hydrate Chemical compound O.CC(C)O XTUSEBKMEQERQV-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 7
- PAFZNILMFXTMIY-UHFFFAOYSA-N cyclohexylamine Chemical compound NC1CCCCC1 PAFZNILMFXTMIY-UHFFFAOYSA-N 0.000 claims description 52
- YBRBMKDOPFTVDT-UHFFFAOYSA-N tert-butylamine Chemical group CC(C)(C)N YBRBMKDOPFTVDT-UHFFFAOYSA-N 0.000 claims description 22
- 239000012071 phase Substances 0.000 claims description 16
- 239000012074 organic phase Substances 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 9
- 238000004458 analytical method Methods 0.000 claims description 8
- 238000001704 evaporation Methods 0.000 claims description 8
- 238000000926 separation method Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- 239000012295 chemical reaction liquid Substances 0.000 claims description 4
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 claims description 4
- 238000004090 dissolution Methods 0.000 claims description 4
- 238000004817 gas chromatography Methods 0.000 claims description 3
- ZCXGMSGCBDSEOY-UHFFFAOYSA-N 2-benzothiazolsulfonic acid Chemical compound C1=CC=C2SC(S(=O)(=O)O)=NC2=C1 ZCXGMSGCBDSEOY-UHFFFAOYSA-N 0.000 abstract description 5
- 239000007791 liquid phase Substances 0.000 abstract description 3
- 238000004064 recycling Methods 0.000 abstract description 3
- 239000012752 auxiliary agent Substances 0.000 abstract description 2
- 229920001971 elastomer Polymers 0.000 abstract description 2
- 238000002360 preparation method Methods 0.000 abstract description 2
- YXIWHUQXZSMYRE-UHFFFAOYSA-N 1,3-benzothiazole-2-thiol Chemical compound C1=CC=C2SC(S)=NC2=C1 YXIWHUQXZSMYRE-UHFFFAOYSA-N 0.000 description 45
- 239000000047 product Substances 0.000 description 16
- 239000012452 mother liquor Substances 0.000 description 10
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 238000004073 vulcanization Methods 0.000 description 6
- 238000003756 stirring Methods 0.000 description 5
- IUJLOAKJZQBENM-UHFFFAOYSA-N n-(1,3-benzothiazol-2-ylsulfanyl)-2-methylpropan-2-amine Chemical compound C1=CC=C2SC(SNC(C)(C)C)=NC2=C1 IUJLOAKJZQBENM-UHFFFAOYSA-N 0.000 description 4
- 229920006395 saturated elastomer Polymers 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 238000007086 side reaction Methods 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- -1 benzothiazole sulfenamide compound Chemical class 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 150000003946 cyclohexylamines Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- DEQZTKGFXNUBJL-UHFFFAOYSA-N n-(1,3-benzothiazol-2-ylsulfanyl)cyclohexanamine Chemical compound C1CCCCC1NSC1=NC2=CC=CC=C2S1 DEQZTKGFXNUBJL-UHFFFAOYSA-N 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 238000004448 titration Methods 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)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention belongs to the field of rubber auxiliary agent preparation, and in particular relates to a method for improving the yield of a synthetic sulfenamide accelerator by pulping isopropanol, which comprises the following steps: 1) Adding MBT, isopropanol, water and raw material amine into a reaction container; 2) After the mixing is finished, adjusting the reaction temperature, dropwise adding sodium hypochlorite oxidant, stopping dropwise adding the oxidant after the end point of oxidation is reached, and ending the reaction. According to the technical scheme, the M-ammonium salt is dissolved in the liquid phase by utilizing the characteristic that the M-ammonium salt is easily dissolved in the isopropanol water solution, so that the problem that MBT is wrapped is avoided, and therefore, the large amine ratio is not used any more to protect the MBT from being oxidized into benzothiazole sulfonate. The amine addition ratio is reduced, and the energy source required by recycling the raw material amine can be effectively reduced.
Description
Technical Field
The invention belongs to the field of rubber auxiliary agent preparation, and particularly relates to a method for improving the yield of a synthetic sulfenamide accelerator by pulping isopropanol.
