CN116102520A - Method for synthesizing accelerator MBTS (DM) by oxygen oxidation method - Google Patents
Method for synthesizing accelerator MBTS (DM) by oxygen oxidation method Download PDFInfo
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- CN116102520A CN116102520A CN202211638364.3A CN202211638364A CN116102520A CN 116102520 A CN116102520 A CN 116102520A CN 202211638364 A CN202211638364 A CN 202211638364A CN 116102520 A CN116102520 A CN 116102520A
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 113
- 239000001301 oxygen Substances 0.000 title claims abstract description 113
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 113
- 238000000034 method Methods 0.000 title claims abstract description 72
- AFZSMODLJJCVPP-UHFFFAOYSA-N dibenzothiazol-2-yl disulfide Chemical compound C1=CC=C2SC(SSC=3SC4=CC=CC=C4N=3)=NC2=C1 AFZSMODLJJCVPP-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 230000003647 oxidation Effects 0.000 title claims abstract description 17
- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 17
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 39
- 239000000047 product Substances 0.000 claims abstract description 39
- 239000003054 catalyst Substances 0.000 claims abstract description 24
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 18
- FBZONXHGGPHHIY-UHFFFAOYSA-N xanthurenic acid Chemical group C1=CC=C(O)C2=NC(C(=O)O)=CC(O)=C21 FBZONXHGGPHHIY-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000001816 cooling Methods 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 9
- 238000001914 filtration Methods 0.000 claims abstract description 9
- 229910052751 metal Inorganic materials 0.000 claims abstract description 7
- 239000002184 metal Substances 0.000 claims abstract description 7
- 238000006479 redox reaction Methods 0.000 claims abstract description 5
- 238000007873 sieving Methods 0.000 claims abstract description 3
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 claims description 20
- 238000002844 melting Methods 0.000 claims description 15
- 230000008018 melting Effects 0.000 claims description 15
- 239000002904 solvent Substances 0.000 claims description 13
- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(I) oxide Inorganic materials [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 claims description 10
- KRFJLUBVMFXRPN-UHFFFAOYSA-N cuprous oxide Chemical compound [O-2].[Cu+].[Cu+] KRFJLUBVMFXRPN-UHFFFAOYSA-N 0.000 claims description 10
- 229940112669 cuprous oxide Drugs 0.000 claims description 10
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 9
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 claims description 7
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 description 5
- 239000011572 manganese Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 description 4
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 3
- KBTJYNAFUYTSNN-UHFFFAOYSA-N [Na].OO Chemical compound [Na].OO KBTJYNAFUYTSNN-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 125000000468 ketone group Chemical group 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000013040 rubber vulcanization Methods 0.000 description 2
- 235000010288 sodium nitrite Nutrition 0.000 description 2
- 238000011179 visual inspection Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- BWGNESOTFCXPMA-UHFFFAOYSA-N Dihydrogen disulfide Chemical compound SS BWGNESOTFCXPMA-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- 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
- C07D277/78—Sulfur atoms attached to a second hetero atom to a second sulphur atom
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Catalysts (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for synthesizing an accelerator MBTS (DM) by an oxygen oxidation method. The invention comprises the following steps: sequentially adding a main catalyst and a cocatalyst into the molten MBT, wherein the main catalyst is 4, 8-dihydroxyquinoline-2-formic acid, the cocatalyst is a metal catalyst capable of undergoing oxidation-reduction reaction, after the temperature is raised to a certain temperature, oxygen with certain pressure is introduced into an oxygen supply system, then the oxygen circularly flows in the oxygen supply system and a reaction kettle, and when the pressure in the reaction kettle is not reduced any more, the reaction is ended, so that a reaction product is obtained; and then filtering, cooling, drying, crushing and sieving the reaction product in sequence to obtain the MBTS (DM) product. The method for synthesizing the accelerator MBTS (DM) by the oxygen oxidation method has the advantage of environmental protection, and the purity of the prepared product is higher.
Description
Technical Field
The invention relates to the technical field of rubber vulcanization accelerator MBTS (DM) production processes, in particular to a method for synthesizing accelerator MBTS (DM) by an oxygen oxidation method.
Background
At present, main processes for producing the rubber vulcanization accelerator MBTS (DM) at home and abroad include a sodium nitrite method, a solvent method and a hydrogen peroxide sodium salt method. The sodium nitrite method has low cost and low equipment requirement, but the generated nitrogen oxides are difficult to treat and pollute the environment, and the situation of elimination is faced; the solvent method belongs to an environment-friendly process, but the solvent consumption of a ton of products is more than 50kg, the environment is polluted, and meanwhile, the energy consumption is high and the production cost is high; the hydrogen peroxide sodium salt method process is also an environment-friendly process and has good product quality, but a large amount of waste water and waste salt can be generated, so that a large environment-friendly risk is increased for enterprises, and the subsequent three-waste treatment cost is high.
