CN117924136A - Continuous synthesis method of methyl ethyl ketone peroxide - Google Patents
Continuous synthesis method of methyl ethyl ketone peroxide Download PDFInfo
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- CN117924136A CN117924136A CN202410075544.8A CN202410075544A CN117924136A CN 117924136 A CN117924136 A CN 117924136A CN 202410075544 A CN202410075544 A CN 202410075544A CN 117924136 A CN117924136 A CN 117924136A
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- methyl ethyl
- ethyl ketone
- ketone peroxide
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- WFUGQJXVXHBTEM-UHFFFAOYSA-N 2-hydroperoxy-2-(2-hydroperoxybutan-2-ylperoxy)butane Chemical compound CCC(C)(OO)OOC(C)(CC)OO WFUGQJXVXHBTEM-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 238000001308 synthesis method Methods 0.000 title claims abstract description 13
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims abstract description 30
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000007788 liquid Substances 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 10
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims description 40
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 16
- 239000012043 crude product Substances 0.000 claims description 16
- 238000002156 mixing Methods 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 12
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- 238000007599 discharging Methods 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- 238000010924 continuous production Methods 0.000 claims description 3
- JCTXKRPTIMZBJT-UHFFFAOYSA-N 2,2,4-trimethylpentane-1,3-diol Chemical compound CC(C)C(O)C(C)(C)CO JCTXKRPTIMZBJT-UHFFFAOYSA-N 0.000 claims description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- XNGIFLGASWRNHJ-UHFFFAOYSA-L phthalate(2-) Chemical compound [O-]C(=O)C1=CC=CC=C1C([O-])=O XNGIFLGASWRNHJ-UHFFFAOYSA-L 0.000 claims description 2
- 229920005862 polyol Polymers 0.000 claims description 2
- 150000003077 polyols Chemical class 0.000 claims description 2
- 238000005086 pumping Methods 0.000 claims description 2
- YNJBWRMUSHSURL-UHFFFAOYSA-N trichloroacetic acid Chemical compound OC(=O)C(Cl)(Cl)Cl YNJBWRMUSHSURL-UHFFFAOYSA-N 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 14
- 238000000926 separation method Methods 0.000 abstract description 6
- 230000007547 defect Effects 0.000 abstract description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 18
- 238000010790 dilution Methods 0.000 description 11
- 239000012895 dilution Substances 0.000 description 11
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 10
- NIQCNGHVCWTJSM-UHFFFAOYSA-N Dimethyl phthalate Chemical compound COC(=O)C1=CC=CC=C1C(=O)OC NIQCNGHVCWTJSM-UHFFFAOYSA-N 0.000 description 8
- 238000003756 stirring Methods 0.000 description 8
- 239000000047 product Substances 0.000 description 7
- 239000012530 fluid Substances 0.000 description 6
- 238000012546 transfer Methods 0.000 description 6
- FBSAITBEAPNWJG-UHFFFAOYSA-N dimethyl phthalate Natural products CC(=O)OC1=CC=CC=C1OC(C)=O FBSAITBEAPNWJG-UHFFFAOYSA-N 0.000 description 4
- 229960001826 dimethylphthalate Drugs 0.000 description 4
- 238000005070 sampling Methods 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 229920006337 unsaturated polyester resin Polymers 0.000 description 3
- 229910000619 316 stainless steel Inorganic materials 0.000 description 2
- 238000010923 batch production Methods 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000000498 cooling water Substances 0.000 description 2
- LSXWFXONGKSEMY-UHFFFAOYSA-N di-tert-butyl peroxide Chemical compound CC(C)(C)OOC(C)(C)C LSXWFXONGKSEMY-UHFFFAOYSA-N 0.000 description 2
- 229910001882 dioxygen Inorganic materials 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000003999 initiator Substances 0.000 description 2
- 150000001451 organic peroxides Chemical class 0.000 description 2
- 238000004806 packaging method and process Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- 238000007171 acid catalysis Methods 0.000 description 1
- 239000002928 artificial marble Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000001273 butane Substances 0.000 description 1
- -1 butanone peroxide Chemical class 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000002894 chemical waste Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000005536 corrosion prevention Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 description 1
- OFBQJSOFQDEBGM-UHFFFAOYSA-N n-pentane Natural products CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a continuous synthesis method of methyl ethyl ketone peroxide, which relates to the field of methyl ethyl ketone peroxide synthesis and aims to solve the problems of high cost, large quality fluctuation among different batches and complicated post-treatment in the prior art, and the technical scheme is that butanone and hydrogen peroxide react in a micro-reactor, and an outlet of the micro-mixer is connected with a coil reactor in series; the coil reactor is placed in a chilled liquid. The continuous synthesis of the methyl ethyl ketone peroxide is realized by utilizing the microchannel reactor, a liquid separation process is not needed, the defects of the patent document 1 and the patent document 2 are overcome, and the production of the methyl ethyl ketone peroxide achieves the purposes of intrinsic safety and green production; batch reaction is carried out to produce a batch of methyl ethyl ketone peroxide, 7-8 hours are needed, and micro-channels are used to produce methyl ethyl ketone peroxide with the same weight, only about 4 hours is needed, so that the production cost is reduced, the production efficiency is improved, and the quality fluctuation among batches can be reduced; in addition, the technical scheme does not need liquid separation, and the post-treatment is simple.