Background
The sulfenamide accelerator is a benzothiazole sulfenamide compound used as a vulcanization accelerator. Sulfenamide accelerators are the most rapidly developing accelerators currently. The length of scorch time and the rate of vulcanization of the sulfenamide accelerator are dependent on the nature of the amine in the accelerator molecule. The more basic the amine, the faster the vulcanization speed, the greater the steric hindrance of the amine, the longer the scorch time, and the lower the sulfur speed. The main varieties of sulfenamide accelerators include N-tert-butyl-2-benzothiazole sulfenamide (NS, TBBS) and N-cyclohexyl-2-benzothiazole sulfenamide (CZ, CBS).
The N-tertiary butyl-2-benzothiazolyl sulfenamide has the advantages of low toxicity, high efficiency, safety at the operation temperature, strong scorch resistance, high vulcanization speed, high stretching stress and the like, and is called as a standard accelerator. With the increase of tire yield and tire meridian rate, the use amount of the accelerator has been gradually increased in recent years; at present, the domestic production scheme is generally a sodium hypochlorite oxidation method, wherein MBT (2-mercaptobenzothiazole) is adopted as a raw material, and is mixed with a tert-butylamine aqueous solution, and an oxidant is dripped for oxidation, and the oxidant is mainly sodium hypochlorite. However, when sodium hypochlorite is used for oxidation, the raw material MBT can produce side reaction to produce benzothiazole sulfonate, so that the feeding ratio of tert-butylamine needs to be increased, so that MBT and excessive tert-butylamine firstly produce tert-butylamine salt of MBT, and the raw material MBT in a reaction system is protected from being oxidized into byproducts by an oxidant, thereby achieving the purpose of improving the product yield. At present, the proper molar ratio of the feed to the domestic manufacturer is tert-butylamine: mbt=3.5:1. The excess tert-butylamine needs to be recovered by distillation, and a large amount of energy is consumed by evaporating the excess tert-butylamine, which belongs to a high energy consumption process.
The N-cyclohexyl-2-benzothiazole secondary yellow amide is a slow-acting vulcanization accelerator widely used at home and abroad, and has the advantages of short vulcanization time and excellent scorch resistance. At present, the domestic production scheme is generally a sodium hypochlorite oxidation method and a hydrogen peroxide and sodium hypochlorite mixed oxidation method, wherein MBT (2-mercaptobenzothiazole) is adopted as a raw material, and is mixed with cyclohexylamine aqueous solution, and oxidant is dropwise added for oxidation, and the oxidant mainly adopts sodium hypochlorite or hydrogen peroxide; however, when sodium hypochlorite or hydrogen peroxide is used for oxidation, the raw material MBT can generate side reaction to produce benzothiazole sulfonate, so that the feeding ratio of the cyclohexylamine needs to be increased, so that MBT and excessive cyclohexylamine firstly generate the cyclohexylamine salt of MBT, and the raw material MBT in a reaction system is protected from being oxidized into byproducts by an oxidant, thereby achieving the purpose of improving the product yield. At present, the proper feeding mole ratio of domestic manufacturers is cyclohexylamine: mbt=2.2:1. The excessive cyclohexylamine needs to be recovered by distillation, and evaporation of the excessive cyclohexylamine consumes a large amount of energy due to azeotropy of the cyclohexylamine and water, and belongs to a high energy consumption process.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a method for improving the yield of a synthetic sulfenamide accelerator by pulping isopropanol.
In order to achieve the above purpose, the invention adopts the following technical scheme:
a method for improving the yield of a synthesized sulfenamide accelerator by pulping isopropanol comprises the following steps:
1) Adding MBT, isopropanol, water and raw material amine into a reaction container;
2) After the mixing is finished, adjusting the reaction temperature, dropwise adding sodium hypochlorite oxidant, stopping dropwise adding the oxidant after the end point of oxidation is reached, and ending the reaction.
The raw material amine is tert-butylamine or cyclohexylamine.
When the raw material amine is tert-butylamine, the mass ratio of the isopropanol to the water is 1:2-2.4, preferably 1:2.2; when the raw material amine is cyclohexylamine, the mass ratio of the isopropanol to the water is 1:2-2.2, preferably 1:2.1.