Therefore, the invention develops a method for synthesizing the accelerator MBTS (DM) by using an oxygen oxidation method with better environmental protection.
Disclosure of Invention
The invention aims to provide a method for synthesizing an accelerator MBTS (DM) by an oxygen oxidation method.
The invention aims at realizing the following technical scheme:
a method for synthesizing accelerator MBTS (DM) by an oxygen oxidation method, which comprises the following steps: sequentially adding a main catalyst and a cocatalyst into the molten MBT, wherein the main catalyst is 4, 8-dihydroxyquinoline-2-formic acid, the cocatalyst is a metal catalyst capable of undergoing oxidation-reduction reaction, after the temperature is raised to a certain temperature, oxygen with certain pressure is introduced into an oxygen supply system, then the oxygen circularly flows in the oxygen supply system and a reaction kettle, and when the pressure in the reaction kettle is not reduced any more, the reaction is ended, so that a reaction product is obtained; and then filtering, cooling, drying, crushing and sieving the reaction product in sequence to obtain the MBTS (DM) product. When the pressure in the reaction kettle is no longer reduced, the oxygen in the oxygen supply system is not consumed any more, and therefore, when the pressure in the reaction kettle is no longer reduced, the time of ending the reaction is the time.
Preferably, the promoter is one or more of manganese oxide, iron oxide and cuprous oxide.
Preferably, the addition amount of the 4, 8-dihydroxyquinoline-2-formic acid accounts for 1 to 2 per mill of the mass of the MBT; the addition amount of the cocatalyst accounts for 0.1 to 0.2 per mill of the mass of the MBT.
Preferably, after the temperature is raised to 170-180 ℃, oxygen with a certain pressure is introduced into the oxygen supply system.
Preferably, oxygen is fed to the oxygen supply system at a pressure of 0.1MPa to 1.0 MPa.
Preferably, the oxygen supply system comprises an oxygen storage tank, a pipeline and a high-pressure pump, wherein the oxygen storage tank is respectively and fixedly connected with a reaction kettle and an oxygen source through pipelines, a control valve is fixedly arranged on the pipeline connecting the oxygen storage tank and the oxygen source, the reaction kettle is fixedly connected with the high-pressure pump through the pipeline, and the high-pressure pump is fixedly connected with the oxygen storage tank through the pipeline; after oxygen with the pressure of 0.1MPa-1.0MPa is introduced into the oxygen supply system, the high-pressure pump is started, so that the oxygen circularly flows in the oxygen supply system.
Preferably, the MBT in the molten state is a finished product obtained by purification by an acid-base method or a solvent method, and the finished product is melted at a temperature of between 170 and 180 ℃.
Beneficial technical effects
The invention adopts oxygen, a main catalyst (4, 8-dihydroxyquinoline-2-formic acid) and a cocatalyst (a metal catalyst capable of carrying out oxidation-reduction reaction) to carry out oxidation synthesis, and belongs to a clean and environment-friendly process. The purity and quality of the MBTS (DM) product prepared by the method reach ideal effects, and the recovered catalyst can be reused.
The invention thoroughly solves the bottleneck of the process for synthesizing MBTS (DM) by taking molten MBT as a raw material through reaction route and process parameter design, and is a novel clean and environment-friendly process. The novel green environment-friendly process is also applicable to MBT with low purity obtained by a solvent method. For MBT obtained by a solvent method, the initial melting point of the MBTS (DM) product synthesized by the method is more than or equal to 166.5 ℃ (U-shaped capillary visual inspection method), and the purity of the MBTS (DM) product is more than or equal to 97.5%, and can reach 97.817% at most; the initial melting point of the MBTS (DM) product synthesized by the method using the acid-base MBT as the raw material is more than or equal to 168.5 ℃ (U-shaped capillary visual inspection method), and the purity of the MBTS (DM) product is more than or equal to 98.497 percent and can reach 99.029 percent at most.
