CN116655508A - Method for preparing tert-butyl peroxybenzoate by using microchannel reactor - Google Patents
Method for preparing tert-butyl peroxybenzoate by using microchannel reactor Download PDFInfo
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- CN116655508A CN116655508A CN202211275608.6A CN202211275608A CN116655508A CN 116655508 A CN116655508 A CN 116655508A CN 202211275608 A CN202211275608 A CN 202211275608A CN 116655508 A CN116655508 A CN 116655508A
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- butyl peroxybenzoate
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- GJBRNHKUVLOCEB-UHFFFAOYSA-N tert-butyl benzenecarboperoxoate Chemical compound CC(C)(C)OOC(=O)C1=CC=CC=C1 GJBRNHKUVLOCEB-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 238000000034 method Methods 0.000 title claims abstract description 24
- 238000006243 chemical reaction Methods 0.000 claims abstract description 54
- CIHOLLKRGTVIJN-UHFFFAOYSA-N tert‐butyl hydroperoxide Chemical compound CC(C)(C)OO CIHOLLKRGTVIJN-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000012043 crude product Substances 0.000 claims abstract description 18
- 239000000463 material Substances 0.000 claims abstract description 18
- PASDCCFISLVPSO-UHFFFAOYSA-N benzoyl chloride Chemical compound ClC(=O)C1=CC=CC=C1 PASDCCFISLVPSO-UHFFFAOYSA-N 0.000 claims abstract description 14
- 159000000000 sodium salts Chemical class 0.000 claims abstract description 14
- 238000004519 manufacturing process Methods 0.000 claims abstract description 11
- 239000003513 alkali Substances 0.000 claims abstract description 10
- 239000007788 liquid Substances 0.000 claims abstract description 7
- 230000035484 reaction time Effects 0.000 claims abstract description 6
- 238000009413 insulation Methods 0.000 claims abstract description 3
- 238000005406 washing Methods 0.000 claims description 45
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 15
- 238000002156 mixing Methods 0.000 claims description 7
- 229910052979 sodium sulfide Inorganic materials 0.000 claims description 7
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims description 7
- 238000004321 preservation Methods 0.000 claims description 6
- 239000002274 desiccant Substances 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 238000011403 purification operation Methods 0.000 claims 1
- 238000003786 synthesis reaction Methods 0.000 abstract description 6
- 239000000243 solution Substances 0.000 description 12
- 239000000047 product Substances 0.000 description 11
- 230000009286 beneficial effect Effects 0.000 description 6
- CWPKTBMRVATCBL-UHFFFAOYSA-N 3-[1-[1-[(2-methylphenyl)methyl]piperidin-4-yl]piperidin-4-yl]-1h-benzimidazol-2-one Chemical compound CC1=CC=CC=C1CN1CCC(N2CCC(CC2)N2C(NC3=CC=CC=C32)=O)CC1 CWPKTBMRVATCBL-UHFFFAOYSA-N 0.000 description 5
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 238000000354 decomposition reaction Methods 0.000 description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- UPIWXMRIPODGLE-UHFFFAOYSA-N butyl benzenecarboperoxoate Chemical group CCCCOOC(=O)C1=CC=CC=C1 UPIWXMRIPODGLE-UHFFFAOYSA-N 0.000 description 3
- 238000007086 side reaction Methods 0.000 description 3
- QEQBMZQFDDDTPN-UHFFFAOYSA-N (2-methylpropan-2-yl)oxy benzenecarboperoxoate Chemical compound CC(C)(C)OOOC(=O)C1=CC=CC=C1 QEQBMZQFDDDTPN-UHFFFAOYSA-N 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- 230000003321 amplification Effects 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 238000004880 explosion Methods 0.000 description 2
- 239000003999 initiator Substances 0.000 description 2
- 238000003199 nucleic acid amplification method Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- MNZAKDODWSQONA-UHFFFAOYSA-N 1-dibutylphosphorylbutane Chemical compound CCCCP(=O)(CCCC)CCCC MNZAKDODWSQONA-UHFFFAOYSA-N 0.000 description 1
- 239000004641 Diallyl-phthalate Substances 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- VQTUBCCKSQIDNK-UHFFFAOYSA-N Isobutene Chemical group CC(C)=C VQTUBCCKSQIDNK-UHFFFAOYSA-N 0.000 description 1
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 description 1