When the mass ratio of the isopropanol to the water is less than 1:2, the centrifugal liquid after the reaction is difficult to separate, and the organic phase cannot be used in the follow-up process. When the mass ratio of isopropyl alcohol to water is greater than 1:2.5, a large amount of product is dissolved before the mother liquor is saturated, so that a large amount of mother liquor needs to be treated later to recover the product.
When the raw material amine is tert-butylamine, the mass ratio of MBT to isopropanol is 1:3-3.6, preferably 1:3.3; when the raw material amine is cyclohexylamine, the mass ratio of MBT to isopropanol is 1:4-4.4, preferably 1:4.2.
when the starting amine is tert-butylamine, the molar ratio of MBT to starting amine is 1:1.3-1.7, preferably 1:1.5; when the starting amine is cyclohexylamine, the molar ratio of MBT to starting amine is 1:1.1-1.3, preferably 1:1.2.
when the raw material amine is tert-butylamine, the reaction temperature in the step 2) is 35-40 ℃; when the starting amine is cyclohexylamine, the reaction temperature in step 2) is 40-45 ℃.
After the mixing in the step 2), firstly adjusting to a dissolution temperature, stirring for 0.5-2h, and then adjusting to a reaction temperature; the dissolution temperature is 5-15 ℃ higher than the reaction temperature.
After the reaction is finished, the separated organic phase is used. Specifically, performing gas chromatographic analysis on the separated organic phase, and supplementing MBT, isopropanol and raw material amine to initiate the reaction proportion of each component according to an analysis result;
when the raw material amine is tert-butylamine, evaporating the water phase after liquid separation to recover the raw material amine, and continuously recovering the residual water phase to obtain an isopropanol water solution;
when the raw material amine is cyclohexylamine, evaporating the water phase after liquid separation to recover the isopropanol water solution, and continuously recovering the residual water phase to obtain the raw material amine.
The judgment mode of the oxidation end point is as follows: when the sodium hypochlorite oxidant is over, a small amount of reaction liquid is taken, and 2-5% copper acetate is used for detecting the oxidation end point.
Compared with the prior art, the invention has the beneficial effects that:
according to the technical scheme, the M-ammonium salt is dissolved in the liquid phase by utilizing the characteristic that the M-ammonium salt is easily dissolved in the isopropanol water solution, so that the problem that MBT is wrapped is avoided, and therefore, the large amine ratio is not used any more to protect the MBT from being oxidized into benzothiazole sulfonate. The amine addition ratio is reduced, and the energy source required by recycling the raw material amine can be effectively reduced. In addition, the centrifuge after the reaction is separated into two phases due to the presence of isopropyl alcohol. The mother liquor of the upper layer can be used mechanically, and the salt water phase of the lower layer is distilled to recover the isopropanol and the raw material amine.
Detailed Description
The present invention will be further described in detail with reference to examples for better understanding of the technical scheme of the present invention by those skilled in the art.
Examples 1 to 3
A method for improving the yield of a synthetic TBBS promoter by pulping isopropanol, which comprises the following steps:
1) Sequentially adding MBT, isopropanol, water and tert-butylamine into a reaction kettle; the molar ratio of MBT to raw material amine is 1:1.3-1.7, and can be specifically 1:1.3, 1:1.5, 1:1.7, 1:1.5 is exemplified as a preferred example.
2) After mixing, the slurry temperature in the kettle is raised to 40-45 ℃ (specifically 40 ℃, 42 ℃ and 45 ℃ are taken as a preferred embodiment for description, the step is to facilitate the dispersion of the M-ammonium salt), after stirring for 1 hour, the material temperature in the kettle is lowered to 35-40 ℃ (specifically 35 ℃, 38 ℃ and 40 ℃, and 40 ℃ is taken as a preferred embodiment for description;
dropwise adding sodium hypochlorite oxidant, taking a small amount of reaction liquid when the sodium hypochlorite oxidant is subjected to titration, detecting an oxidation end point by using 2-5% copper acetate, stopping dropwise adding the oxidant after the oxidation end point is reached, continuously stirring for 10 minutes, retesting the oxidation end point, and stopping the reaction after the reaction is qualified;
after the reaction, the organic phase liquid chromatograph analyzes the product composition.