Description
Technical Field
The invention relates to the field of methyl ethyl ketone peroxide synthesis, in particular to a continuous synthesis method of methyl ethyl ketone peroxide.
Background
Methyl ethyl ketone peroxide, english name: 2-Butanoneperoxide; ethylmethylketone peroxide also called butanone peroxide, room temperature initiator, colorless transparent liquid. The commercial methyl ethyl ketone peroxide is a mixture with the content of 40-60 percent, and can react vigorously when contacting heavy metal ions and reducing agents.
Methyl ethyl ketone peroxide is the most widely used curing agent in the curing of unsaturated polyester resins. The composite material is widely applied to buttons, daylighting boards, artificial agates, artificial marble, corrosion prevention, yacht, gel coats, artware, wind energy blades, polyester pipelines and other products. By the end of 2018, the annual output of unsaturated polyester resin in China is about 530 ten thousand tons, and the actual operating rate is 56 percent, so that the annual output of unsaturated polyester resin 2018 is about 300 ten thousand tons. The annual sales of methyl ethyl ketone peroxide in 2018 is about 3 ten thousand tons according to the use ratio of the unsaturated resin and the methyl ethyl ketone peroxide.
The methyl ethyl ketone peroxide product is used as organic peroxide, 5.2 dangerous chemicals, and the peroxide bond length contained in the molecule is 1.23 times of the dioxygen bond length in the oxygen molecule, but the bond energy is only 41% of the dioxygen bond. The relative long bond and low bond energy determine the characteristics of unstable methyl ethyl ketone peroxide, easy decomposition and the like, and is extremely sensitive to heat, friction, vibration and impact. When the material is heated, vibrated or rubbed, the peroxide bond can be broken, 2 free radicals with strong reactivity are generated, and uncontrollable explosion accidents occur.
At present, batch process is mainly used by domestic manufacturers for synthesizing methyl ethyl ketone peroxide because of the characteristics of batch process: the heat release is concentrated, the operation time is long, and the quality fluctuation among batches is large; complexity of methyl ethyl ketone peroxide reaction: the methyl ethyl ketone peroxide with different structures has different activities and different active oxygen contents, so that different application experiences can be generated when the methyl ethyl ketone peroxide is applied to downstream customers, the properties of the produced products are different, and great trouble is caused to the customers. With the increasing importance of the national and government on environmental protection and safe production, the development of efficient, safe and continuous synthesis process and equipment of methyl ethyl ketone peroxide is a necessary trend.
Microchannel reactors are a type of reactor that utilizes precision machining techniques to produce a fluid flow channel having a size of between 10 and 1000 μm. The microchannel reactor mainly adopts a static mixing mode, and utilizes a special structure in a channel to repeatedly cut and combine fluid so as to shorten a diffusion path, and a single-phase or multi-phase system with micron-scale dispersion is formed to strengthen the reaction process, so that the effect of rapid mixing is achieved. The microchannel reactor has larger specific surface area, and the heat exchange efficiency is 100-200 times that of common industrial equipment; . The micro-channel reactor has a limited liquid holdup due to the small channel size, so that the safety is greatly improved for some flammable and explosive high-risk reactions, and the temperature distribution can be uniform in a short time due to the reduced volume inside the reactor. Based on the advantages of the micro-channel reactor, the invention adopts the micro-channel reactor to improve the methyl ethyl ketone peroxide synthesis process.
