CN111072542A - Method for continuously producing diisobutyronitrile peroxide by multi-point feeding and intensive mixing - Google Patents
Method for continuously producing diisobutyronitrile peroxide by multi-point feeding and intensive mixing Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 28
- 238000002156 mixing Methods 0.000 title claims abstract description 23
- 150000002978 peroxides Chemical class 0.000 title description 2
- DGMOBVGABMBZSB-UHFFFAOYSA-N 2-methylpropanoyl chloride Chemical compound CC(C)C(Cl)=O DGMOBVGABMBZSB-UHFFFAOYSA-N 0.000 claims abstract description 55
- 238000006243 chemical reaction Methods 0.000 claims abstract description 49
- 239000003513 alkali Substances 0.000 claims abstract description 37
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 33
- 150000003839 salts Chemical class 0.000 claims abstract description 16
- 239000012295 chemical reaction liquid Substances 0.000 claims abstract description 14
- RPBWMJBZQXCSFW-UHFFFAOYSA-N 2-methylpropanoyl 2-methylpropaneperoxoate Chemical compound CC(C)C(=O)OOC(=O)C(C)C RPBWMJBZQXCSFW-UHFFFAOYSA-N 0.000 claims abstract description 10
- TVWBTVJBDFTVOW-UHFFFAOYSA-N 2-methyl-1-(2-methylpropylperoxy)propane Chemical compound CC(C)COOCC(C)C TVWBTVJBDFTVOW-UHFFFAOYSA-N 0.000 claims abstract 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 27
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 19
- 230000035484 reaction time Effects 0.000 claims description 8
- GTJOHISYCKPIMT-UHFFFAOYSA-N 2-methylundecane Chemical compound CCCCCCCCCC(C)C GTJOHISYCKPIMT-UHFFFAOYSA-N 0.000 claims description 6
- SGVYKUFIHHTIFL-UHFFFAOYSA-N Isobutylhexyl Natural products CCCCCCCC(C)C SGVYKUFIHHTIFL-UHFFFAOYSA-N 0.000 claims description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 6
- VKPSKYDESGTTFR-UHFFFAOYSA-N isododecane Natural products CC(C)(C)CC(C)CC(C)(C)C VKPSKYDESGTTFR-UHFFFAOYSA-N 0.000 claims description 6
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 5
- 239000008096 xylene Substances 0.000 claims description 5
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 239000002585 base Substances 0.000 claims 5
- 230000007062 hydrolysis Effects 0.000 abstract description 4
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 4
- 150000001263 acyl chlorides Chemical class 0.000 abstract description 3
- 238000007086 side reaction Methods 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 74
- 239000007864 aqueous solution Substances 0.000 description 5
- 230000002708 enhancing effect Effects 0.000 description 5
- -1 polyethylene Polymers 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- 239000003999 initiator Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000002194 synthesizing effect Effects 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000004880 explosion Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 1
- 238000007259 addition reaction Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 150000001451 organic peroxides Chemical class 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 239000003505 polymerization initiator Substances 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C407/00—Preparation of peroxy compounds
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for continuously producing diisobutyl peroxide by multipoint feeding and intensive mixing, which comprises the following steps: (1) continuously feeding aqueous hydrogen peroxide and an aqueous alkali solution stream 1 into a first flow reactor for salt forming reaction; (2) carrying out IBP generation reaction on the reaction liquid obtained in the step (1) and isobutyryl chloride solution stream 1 which is continuously added in a second flow reactor; (3) enabling the reaction liquid obtained in the step (2) and an aqueous alkali stream 2 which is continuously added to enter a third flow reactor for salt forming reaction; (4) carrying out IBP generation reaction on the reaction liquid obtained in the step (3) and an isobutyryl chloride solution stream 2 which is continuously added in a fourth flow reactor; IBP is an abbreviation for diisobutyryl peroxide. The method can obviously reduce the side reactions such as acyl chloride hydrolysis and the like, improve the IBP yield, and timely remove the reaction heat, so that the whole reaction is carried out under the continuous condition of safety and environmental protection.