1. The reaction results were examined at different amine ratios, and table 1 shows the mass and mass ratio of the raw materials added in step 1), and table 2 shows the conversion of MBT, the yield of the product, and the purity of the crystals, which were obtained correspondingly.
TABLE 1
TABLE 2
Considering the mass ratio of MBT to isopropanol as 1:3.3, molar ratio of MBT to starting amine 1:1.5, the product yield and the purity of the crystallized product reach the best, and meet the quality requirement of national standard products, so that the mother liquor is used as a preferable example for application.
2. The saturated mother liquor is used mechanically for investigation;
the separated organic phase is used mechanically, firstly, the separated organic phase is subjected to gas chromatography analysis, and MBT, isopropanol and raw material amine are supplemented according to the analysis result to the initial reaction proportion of each component (in the embodiment, isopropanol is supplemented according to the mass ratio of MBT to isopropanol of 1:3.3, tert-butylamine is supplemented according to the mole ratio of MBT to raw material amine of 1:1.5, and raw material MBT is supplemented simultaneously); evaporating the water phase after liquid separation to recover the raw material amine, and continuously recovering the residual water phase to obtain the isopropanol water solution.
The application was continued for 30 total application cycles per 5 sample mix analyses, the application results are shown in Table 3, the mass ratio of isopropanol to MBT in Table 3, and the amine addition ratio was the molar ratio of tert-butylamine to MBT.
TABLE 3 Table 3
After the mother liquor is reused for 30 times, the yield and the product quality are not reduced, and the reuse requirement is met.
Examples 4 to 6
A method for improving the yield of a synthetic CBS promoter by pulping isopropanol, which comprises the following steps:
1) Sequentially adding water, MBT, isopropanol and cyclohexylamine into a reaction kettle; the molar ratio of MBT to cyclohexylamine is 1:1.1-1.3, and can be specifically 1:1.1, 1:1.2, 1:1.3, 1:1.2 is exemplified as a preferred example.
2) After mixing, the slurry temperature in the kettle is raised to 50-60 ℃ (specifically 50 ℃, 55 ℃, 60 ℃ and 60 ℃ are used as a preferred embodiment for the purpose of facilitating the dispersion of the M-ammonium salt), and after stirring for 1 hour, the material temperature in the kettle is lowered to 40-45 ℃ (specifically 40 ℃, 42 ℃ and 45 ℃ are used as a preferred embodiment for the purpose of the description);
and (3) dropwise adding sodium hypochlorite oxidant, taking a small amount of reaction liquid when the sodium hypochlorite oxidant is titrated, detecting an oxidation end point by using 2-5% copper acetate, stopping dropwise adding the oxidant after the oxidation end point is reached, continuously stirring for 10 minutes, retesting the oxidation end point, and stopping the reaction after the reaction is qualified.
After the reaction, the organic phase liquid chromatograph analyzes the product composition.
1. Examine the data analyzed at different amine throw ratios: table 4 shows the mass and mass ratio of the raw materials added in step 1), and Table 5 shows the conversion, product yield and crystal purity of the corresponding MBT.
TABLE 4 Table 4
TABLE 5
Considering the mass ratio of MBT to isopropanol as 1:4.2, molar ratio of MBT to cyclohexylamine is 1:1.2, the product yield and the purity of the crystallized product reach the best, and meet the quality requirements of national standard products; therefore, the mother liquor is applied as a preferable example.
2. Inspection of saturated mother liquor
The separated organic phase is used mechanically, firstly, the separated organic phase is subjected to gas chromatography analysis, and MBT, isopropanol and raw material amine are supplemented according to the analysis result to the initial reaction proportion of each component (in the embodiment, isopropanol is supplemented according to the mass ratio of MBT to isopropanol of 1:4.2, cyclohexylamine is supplemented according to the molar ratio of MBT to raw material amine of 1:1.2, and raw material MBT is supplemented simultaneously); evaporating the water phase after liquid separation to recover the isopropanol water solution, and continuously recovering the residual water phase to obtain the raw material amine.
The application was continued for 30 total application cycles per 5 sample mix analyses, the application results are shown in Table 6, the mass ratio of isopropanol to MBT in Table 6, and the amine addition ratio was the molar ratio of cyclohexylamine to MBT.