At present, many studies on the use of micro-channel reactors for peroxides in China have been reported, for example: patent document 1 (chinese patent CN 1800161B) discloses a method and a microreactor for continuously producing methyl ethyl ketone peroxide by rapidly and uniformly mixing a methyl ethyl ketone solution with a mixture of hydrogen peroxide and sulfuric acid in a micromixer, and then further reacting in the microreactor to obtain a methyl ethyl ketone peroxide solution. Patent document 2 (chinese patent CN 114349675B) discloses a continuous synthesis method and system of methyl ethyl ketone peroxide, which realizes continuous synthesis of methyl ethyl ketone peroxide and a method of fast oil-water liquid, and indicates the direction for industrial and intrinsically safe methyl ethyl ketone peroxide. Patent document 3 (chinese patent CN 110128314B) discloses that the microchannel reactor proves feasibility in continuously synthesizing 2, 2-bis (t-butyl peroxide) butane, and the application prospect of the microchannel reactor is wider by the acid catalysis of butanone and t-butyl peroxide. The global maximum of the manufacturers of synthetic organic peroxides, namely the use of industrial-scale microchannel reactors for the synthetic production of methyl ethyl ketone peroxide, is United Initiators in germany, which has been safely produced for many years.
Patent document 1 has conducted a favorable search for a microreactor and confirmed the feasibility of microreaction. But no further work is done on the post-treatment.
Patent document 2 has conducted intensive studies on the synthesis of methyl ethyl ketone peroxide by micro-reaction, and oil-water separation at the rear end has also conducted intensive studies, and the introduction of inorganic salts promotes the separation of liquid, but also causes the problem of treatment of chemical waste liquid, and also increases the production cost.
Disclosure of Invention
In view of the problems existing in the prior art, the invention discloses a continuous synthesis method of methyl ethyl ketone peroxide, which adopts the technical scheme that the method comprises the following steps:
step1, pumping a raw material A and a raw material B into a microchannel reactor;
Step 2, discharging from an outlet of the microchannel reactor after full reaction to obtain a crude product C;
step 3, blending the crude product C obtained in the step 2;
In the step 1, the raw material A is one or more of solvent, acid and butanone, wherein butanone is necessary in the raw material A, and the raw material B is one or two of hydrogen peroxide and acid, wherein hydrogen peroxide is necessary in the raw material B; the microchannel reactor further comprises a micromixer and a coil reactor, wherein the outlet of the micromixer is connected with the coil reactor in series; the coil reactor is placed in a chilled liquid.
As a preferable technical scheme of the invention, in the step 1, the solvent is of a common industrial grade, and the component is one or a mixture of more than one of phthalate, 2, 4-trimethyl-1, 3-pentanediol diisobutyrate and polyol, and the mass concentration is 0-60%.
As a preferable technical scheme of the invention, the acid is one or more mixed solutions of nitric acid, sulfuric acid, phosphoric acid, acetic acid and trichloroacetic acid, and the mass concentration is 0.01-1%.
As a preferable technical scheme of the invention, the raw material A and the raw material B are 1:0.2-2.0.
As a preferable technical scheme of the invention, the mass concentration of butanone in the raw material A is 40-100%, the mass concentration of hydrogen peroxide in the raw material B is 50-80%, and the molar ratio of the butanone to the hydrogen peroxide is 1:1.0-3.0.
As a preferable technical scheme of the invention, the raw materials A and B are cooled to 15 ℃ before being introduced into the microchannel reactor.
As a preferable technical scheme of the invention, the micro-mixer is a 3-channel 316 stainless steel mixer, and after the channel 1 and the channel 2 are combined in the mixer, the mixture flows in a three-dimensional structure channel of the micro-mixer and is discharged from the channel 3. The volume of the micromixer is 2.0-200 ml, the flow is 10-8000 l/h, and the residence time is 1.0-1000 ms.
As a preferable technical scheme of the invention, the temperature of the micro-reactor is 0-60 ℃.