In the present invention, the cocatalyst is a metal catalyst capable of undergoing oxidation-reduction reaction, and the mechanism of participation of the metal cations in the reaction is consistent, so that the reaction mechanism is explained by taking metal Mn ions as a representative in the present application, and specifically shown as follows:
oxygen in this application will Mn 2+ Oxidation to Mn n+ (4≥n>2) Is itself reduced to O 2- ；
Mn n+ (4≥n>2) The two hydroxyls on the 4, 8-dihydroxyquinoline-2-formic acid are oxidized into two ketone groups, the 2-carboxylic acid quinoline derivative with the hydroxyls changed into the ketone groups has stronger oxidizing property, MBT in a molten state is unstable, the formed MBT free radicals form symmetrical Disulfide MBTS (DM) under the oxidizing action of the 2-carboxylic acid quinoline derivative, and the oxygen participating in the reaction finally generates water.
Drawings
FIG. 1 is a schematic diagram of the connection between an oxygen supply system and an autoclave in the present application;
fig. 2 to 7 are liquid chromatograms of the first to sixth embodiments, respectively.
In the figure: 1. an oxygen source, 2, a control valve, 3, an oxygen storage tank, 4, a pipeline, 5, a reaction kettle, 6 and a high-pressure pump.
Detailed Description
The English names commonly used in the field of accelerator MBTS (DM) are MBTS and DM, and the product names of the accelerator MBTS (DM) in the six attached drawings provided by the application are marked by DM.
Embodiment one: adding 600g of molten MBT into an autoclave with the volume of 2L, sequentially adding 0.6g of a main catalyst and 0.06g of a cocatalyst into the autoclave, wherein the main catalyst is 4, 8-dihydroxyquinoline-2-formic acid, the cocatalyst is manganese oxide, heating to 170 ℃, opening a control valve 2 arranged on a pipeline 4 connecting an oxygen storage tank 3 and an oxygen source 1 after the temperature is stabilized to 170 ℃, introducing oxygen with the pressure of 0.1MPa into the oxygen storage tank 3 of an oxygen supply system by utilizing the oxygen source 1, closing the control valve 2, opening a high-pressure pump 6, circularly flowing the oxygen in the oxygen supply system and the reaction kettle 5 under the action of the high-pressure pump 6, and ending the reaction when the pressure in the reaction kettle 5 is not reduced any more, thus obtaining a reaction product; and then filtering, cooling, drying and crushing the reaction product in sequence to obtain an MBTS (DM) product, and measuring the initial melting point of the MBTS (DM) product at 168.5 ℃ and the purity of 98.497%. In the first embodiment, the MBT in the molten state is a product obtained by purifying the MBT by an acid-base method, and melting the MBT at 180 ℃.
Embodiment two: 600g of molten MBT is put into an autoclave with the volume of 2L, then 1.2g of main catalyst and 0.12g of cocatalyst are sequentially put into the autoclave, the main catalyst is 4, 8-dihydroxyquinoline-2-formic acid, the cocatalyst is manganese oxide, then the temperature is raised to 175 ℃, after the temperature is stabilized to 175 ℃, a control valve 2 arranged on a pipeline 4 connecting an oxygen storage tank 3 and an oxygen source 1 is opened, oxygen with the pressure of 0.2MPa is introduced into the oxygen storage tank 3 of an oxygen supply system by utilizing the oxygen source 1, then the control valve 2 is closed, then a high-pressure pump 6 is started, the oxygen circularly flows in the oxygen supply system and the reaction kettle 5 under the action of the high-pressure pump 6, and when the pressure in the reaction kettle 5 is no longer reduced, the reaction is ended, and a reaction product is obtained; and then filtering, cooling, drying and crushing the reaction product in sequence to obtain an MBTS (DM) finished product, and measuring the initial melting point 166.5 ℃ and the purity 97.495% of the MBTS (DM) finished product. In the second embodiment, the MBT of the solvent method is obtained by purifying a finished product by the solvent method and melting the finished product at a temperature of 170 ℃.
Embodiment III: 1000g of MBT in a molten state is put into an autoclave with a volume of 2L, and then 1.5g of main catalyst and 0.15g of cocatalyst are sequentially put into the autoclave; the main catalyst is 4, 8-dihydroxyquinoline-2-formic acid, the cocatalyst is a mixture of ferric oxide and cuprous oxide, and the mass of the ferric oxide and the cuprous oxide is 0.075g respectively; then heating to 175 ℃, after the temperature is stabilized to 175 ℃, opening a control valve 2 arranged on a pipeline 4 connecting an oxygen storage tank 3 and an oxygen source 1, introducing oxygen with the pressure of 0.5MPa into the oxygen storage tank 3 of an oxygen supply system by using the oxygen source 1, then closing the control valve 2, then opening a high-pressure pump 6, and under the action of the high-pressure pump 6, enabling the oxygen to circularly flow in the oxygen supply system and a reaction kettle 5, and ending the reaction when the pressure in the reaction kettle 5 is not reduced any more, thus obtaining a reaction product; and then filtering, cooling, drying and crushing the reaction product in sequence to obtain an MBTS (DM) finished product, and measuring the initial melting point 169.1 ℃ and the purity 98.846% of the MBTS (DM) finished product. In the third embodiment, the MBT in the molten state is a finished product obtained by purifying by an acid-base method, and melting the finished product at a temperature of 175 ℃.