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- QUDWYFHPNIMBFC-UHFFFAOYSA-N bis(prop-2-enyl) benzene-1,2-dicarboxylate Chemical compound C=CCOC(=O)C1=CC=CC=C1C(=O)OCC=C QUDWYFHPNIMBFC-UHFFFAOYSA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- ATADHKWKHYVBTJ-UHFFFAOYSA-N hydron;4-[1-hydroxy-2-(methylamino)ethyl]benzene-1,2-diol;chloride Chemical compound Cl.CNCC(O)C1=CC=C(O)C(O)=C1 ATADHKWKHYVBTJ-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229920006305 unsaturated polyester Polymers 0.000 description 1
- -1 wherein Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C407/00—Preparation of peroxy compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0093—Microreactors, e.g. miniaturised or microfabricated reactors
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C407/00—Preparation of peroxy compounds
- C07C407/003—Separation; Purification; Stabilisation; Use of additives
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for preparing tert-butyl peroxybenzoate by using a microchannel reactor, which comprises the following steps: adding liquid alkali into tert-butyl hydroperoxide, standing for layering, and separating to obtain lower sodium salt; introducing the obtained sodium salt into a micro-channel reactor, and simultaneously introducing benzoyl chloride into the micro-channel reactor for mixed reaction; introducing the materials at the outlet of the microchannel reactor into an RTB reactor for thermal insulation reaction to obtain a tert-butyl peroxybenzoate crude product; and purifying the crude product of tert-butyl peroxybenzoate to obtain tert-butyl peroxybenzoate. The invention adopts continuous feeding, realizes the synthesis reaction through the micro-channel reactor, shortens the reaction time from a traditional few hours to tens of seconds to a few minutes, and obviously improves the reaction efficiency. The whole reaction process in the microchannel reactor used in the invention is continuous reaction, and the method is safe and environment-friendly, has high production efficiency, small equipment occupation area and simple operation, can reduce manual operation and reduce production cost.
Description
Technical Field
The invention relates to the field of organic synthesis, in particular to a method for preparing tert-butyl peroxybenzoate by using a microchannel reactor.
Background
Tert-butyl peroxybenzoate (TBPB or CP-02 for short) is a colorless to yellowish liquid, has slightly aromatic smell, is insoluble in water, and can be dissolved in organic solvent. Tertiary butyl peroxybenzoate is widely used as an initiator in the polymerization of ethylene, styrene, propylene, vinyl acetate, diallyl phthalate, and isobutylene; in the process of curing unsaturated polyester, the method is widely applied to molding processes such as SMC, BMC, DMC drawing agents and the like; meanwhile, the method can also be applied to the same two-component curing system with higher activity, such as MEPK, BPO or TBPO.
At present, sulfuric acid or other acids are used as catalysts, hydrogen peroxide is used as an oxidant, tertiary butyl hydroperoxide is prepared by catalytic oxidation of tertiary butyl alcohol, and then tertiary butyl peroxybenzoate is synthesized by reaction with aqueous solution of hydroxide (commonly used sodium hydroxide or potassium hydroxide) of alkali metal and benzoyl chloride, so that the tertiary butyl peroxybenzoate is the most commonly used process route.
Chinese patent CN1763001a discloses a process for producing tert-butyl peroxybenzoate, after preparing sodium salt, dropping sodium salt into benzoyl chloride, controlling temperature to react, and keeping temperature after dropping, which requires 1-3h, and the reaction process is complex and the production efficiency is low. Chinese patent CN105175303a discloses a process for preparing t-butyl peroxybenzoate initiator, wherein, hydrogen peroxide, sulfuric acid, t-butyl peroxybenzoate and benzoyl chloride are added for synthesis, and the raw materials used for synthesis are complex and various, and are not suitable for industrial batch production.