Description
Technical Field
The invention provides a preparation method of polymer synthesis initiator diisobutyronitrile (IBP), in particular relates to a method for continuously producing IBP by multipoint feeding and intensive mixing, and belongs to the technical field of initiator production.
Background
IBP is a novel polymerization initiator, has the characteristics of high oxygen content, good low-temperature activity and the like, and is mainly used as an initiator for synthesizing high molecular polymers in the industries of polyvinyl chloride, polyethylene, organic glass and the like. IBP is also a D-type liquid organic peroxide, has poor thermal stability, can be decomposed at 0 ℃ in a self-accelerating way, and is easy to explode. In addition, isobutyryl chloride used as a raw material for synthesizing IBP is easy to hydrolyze, and is hydrolyzed more rapidly under an alkaline condition, which is not beneficial to the improvement of the yield of the IBP.
At present, the industrial method for synthesizing IBP is intermittent synthesis in a stirring reaction kettle, a large amount of reaction heat is released in the synthesis, and the dropwise addition reaction time is long in order to remove the heat in time; adding alkali once to ensure that the isobutyryl chloride has more hydrolysis side reactions; the IBP stock in the stirred tank is increased in the later stage of the reaction, and a great risk of decomposition and explosion of the IBP exists.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a method for continuously producing diisobutyryl peroxide by multi-point feeding and intensive mixing.
The technical scheme of the invention is summarized as follows:
a method for continuously producing diisobutyryl peroxide by multi-point feeding and intensive mixing comprises the following steps:
(1) continuously feeding aqueous hydrogen peroxide and an aqueous alkali solution stream 1 into a first flow reactor for salt forming reaction;
(2) carrying out IBP generation reaction on the reaction liquid obtained in the step (1) and isobutyryl chloride solution stream 1 which is continuously added in a second flow reactor;
(3) enabling the reaction liquid obtained in the step (2) and an aqueous alkali stream 2 which is continuously added to enter a third flow reactor for salt forming reaction;
(4) carrying out IBP generation reaction on the reaction liquid obtained in the step (3) and an isobutyryl chloride solution stream 2 which is continuously added in a fourth flow reactor;
IBP is an abbreviation for diisobutyryl peroxide.
The sum of the flow rate of the aqueous alkali solution stream 1 and the flow rate of the aqueous alkali solution stream 2 is the total aqueous alkali solution flow rate, and the flow rate of the aqueous alkali solution stream 1 accounts for 55-99% of the total aqueous alkali solution flow rate.
The sum of the flow of the isobutyryl chloride stream 1 and the flow of the isobutyryl chloride solution stream 2 is the total isobutyryl chloride solution flow, and the flow of the isobutyryl chloride solution stream 1 accounts for 50-95% of the total isobutyryl chloride solution flow.
The mass concentration of the hydrogen peroxide solution is 5-50 percent;
the mass concentration of the alkaline water solution is 5-40%, and the alkali is sodium hydroxide or potassium hydroxide.
The mass concentration of the isobutyryl chloride solution is 30-100%, and the solvent of the isobutyryl chloride solution is toluene, xylene, isododecane or cyclohexane.
The salt forming reaction temperature of the step (1) is-20 ℃, and the reaction time is 1-600 s.
The salt forming reaction temperature of the step (3) is-20 ℃, and the reaction time is 1-600 s.
The reaction temperature for generating IBP in the step (2) is-10-30 ℃, and the reaction time is 1-600 s.
The reaction temperature for generating IBP in the step (4) is-10-30 ℃, and the reaction time is 1-600 s.
The first flow reactor, the second flow reactor, the third flow reactor and the fourth flow reactor are the same type of reactor for enhancing mixing and heat transfer or different types of reactors for enhancing mixing and heat transfer.