Embodiment four: putting 900g of molten MBT into an autoclave with a volume of 2L, sequentially putting 0.9g of a main catalyst and 0.09g of a cocatalyst into the autoclave, wherein the main catalyst is 4, 8-dihydroxyquinoline-2-formic acid, the cocatalyst is a mixture of manganese oxide, ferric oxide and cuprous oxide, the mass of each of the manganese oxide, the ferric oxide and the cuprous oxide is 0.03g, then heating to 177 ℃, after the temperature is stabilized to 177 ℃, opening a control valve 2 arranged on a pipeline 4 connecting an oxygen storage tank 3 and an oxygen source 1, introducing oxygen with a pressure of 0.7MPa into the oxygen storage tank 3 of an oxygen supply system by utilizing the oxygen source 1, then closing the control valve 2, then opening a high-pressure pump 6, circularly flowing the oxygen in the oxygen supply system and the reaction kettle 5 under the action of the high-pressure pump 6, and ending the reaction when the pressure in the reaction kettle 5 is not reduced any more, thus obtaining a reaction product; and then filtering, cooling, drying and crushing the reaction product in sequence to obtain an MBTS (DM) finished product, and measuring the initial melting point 166.8 ℃ and the purity 97.697% of the MBTS (DM) finished product. In the fourth embodiment, the MBT of the solvent method is obtained by purifying a finished product by the solvent method and melting the finished product at a temperature of 170 ℃.
Fifth embodiment: 1000g of MBT in a molten state is put into an autoclave with a volume of 2L, and then 1g of main catalyst and 0.1g of cocatalyst are sequentially put into the autoclave; wherein the main catalyst is 4, 8-dihydroxyquinoline-2-formic acid, the cocatalyst is a mixture of manganese oxide and cuprous oxide, and the mass of the manganese oxide and the cuprous oxide is 0.05g respectively; then heating to 180 ℃, opening a control valve 2 arranged on a pipeline 4 connecting an oxygen storage tank 3 and an oxygen source 1 after the temperature is stabilized to 180 ℃, introducing oxygen with the pressure of 1.0MPa into the oxygen storage tank 3 of an oxygen supply system by using the oxygen source 1, closing the control valve 2, then opening a high-pressure pump 6, and circularly flowing the oxygen in the oxygen supply system and a reaction kettle 5 under the action of the high-pressure pump 6, wherein when the pressure in the reaction kettle 5 is not reduced any more, the reaction is ended, and a reaction product is obtained; and then filtering, cooling, drying and crushing the reaction product in sequence to obtain an MBTS (DM) finished product, and measuring the initial melting point 169.7 ℃ and the purity 99.029% of the MBTS (DM) finished product. In the fifth embodiment, the MBT in the molten state is a finished product obtained by purifying by an acid-base method, and melting the finished product at a temperature of 180 ℃.
Example six: 900g of MBT in a molten state was put into an autoclave having a volume of 2L, and then 0.9g of the recovered procatalyst and 0.09g of the recovered cocatalyst were sequentially put into the autoclave; wherein the main catalyst is 4, 8-dihydroxyquinoline-2-formic acid, the cocatalyst is a mixture of recovered manganese oxide, recovered ferric oxide and recovered cuprous oxide, and the mass of the manganese oxide, the ferric oxide and the cuprous oxide is 0.03g respectively; then heating to 180 ℃, opening a control valve 2 arranged on a pipeline 4 connecting an oxygen storage tank 3 and an oxygen source 1 after the temperature is stabilized to 180 ℃, introducing oxygen with the pressure of 0.1MPa into the oxygen storage tank 3 of an oxygen supply system by using the oxygen source 1, closing the control valve 2, then opening a high-pressure pump 6, and circularly flowing the oxygen in the oxygen supply system and a reaction kettle 5 under the action of the high-pressure pump 6, wherein when the pressure in the reaction kettle 5 is not reduced any more, the reaction is ended, and a reaction product is obtained; and then filtering, cooling, drying and crushing the reaction product in sequence to obtain an MBTS (DM) finished product, and measuring the initial melting point 167.1 ℃ and the purity 97.817% of the MBTS (DM) finished product. In the sixth embodiment, the MBT of the solvent method is obtained by purifying a product by the solvent method and melting the product at a temperature of 170 ℃.