The microchannel reaction equipment has a range of characteristics not possessed by conventional reactors: the channel size is miniaturized, the heat exchange specific surface area is large, the mass and heat transfer characteristics are excellent, the continuous reaction is realized, the direct amplification by a step-by-step amplification test can be skipped, the production is flexible, and the safety performance is high.
At present, no report of synthesizing tert-butyl peroxybenzoate by using a micro-channel reactor is seen in the field, so that the method for preparing tert-butyl peroxybenzoate by using the micro-channel reactor, which is safe and environment-friendly and can improve the production efficiency and the resource utilization rate, is a technical problem to be solved by the person skilled in the art.
Disclosure of Invention
In view of the above, the invention provides a method for preparing tert-butyl peroxybenzoate by using a microchannel reactor, so as to meet various requirements in the industrial production of tert-butyl peroxybenzoate, and obtain a finished product of tert-butyl peroxybenzoate simply, economically and efficiently.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a method for preparing tert-butyl peroxybenzoate by using a microchannel reactor, comprising the following steps:
(1) Adding liquid alkali into tert-butyl hydroperoxide, standing for layering, and separating to obtain lower sodium salt;
(2) Introducing the obtained sodium salt into a micro-channel reactor at a flow rate of 200-500L/h, and simultaneously introducing benzoyl chloride into the micro-channel reactor at a flow rate of 20-50L/h for mixing reaction;
(3) Introducing the materials at the outlet of the microchannel reactor into an RTB reactor for thermal insulation reaction to obtain a tert-butyl peroxybenzoate crude product;
(4) And purifying the crude product of tert-butyl peroxybenzoate to obtain tert-butyl peroxybenzoate.
Further, the molar ratio of benzoyl chloride to tert-butyl hydroperoxide is 1:1.05-1.5.
The beneficial effect of adopting above-mentioned further scheme lies in:
the range of the material molar ratio in the reaction is controlled, so that the reaction is more complete and the generation of side reaction is reduced; meanwhile, excessive input raw materials and residual products can be avoided, and the purity and quality of subsequent target products are influenced.
Further, the mixed reaction temperature in the step (2) is 10-40 ℃ and the reaction time is 30-200s.
The beneficial effect of adopting above-mentioned further scheme lies in:
by adopting the above control of the temperature range in the reaction, the reaction can be performed faster, the reaction rate can be improved, and the self-acceleration decomposition of materials caused by the overhigh reaction temperature can be prevented, so that the combustion or explosion can be prevented.
The range of time in the reaction is controlled, so that the too short residence time and incomplete reaction are avoided; avoiding the overlong residence time, resulting in small amount of decomposition of the product and low yield.
Further, the heat preservation temperature in the step (3) is 10-40 ℃, and the heat preservation reaction time is 10-30min.
The beneficial effect of adopting above-mentioned further scheme lies in: by adopting the temperature range in the control and heat preservation, the reaction can be performed faster, the reaction rate is improved, and the self-acceleration decomposition of materials caused by overhigh reaction temperature can be prevented, so that the combustion or explosion is caused.
The range of the time in the heat preservation is controlled, so that the too short residence time and incomplete reaction are avoided; avoiding the overlong residence time, resulting in small amount of decomposition of the product and low yield.
Further, the purifying operation in step (4) is:
1) Adding the obtained tert-butyl peroxybenzoate crude product into a reaction kettle, adding dilute alkali solution according to the oil-water mass ratio of 1:1, stirring and washing, controlling the temperature at 10-40 ℃ during washing, washing for 30-60min, standing for layering, and taking an oil layer for later use;
2) Continuously putting the oil layer obtained in the step 1) into a reaction kettle, adding sodium sulfide solution according to the oil-water mass ratio of 1:1, stirring and washing, controlling the temperature at 10-40 ℃ during washing, washing for 30-60min, standing for layering, and taking the oil layer for later use;
3) And (3) continuously putting the oil layer obtained in the step (2) into a reaction kettle, adding water according to the oil-water mass ratio of 1:1, stirring and washing, controlling the temperature at 10-40 ℃ during washing, washing for 30-60min, standing for layering, and drying the obtained oil layer by adopting a drying agent to obtain the tert-butyl peroxybenzoate.