The method can effectively solve the problems of excessive hydrogen peroxide, long reaction time, excessive acyl chloride hydrolysis, easy explosion of a large amount of IBP in the reaction kettle due to over-temperature and the like in the existing IBP production process. The invention adopts the multipoint feeding and reinforced mixing technology to carry out the continuous synthesis of IBP, thereby not only realizing the second-level mixing of reaction materials, but also improving the molar ratio of hydrogen peroxide to alkali and reducing the alkalinity of the solution, further improving the reaction efficiency and reducing the occurrence of side reactions of acyl chloride easy hydrolysis; in addition, the continuous production can also reduce the labor cost and avoid the problem of batch stability of the batch process. The enhanced mixing and heat transfer reactor has excellent enhanced mixing performance, and can ensure that fluid is uniformly mixed or dispersed within second-level time; meanwhile, the heat transfer can be enhanced, and the reaction heat can be removed in time. The alkaline aqueous solution is added in multiple points, so that the molar ratio of hydrogen peroxide to alkali can be improved, more alkali can be converted into hydrogen peroxide, and the alkalinity of the solution is reduced; the isobutyryl chloride is added in multiple points, which is beneficial to improving the selectivity of the isobutyryl chloride and the hydrogen peroxide to generate the IBP. Therefore, the method for preparing IBP by adopting multi-point feeding and reinforced mixing can effectively solve the defects of the traditional IBP industrial production.
Detailed Description
The present invention will be further illustrated by the following specific examples. The present invention is not limited by the following examples, and specific embodiments may be determined according to the technical solutions and practical situations of the present invention. All the percentage units in the invention are mass percentages.
IBP is an abbreviation for diisobutyryl peroxide.
Example 1
A method for continuously producing diisobutyryl peroxide by multi-point feeding and intensive mixing comprises the following steps:
(1) enabling a 20% aqueous hydrogen peroxide solution (with volume flow set to be 9.7ml/min through a 1# metering pump) and a 5% aqueous sodium hydroxide solution stream 1 (with volume flow set to be 41.7ml/min through a 2# metering pump), starting the 1# metering pump and the 2# metering pump simultaneously, enabling the aqueous hydrogen peroxide solution and the aqueous sodium hydroxide solution to be respectively introduced into the 1# metering pump and the 2# metering pump, and continuously entering a first flow reactor (a microchannel reactor) to perform salt forming reaction for 120s at-10 ℃;
(2) reacting the reaction solution obtained in the step (1) with a continuously added isobutyryl chloride toluene solution stream 1 (isobutyryl chloride toluene solution is added through a 3# metering pump, the volume flow is 6.8ml/min) with the concentration of 70% in a second flow reactor (microchannel reactor), wherein the reaction temperature is-5 ℃, the retention time is 60s, and IBP is generated;
(3) enabling the reaction liquid obtained in the step (2) and a stream 2 (with volume flow of 34.2ml/min by a 4# metering pump) continuously added with 5% sodium hydroxide aqueous solution to enter a third flow reactor (a microchannel reactor) to perform salt forming reaction at-5 ℃ for 120 s;
(4) enabling the reaction liquid obtained in the step (3) and a continuously added isobutyryl chloride solution stream 2 (with the volume flow of 6.8ml/min through a 5# metering pump) with the concentration of 70% to stay in a fourth flow reactor (a microchannel reactor) at the temperature of 0 ℃ for 60s to generate IBP reaction; the product obtained after the reaction is immediately cooled at the temperature of minus 20 ℃.
The sum of the flow of the aqueous alkali stream 1 and the flow of the aqueous alkali stream 2 is the total aqueous alkali flow, and the flow of the aqueous alkali stream 1 accounts for 55% of the total aqueous alkali flow.
The sum of the flow rate of the isobutyryl chloride solution stream 1 and the flow rate of the isobutyryl chloride solution stream 2 is the total isobutyryl chloride solution flow rate, and the flow rate of the isobutyryl chloride solution stream 1 accounts for 50% of the total isobutyryl chloride solution flow rate.