Claims (7)
1. A method for synthesizing accelerator MBTS (DM) by an oxygen oxidation method is characterized in that: the method comprises the following steps: sequentially adding a main catalyst and a cocatalyst into the molten MBT, wherein the main catalyst is 4, 8-dihydroxyquinoline-2-formic acid, the cocatalyst is a metal catalyst capable of undergoing oxidation-reduction reaction, after the temperature is raised to a certain temperature, oxygen with certain pressure is introduced into an oxygen supply system, then the oxygen circularly flows in the oxygen supply system and a reaction kettle, and when the pressure in the reaction kettle is not reduced any more, the reaction is ended, so that a reaction product is obtained; and then filtering, cooling, drying, crushing and sieving the reaction product in sequence to obtain the MBTS (DM) product.
2. The method for synthesizing the accelerator MBTS (DM) by an oxygen oxidation method according to claim 1, wherein the method comprises the following steps: the promoter is one or more of manganese oxide, ferric oxide and cuprous oxide.
3. The method for synthesizing the accelerator MBTS (DM) by an oxygen oxidation method according to claim 1, wherein the method comprises the following steps: the addition amount of the 4, 8-dihydroxyquinoline-2-formic acid accounts for 1 to 2 per mill of the mass of the MBT; the addition amount of the cocatalyst accounts for 0.1 to 0.2 per mill of the mass of the MBT.
4. The method for synthesizing the accelerator MBTS (DM) by an oxygen oxidation method according to claim 1, wherein the method comprises the following steps: after the temperature is raised to 170-180 ℃, oxygen with certain pressure is introduced into the oxygen supply system.
5. The method for synthesizing the accelerator MBTS (DM) by an oxygen oxidation method according to claim 1, wherein the method comprises the following steps: oxygen with the pressure of 0.1MPa to 1.0MPa is introduced into the oxygen supply system.
6. The method for synthesizing the accelerator MBTS (DM) by an oxygen oxidation method according to claim 1, wherein the method comprises the following steps: the oxygen supply system comprises an oxygen storage tank, a pipeline and a high-pressure pump, wherein the oxygen storage tank is respectively and fixedly connected with a reaction kettle and an oxygen source through pipelines, a control valve is fixedly arranged on the pipeline connecting the oxygen storage tank and the oxygen source, the reaction kettle is fixedly connected with the high-pressure pump through the pipeline, and the high-pressure pump is fixedly connected with the oxygen storage tank through the pipeline; after oxygen with the pressure of 0.1MPa-1.0MPa is introduced into the oxygen supply system, the high-pressure pump is started, so that the oxygen circularly flows in the oxygen supply system.
7. The method for synthesizing the accelerator MBTS (DM) by an oxygen oxidation method according to claim 1, wherein the method comprises the following steps: the molten MBT is a finished product obtained by purifying by an acid-base method or a solvent method, and the finished product is obtained by melting at a temperature of 170-180 ℃.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1994015927A1 (en) * | 1992-12-30 | 1994-07-21 | Monsanto Company | Catalytic oxidation process |
| CN105175353A (en) * | 2015-10-15 | 2015-12-23 | 内蒙古科迈化工有限公司 | Method for performing ammonolysis on oxygen to obtain rubber accelerator MBT by oxidization-synthesis |
| CN113603656A (en) * | 2021-10-08 | 2021-11-05 | 科迈化工股份有限公司 | Production process of rubber vulcanization accelerator MBTS |
-
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- 2022-12-19 CN CN202211638364.3A patent/CN116102520B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1994015927A1 (en) * | 1992-12-30 | 1994-07-21 | Monsanto Company | Catalytic oxidation process |
| CN105175353A (en) * | 2015-10-15 | 2015-12-23 | 内蒙古科迈化工有限公司 | Method for performing ammonolysis on oxygen to obtain rubber accelerator MBT by oxidization-synthesis |
| CN113603656A (en) * | 2021-10-08 | 2021-11-05 | 科迈化工股份有限公司 | Production process of rubber vulcanization accelerator MBTS |
Non-Patent Citations (1)
| Title |
|---|
| 蒋士峰;黎振球;: "2-硫醇基苯并噻唑铵盐氧气氧化法制备2, 2\'-二硫代二苯并噻唑", 合成橡胶工业, no. 05, 15 September 2015 (2015-09-15) * |
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