Further, the dilute alkali solution in the step 1) is sodium hydroxide solution with the mass concentration of 2-10%.
Still further, the sodium sulfide solution in step 2) has a mass concentration of 1 to 3%.
The beneficial effect of adopting above-mentioned further scheme lies in: according to the invention, the purification treatment is carried out on the TBPB crude product obtained by synthesis, so that impurities in the product are reduced, the product quality is improved, and the method is beneficial to the application of relevant downstream.
The invention has the beneficial effects that:
1. the invention adopts continuous feeding, realizes the synthesis reaction through the micro-channel reactor, shortens the reaction time from a traditional few hours to tens of seconds to a few minutes, and obviously improves the reaction efficiency.
2. The microchannel reactor used in the invention can strengthen the mass transfer and heat transfer performance, keep the reaction temperature constant, avoid the phenomenon of bouncing temperature, reduce the occurrence of side reaction, and improve the safety of the reaction process.
3. In the scheme of the invention, the reaction materials are accurately added by the feed pump, so that the yield reduction caused by the increase of side reactions due to inaccurate local stoichiometry is avoided.
4. The whole reaction process in the microchannel reactor used in the invention is continuous reaction, is safe and environment-friendly, has high production efficiency, small equipment occupation area and simple operation, can reduce manual operation, reduces production cost and ensures production economy.
5. The method has the advantages that the reaction yield is obviously improved, the yield reaches 90-95%, and the purity of the product obtained by final post-treatment reaches 99.0-99.5%.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
A method for preparing tert-butyl peroxybenzoate by using a microchannel reactor, comprising the following steps:
(1) Adding liquid alkali into tert-butyl hydroperoxide, standing for layering, and separating to obtain lower sodium salt;
(2) After the micro-channel reactor is preheated to 15 ℃, introducing the obtained sodium salt into the micro-channel reactor at a flow rate of 220L/h, simultaneously introducing benzoyl chloride into the micro-channel reactor at a flow rate of 20L/h, wherein the two materials are in a stable state when the flow rate is constant to be the set flow rate, mixing the materials in the stable state and mixing the materials at 15 ℃ for reaction for 30 seconds, and the molar ratio of the benzoyl chloride to the tert-butyl hydroperoxide is 1:1.08;
(3) Introducing the materials at the outlet of the microchannel reactor into an RTB reactor, preserving the temperature at 15 ℃, and reacting for 10min to obtain a tert-butyl peroxybenzoate crude product;
(4) Purifying the tert-butyl peroxybenzoate crude product according to the following operation:
1) Adding the obtained tert-butyl peroxybenzoate crude product into a reaction kettle, adding 10% sodium hydroxide solution according to the oil-water mass ratio of 1:1, stirring and washing, controlling the temperature at 40 ℃ during washing, washing for 30min, standing for layering, and taking an oil layer for later use;
2) Continuously putting the oil layer obtained in the step 1) into a reaction kettle, adding 1% sodium sulfide solution according to the oil-water mass ratio of 1:1, stirring and washing, controlling the temperature at 140 ℃ during washing, washing for 30min, standing for layering, and taking the oil layer for later use;
3) Continuously putting the oil layer obtained in the step 2) into a reaction kettle, adding water according to the oil-water mass ratio of 1:1 for stirring and washing, controlling the temperature at 140 ℃ during washing, washing for 30min, standing for layering, drying the obtained oil layer by adopting a drying agent to obtain tert-butyl peroxybenzoate, and measuring the reaction yield to be 90.8% and the TBPB finished product content to be 99.3%.