The yield of IBP product obtained according to the process of example 1 of the present invention was 86.7%.
Example 2
A method for continuously producing diisobutyryl peroxide by multi-point feeding and intensive mixing comprises the following steps:
(1) the method comprises the following steps of (1) continuously feeding 10% aqueous hydrogen peroxide (volume flow is set to be 11.9ml/min through a 1# metering pump) and 30% aqueous sodium hydroxide stream 1 (volume flow is set to be 27.0ml/min through a 2# metering pump), simultaneously starting the 1# metering pump and the 2# metering pump, respectively feeding the aqueous hydrogen peroxide and the aqueous sodium hydroxide into the 1# metering pump and the 2# metering pump, and continuously feeding the aqueous hydrogen peroxide and the aqueous sodium hydroxide into a first flow reactor (a high-shear reactor) to perform salt forming reaction for 300s at 0 ℃;
(2) reacting the reaction solution obtained in the step (1) with a continuously added isobutyryl chloride xylene solution stream 1 (the isobutyryl chloride xylene solution is added through a 3# metering pump, and the volume flow is 46.2ml/min) with the concentration of 30% in a second flow reactor (a microchannel reactor) at the temperature of-10 ℃ for 600s to perform a reaction for generating IBP;
(3) enabling the reaction liquid obtained in the step (2) and a stream 2 (with volume flow of 17.8ml/min by a 4# metering pump) continuously added with 5% sodium hydroxide aqueous solution to enter a third flow reactor (high-shear reactor) to perform salt forming reaction for 300s at 0 ℃;
(4) reacting the reaction solution obtained in the step (3) with a continuously added isobutyryl chloride xylene solution stream 2 (volume flow is 11.6ml/min by a 5# metering pump) at 10 ℃ for 300s in a fourth flow reactor (microchannel reactor) to generate IBP; the product obtained after the reaction is immediately cooled at the temperature of minus 20 ℃.
The sum of the flow rate of the aqueous alkali solution stream 1 and the flow rate of the aqueous alkali solution stream 2 is the total aqueous alkali solution flow rate, and the flow rate of the aqueous alkali solution stream 1 accounts for 80% of the total aqueous alkali solution flow rate.
The sum of the flow rate of the isobutyryl chloride solution stream 1 and the flow rate of the isobutyryl chloride solution stream 2 is the total isobutyryl chloride solution flow rate, and the flow rate of the isobutyryl chloride solution stream 1 accounts for 80% of the total isobutyryl chloride solution flow rate.
The yield of IBP product obtained according to the process of example 1 of the present invention was 82.0%.
Example 3
A method for continuously producing diisobutyryl peroxide by multi-point feeding and intensive mixing comprises the following steps:
(1) enabling a 50% aqueous hydrogen peroxide solution (with a volume flow set to be 2.2ml/min through a # 1 metering pump) and a 5% aqueous potassium hydroxide solution stream 1 (with a volume flow set to be 50.0ml/min through a # 2 metering pump), simultaneously starting the # 1 metering pump and the # 2 metering pump, respectively introducing the aqueous hydrogen peroxide solution and the aqueous potassium hydroxide solution into the # 1 metering pump and the # 2 metering pump, and continuously introducing the aqueous hydrogen peroxide solution and the aqueous potassium hydroxide solution into a first flow reactor (a micro-tube reactor) to perform a salt forming reaction for 600s at-20 ℃;
(2) reacting the reaction solution obtained in the step (1) with an isobutyryl chloride isododecane solution (30% isobutyryl chloride cyclohexane solution can also be adopted) continuously added with an isobutyryl chloride isododecane solution 1 (the isobutyryl chloride isododecane solution is added through a 3# metering pump, the volume flow is 16.7ml/min) in a second flow reactor (a microchannel reactor) at the temperature of-10 ℃ for 600s to generate IBP;
(3) enabling the reaction liquid obtained in the step (2) and a stream 2 (with a volume flow of 21.3ml/min by a 4# metering pump) continuously added with 5% potassium hydroxide aqueous solution to enter a third flow reactor (a micro-tube reactor) to perform salt forming reaction for 600s at the temperature of minus 20 ℃;
(4) reacting the reaction solution obtained in the step (3) with a continuously added stream 2 (with a volume flow of 9.0ml/min by using a 5# metering pump) of an isobutyryl chloride isododecane solution with the concentration of 30% (or using an isobutyryl chloride cyclohexane solution with the concentration of 30%) in a fourth flow reactor (a microchannel reactor) at the temperature of-10 ℃ for 600s to generate IBP; the product obtained after the reaction is immediately cooled at the temperature of minus 20 ℃.