TABLE 6
After the mother liquor is reused for 30 times, the yield and the product quality are not reduced, and the reuse requirement is met.
In summary, the technical scheme of the application utilizes the characteristic that the M-ammonium salt is easily dissolved in isopropanol water solution, and the M-ammonium salt is dissolved in liquid phase, so that the problem that MBT is wrapped is avoided, and therefore, a large amine ratio is not used any more to protect the MBT from being oxidized into benzothiazole sulfonate. The amine addition ratio is reduced, so that the energy source required for recycling the cyclohexylamine can be effectively reduced. In addition, the centrifuge after the reaction is separated into two phases due to the presence of isopropyl alcohol. The mother liquor of the upper layer can be used mechanically, and the salt water phase of the lower layer is distilled to recover the isopropanol and the cyclohexylamine.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (10)
1. The method for improving the yield of the synthesized sulfenamide accelerator by pulping isopropanol is characterized by comprising the following steps of:
1) Adding MBT, isopropanol, water and raw material amine into a reaction container;
2) After the mixing is finished, adjusting the reaction temperature, dropwise adding sodium hypochlorite oxidant, stopping dropwise adding the oxidant after the end point of oxidation is reached, and ending the reaction.
2. The method for improving the yield of the synthesized sulfenamide accelerator by pulping isopropanol according to claim 1, wherein the raw material amine is tert-butylamine or cyclohexylamine.
3. The method for improving the yield of the synthesized sulfenamide accelerator by pulping isopropanol according to claim 2, which is characterized in that when the raw material amine is tert-butylamine, the mass ratio of the isopropanol to water is 1:2-2.4; when the raw material amine is cyclohexylamine, the mass ratio of the isopropanol to the water is 1:2-2.2.
4. The method for improving the yield of the synthesized sulfenamide accelerator by pulping isopropanol according to claim 2, wherein when the raw material amine is tert-butylamine, the mass ratio of MBT to isopropanol is 1:3-3.6; when the raw material amine is cyclohexylamine, the mass ratio of MBT to isopropanol is 1:4-4.4.
5. The method for improving the yield of the synthesized sulfenamide accelerator by pulping isopropanol according to claim 2, wherein when the raw material amine is tert-butylamine, the molar ratio of MBT to the raw material amine is 1:1.3-1.7; when the raw material amine is cyclohexylamine, the molar ratio of MBT to the raw material amine is 1:1.1-1.3.
6. The method for improving the yield of the synthesized sulfenamide accelerator by pulping isopropanol according to claim 3, wherein when the raw material amine is tert-butylamine, the reaction temperature in the step 2) is 35-40 ℃; when the starting amine is cyclohexylamine, the reaction temperature in step 2) is 40-45 ℃.
7. The method for improving the yield of the synthesized sulfenamide accelerator by pulping isopropanol according to claim 1, which is characterized in that after the mixing is finished, the mixture is firstly adjusted to a dissolution temperature, stirred for 0.5-2h, and then adjusted to a reaction temperature; the dissolution temperature is 5-15 ℃ higher than the reaction temperature.
8. The method for improving the yield of the synthesized sulfenamide accelerator by pulping isopropanol according to claim 1, wherein after the reaction is finished, the separated organic phase is used.
9. The method for improving the yield of the synthesized sulfenamide accelerator by pulping isopropanol according to claim 8, which is characterized in that the separated organic phase is subjected to gas chromatography, and MBT, isopropanol and raw material amine are supplemented to the initial reaction proportion of each component according to the analysis result;
when the raw material amine is tert-butylamine, evaporating the water phase after liquid separation to recover the raw material amine, and continuously recovering the residual water phase to obtain an isopropanol water solution;
when the raw material amine is cyclohexylamine, evaporating the water phase after liquid separation to recover the isopropanol water solution, and continuously recovering the residual water phase to obtain the raw material amine.
10. The method for improving the yield of the synthesized sulfenamide accelerator by pulping isopropanol according to claim 1, wherein the judgment method of the oxidation end point is as follows: when the sodium hypochlorite oxidant is over, a small amount of reaction liquid is taken, and 2-5% copper acetate is used for detecting the oxidation end point.
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