Example 2
A method for preparing tert-butyl peroxybenzoate by using a microchannel reactor, comprising the following steps:
(1) Adding liquid alkali into tert-butyl hydroperoxide, standing for layering, and separating to obtain lower sodium salt;
(2) After the micro-channel reactor is preheated to 20 ℃, the obtained sodium salt is introduced into the micro-channel reactor at a flow rate of 280L/h, and benzoyl chloride is introduced into the micro-channel reactor at a flow rate of 30L/h, wherein the two materials are in a stable state when the flow rate is constant to be the set flow rate, the materials are mixed in the stable state and are mixed and reacted at 20 ℃ for 60 seconds, and the molar ratio of the benzoyl chloride to the tert-butyl hydroperoxide is 1:1.06;
(3) Introducing the materials at the outlet of the microchannel reactor into an RTB reactor, preserving heat at 20 ℃, and reacting for 20min to obtain a tert-butyl peroxybenzoate crude product;
(4) Purifying the tert-butyl peroxybenzoate crude product according to the following operation:
1) Adding the obtained tert-butyl peroxybenzoate crude product into a reaction kettle, adding 2% sodium hydroxide solution according to the oil-water mass ratio of 1:1, stirring and washing, controlling the temperature at 10 ℃ during washing, washing for 60min, standing for layering, and taking an oil layer for later use;
2) Continuously putting the oil layer obtained in the step 1) into a reaction kettle, adding 3% sodium sulfide solution according to the oil-water mass ratio of 1:1, stirring and washing, controlling the temperature at 10 ℃ during washing, washing for 60min, standing for layering, and taking the oil layer for later use;
3) Continuously putting the oil layer obtained in the step 2) into a reaction kettle, adding water according to the oil-water mass ratio of 1:1 for stirring and washing, controlling the temperature at 10 ℃ during washing, washing for 60min, standing for layering, drying the obtained oil layer by adopting a drying agent to obtain tert-butyl peroxybenzoate, and measuring the reaction yield to be 92.3% and the TBPB finished product content to be 99.1%.
Example 3
A method for preparing tert-butyl peroxybenzoate by using a microchannel reactor, comprising the following steps:
(1) Adding liquid alkali into tert-butyl hydroperoxide, standing for layering, and separating to obtain lower sodium salt;
(2) After the micro-channel reactor is preheated to 35 ℃, introducing the obtained sodium salt into the micro-channel reactor at a flow rate of 360L/h, simultaneously introducing benzoyl chloride into the micro-channel reactor at a flow rate of 40L/h, wherein the two materials are in a stable state when the flow rate is constant to be the set flow rate, mixing the materials in the stable state and mixing the materials at 35 ℃ for reaction for 120s, and the molar ratio of the benzoyl chloride to the tert-butyl hydrogen peroxide is 1:1.05;
(3) Introducing the materials at the outlet of the microchannel reactor into an RTB reactor, preserving the temperature at 35 ℃, and reacting for 30min to obtain a tert-butyl peroxybenzoate crude product;
(4) Purifying the tert-butyl peroxybenzoate crude product according to the following operation:
1) Adding the obtained tert-butyl peroxybenzoate crude product into a reaction kettle, adding 6% sodium hydroxide solution according to the oil-water mass ratio of 1:1, stirring and washing, controlling the temperature at 25 ℃ during washing, washing for 40min, standing for layering, and taking an oil layer for later use;
2) Continuously putting the oil layer obtained in the step 1) into a reaction kettle, adding 2% sodium sulfide solution according to the oil-water mass ratio of 1:1, stirring and washing, controlling the temperature at 25 ℃ during washing, washing for 40min, standing for layering, and taking the oil layer for later use;
3) Continuously putting the oil layer obtained in the step 2) into a reaction kettle, adding water according to the oil-water mass ratio of 1:1 for stirring and washing, controlling the temperature at 25 ℃ during washing, washing for 40min, standing for layering, drying the obtained oil layer by adopting a drying agent to obtain tert-butyl peroxybenzoate, and measuring the reaction yield to be 94.1% and the TBPB finished product content to be 99.5%.