The sum of the flow rate of the aqueous alkali solution stream 1 and the flow rate of the aqueous alkali solution stream 2 is the total aqueous alkali solution flow rate, and the flow rate of the aqueous alkali solution stream 1 accounts for 70% of the total aqueous alkali solution flow rate.
The sum of the flow rate of the isobutyryl chloride solution stream 1 and the flow rate of the isobutyryl chloride solution stream 2 is the total isobutyryl chloride solution flow rate, and the flow rate of the isobutyryl chloride solution stream 1 accounts for 65% of the total isobutyryl chloride solution flow rate.
The yield of IBP product obtained according to the process of example 1 of the present invention was 89.1%.
Example 4
A method for continuously producing diisobutyryl peroxide by multi-point feeding and intensive mixing comprises the following steps:
(1) 5% aqueous hydrogen peroxide (volume flow is set to be 63.5ml/min through a 1# metering pump) and 40% aqueous potassium hydroxide stream 1 (volume flow is set to be 15.0ml/min through a 2# metering pump), starting the 1# metering pump and the 2# metering pump simultaneously, leading the aqueous hydrogen peroxide and the aqueous potassium hydroxide solution into the 1# metering pump and the 2# metering pump respectively, and continuously entering a first flow reactor (a high-shear reactor) for salt forming reaction for 1s at 20 ℃;
(2) reacting the reaction solution obtained in the step (1) with isobutyryl chloride (100%) stream 1 (the isobutyryl chloride is added through a 3# metering pump, and the volume flow rate is 14.6ml/min) continuously added in a second flow reactor (a micro-tube reactor) at 30 ℃ for 1s to generate IBP;
(3) enabling the reaction liquid obtained in the step (2) and a continuously added potassium hydroxide aqueous solution stream 2 with the concentration of 40% (passing through a 4# metering pump, the volume flow rate is 0.2ml/min) to enter a third flow reactor (high-shear reactor) to carry out salt forming reaction for 1s at the temperature of 20 ℃;
(4) reacting the reaction solution obtained in the step (3) with a continuously added isobutyryl chloride (100%) stream 2 (volume flow of 0.8ml/min by a 5# metering pump) in a fourth flow reactor (a micro-tube reactor) at 30 ℃ for 1s to generate IBP; the product obtained after the reaction is immediately cooled at the temperature of minus 20 ℃.
The sum of the flow rate of the aqueous alkali solution stream 1 and the flow rate of the aqueous alkali solution stream 2 is the total aqueous alkali solution flow rate, and the flow rate of the aqueous alkali solution stream 1 accounts for 99% of the total aqueous alkali solution flow rate.
The sum of the flow rate of the isobutyryl chloride solution stream 1 and the flow rate of the isobutyryl chloride solution stream 2 is the total isobutyryl chloride solution flow rate, and the flow rate of the isobutyryl chloride solution stream 1 accounts for 95% of the total isobutyryl chloride solution flow rate.
The yield of IBP product obtained according to the process of example 1 of the present invention was 85.2%.
The first flow reactor, the second flow reactor, the third flow reactor and the fourth flow reactor are the same type of reactors for enhancing mixing and heat transfer, such as: a microchannel reactor; the first flow reactor and the third flow reactor may be the same type of mixing and heat transfer enhancing reactor, for example: the high shear reactor, the second flow reactor and the fourth flow reactor are of the same type of mixing and heat transfer enhancing reactor, such as a micro-tube reactor.