While embodiments of the present invention have been shown and described above, it will be understood that the above embodiments are illustrative and not to be construed as limiting the invention, and that variations, modifications, alternatives and variations may be made to the above embodiments by one of ordinary skill in the art within the scope of the invention.
Claims (7)
1. A process for preparing tert-butyl peroxybenzoate using a microchannel reactor comprising the steps of:
(1) Adding liquid alkali into tert-butyl hydroperoxide, standing for layering, and separating to obtain lower sodium salt;
(2) Introducing the obtained sodium salt into a micro-channel reactor at a flow rate of 200-500L/h, and simultaneously introducing benzoyl chloride into the micro-channel reactor at a flow rate of 20-50L/h for mixing reaction;
(3) Introducing the materials at the outlet of the microchannel reactor into an RTB reactor for thermal insulation reaction to obtain a tert-butyl peroxybenzoate crude product;
(4) And purifying the crude product of tert-butyl peroxybenzoate to obtain tert-butyl peroxybenzoate.
2. The method for preparing tert-butyl peroxybenzoate using a microchannel reactor according to claim 1 wherein the molar ratio of benzoyl chloride to tert-butyl hydroperoxide is 1:1.05-1.5.
3. The method for preparing tert-butyl peroxybenzoate using a microchannel reactor according to claim 1 wherein the mixing reaction temperature in step (2) is 10-40 ℃ and the reaction time is 30-200s.
4. The method for preparing tert-butyl peroxybenzoate by using a micro-channel reactor according to claim 1, wherein the temperature of the heat preservation in the step (3) is 10-40 ℃ and the reaction time of the heat preservation is 10-30min.
5. The process for preparing tert-butyl peroxybenzoate using a microchannel reactor according to claim 1 wherein the purification operation in step (4) is:
1) Adding the obtained tert-butyl peroxybenzoate crude product into a reaction kettle, adding dilute alkali solution according to the oil-water mass ratio of 1:1, stirring and washing, controlling the temperature at 10-40 ℃ during washing, washing for 30-60min, standing for layering, and taking an oil layer for later use;
2) Continuously putting the oil layer obtained in the step 1) into a reaction kettle, adding sodium sulfide solution according to the oil-water mass ratio of 1:1, stirring and washing, controlling the temperature at 10-40 ℃ during washing, washing for 30-60min, standing for layering, and taking the oil layer for later use;
3) And (3) continuously putting the oil layer obtained in the step (2) into a reaction kettle, adding water according to the oil-water mass ratio of 1:1, stirring and washing, controlling the temperature at 10-40 ℃ during washing, washing for 30-60min, standing for layering, and drying the obtained oil layer by adopting a drying agent to obtain the tert-butyl peroxybenzoate.
6. The method for preparing tert-butyl peroxybenzoate using a microchannel reactor according to claim 5 wherein the dilute alkali solution in step 1) is sodium hydroxide solution with a mass concentration of 2-10%.
7. The method for preparing tert-butyl peroxybenzoate using a microchannel reactor according to claim 5 wherein the sodium sulfide solution in step 2) has a mass concentration of 1-3%.
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| CN202211275608.6A CN116655508A (en) | 2022-10-18 | 2022-10-18 | Method for preparing tert-butyl peroxybenzoate by using microchannel reactor |
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| CN202211275608.6A CN116655508A (en) | 2022-10-18 | 2022-10-18 | Method for preparing tert-butyl peroxybenzoate by using microchannel reactor |
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| CN116655508A true CN116655508A (en) | 2023-08-29 |
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| CN202211275608.6A Pending CN116655508A (en) | 2022-10-18 | 2022-10-18 | Method for preparing tert-butyl peroxybenzoate by using microchannel reactor |
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- 2022-10-18 CN CN202211275608.6A patent/CN116655508A/en active Pending
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