The reactors are all commercial products.
Claims (10)
1. A method for continuously producing diisobutyl peroxide by multi-point feeding and intensive mixing is characterized by comprising the following steps:
(1) continuously feeding aqueous hydrogen peroxide and an aqueous alkali solution stream 1 into a first flow reactor for salt forming reaction;
(2) carrying out IBP generation reaction on the reaction liquid obtained in the step (1) and isobutyryl chloride solution stream 1 which is continuously added in a second flow reactor;
(3) enabling the reaction liquid obtained in the step (2) and an aqueous alkali stream 2 which is continuously added to enter a third flow reactor for salt forming reaction;
(4) carrying out IBP generation reaction on the reaction liquid obtained in the step (3) and an isobutyryl chloride solution stream 2 which is continuously added in a fourth flow reactor;
IBP is an abbreviation for diisobutyryl peroxide.
2. The process according to claim 1, characterized in that the sum of the flow of aqueous base stream 1 and the flow of aqueous base stream 2 is the total aqueous base flow, said aqueous base stream 1 flow being between 55% and 99% of the total aqueous base flow.
3. The method according to claim 1, characterized in that the sum of the flow rate of isobutyryl chloride stream 1 and the flow rate of isobutyryl chloride solution stream 2 is the total isobutyryl chloride solution flow rate, said isobutyryl chloride solution stream 1 flow rate being 50-95% of the total isobutyryl chloride solution flow rate.
4. The method according to claim 1 or 2, characterized in that the hydrogen peroxide solution has a mass concentration of 5% to 50%; the mass concentration of the alkaline water solution is 5-40%, and the alkali is sodium hydroxide or potassium hydroxide.
5. The method according to claim 1 or 3, wherein the mass concentration of the isobutyryl chloride solution is 30% to 100%, and the solvent of the isobutyryl chloride solution is toluene, xylene, isododecane, or cyclohexane.
6. The method as claimed in claim 1, wherein the salt-forming reaction temperature in step (1) is-20 to 20 ℃ and the reaction time is 1 to 600 s.
7. The method as claimed in claim 1, wherein the salt-forming reaction temperature in step (3) is-20 to 20 ℃ and the reaction time is 1 to 600 s.
8. The method according to claim 1, wherein the IBP produced in step (2) is reacted at a temperature of-10 to 30 ℃ for 1 to 600 seconds.
9. The method according to claim 1, wherein the IBP formed in step (4) is reacted at a temperature of-10 to 30 ℃ for 1 to 600 seconds.
10. The process of claim 1, wherein the first flow reactor, the second flow reactor, the third flow reactor, and the fourth flow reactor are the same type of enhanced mixing and heat transfer reactor or different types of enhanced mixing and heat transfer reactors.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115611795A (en) * | 2022-08-25 | 2023-01-17 | 鄂尔多斯市瀚博科技有限公司 | A kind of synthetic method of diisobutyryl peroxide |
| CN116284509A (en) * | 2023-03-06 | 2023-06-23 | 鄂尔多斯市瀚博科技有限公司 | Method for in-situ synthesis of high-thermal-stability polyvinyl chloride resin |
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| CN110256320A (en) * | 2019-06-29 | 2019-09-20 | 淄博正华助剂股份有限公司 | The synthetic method of dicetyl peroxydicarbonate two (2- ethylhexyl) ester |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115611795A (en) * | 2022-08-25 | 2023-01-17 | 鄂尔多斯市瀚博科技有限公司 | A kind of synthetic method of diisobutyryl peroxide |
| CN116284509A (en) * | 2023-03-06 | 2023-06-23 | 鄂尔多斯市瀚博科技有限公司 | Method for in-situ synthesis of high-thermal-stability polyvinyl chloride resin |
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