As a preferable technical scheme of the invention, the coil pipe reactor is made of 316 stainless steel, and the pipe body is made ofThe length of the pipeline is 10-100 meters.
The invention has the beneficial effects that: the invention utilizes the characteristics of rapid and efficient mixing and exothermic reaction dispersion of the microchannel reactor to realize continuous synthesis of the methyl ethyl ketone peroxide, does not need a liquid separation process, solves the defects of the patent document 1 and the patent document 2, and ensures that the production of the methyl ethyl ketone peroxide achieves the purposes of intrinsic safety and green production; batch reaction is carried out to produce a batch of methyl ethyl ketone peroxide, 7-8 hours are needed, and micro-channels are used to produce methyl ethyl ketone peroxide with the same weight, only about 4 hours is needed, so that the production cost is reduced, the production efficiency is improved, and the quality fluctuation among batches can be reduced; in addition, the technical scheme does not need liquid separation, and the post-treatment is simple.
Drawings
FIG. 1 is a schematic flow chart of the present invention.
Detailed Description
Example 1
As shown in fig. 1, a first embodiment of the present invention is disclosed, and the technical scheme adopted is that the method includes the following steps:
1. The raw materials are selected as follows: 70% hydrogen peroxide, concentrated sulfuric acid, butanone, dimethyl phthalate, 20% sodium hydroxide and diglycol, wherein the sulfuric acid and the sodium hydroxide are in reagent grade, and the balance is industrial grade raw materials.
2. Preparing a reactor: the reactor adopts a micro-reactor, comprising a micro-mixer and a coil reactor. The micro mixer is provided with two feeding ports (channel 1, channel 2) and a discharging port (channel 3) on one side, the two feeding ports are communicated with a three-dimensional channel inlet with the length of 100 mu m after being converged in the micro mixer, and an outlet of the micro channel is connected with the outside through the channel 3. The inlet of the coil reactor is connected in series with the channel 3 of the micromixer, the coil reactor is placed in the refrigerating fluid, and the specification of the coil is thatThe outlet of the coil reactor is the crude product, with a length of 60 meters.
3. The specific operation is as follows:
Step 1, 874kg of dimethyl phthalate is moved into the blending kettle 01, stirring is started, a cooling water inlet and outlet valve of the blending kettle 01 is opened, 1.4 kg of 98% sulfuric acid is slowly added into the blending kettle 01, and 856kg of butanone is transferred into the blending kettle 01. The temperature is controlled to be about 15 ℃. After stirring for 15 minutes, the stirring was stopped, and the raw material in the preparation kettle 01 was set as the raw material A.
Step 2, transferring 955kg of 70% hydrogen peroxide into the overhead tank 01, cooling to about 15 ℃ and obtaining a raw material B.
And 3, setting the temperature of a heat exchanger of the microreactor to 15 ℃, and opening a refrigerating fluid inlet and outlet valve of the heat exchanger.
Step 4, respectively setting the flow rate of the raw material A transfer pump: 7.2kg/min, raw material B transfer pump flow:
3.96kg/min, starting the transfer pumps of the raw materials A and B.
And 5, feeding the crude product into a dilution kettle 01, and sampling the crude product in a central control way at an outlet of the crude product.
And 6, switching the crude product to the dilution kettle 02 when the weight of the crude product of the dilution kettle 01 reaches 2650 kg.
And 7, adding 11.5kg of 20% sodium hydroxide into the dilution kettle 01, and transferring 500kg of diethylene glycol.
And 8, stirring the dilution kettle 01 for half an hour, sampling, and transferring to a finished product tank for packaging and warehousing after the dilution kettle is qualified.
Example 2
As shown in fig. 1, a first embodiment of the present invention is disclosed, and the technical scheme adopted is that the method includes the following steps:
1. The raw materials are selected as follows: 70% hydrogen peroxide, 70% concentrated sulfuric acid, butanone, dimethyl phthalate, 20% sodium hydroxide and diethylene glycol, wherein the sulfuric acid and the sodium hydroxide are reagent grade, and the balance is industrial grade raw materials. 2. Preparing a reactor: the reactor adopts a micro-reactor, comprising a micro-mixer and a coil reactor. The micro mixer is provided with two feeding ports (channel 1, channel 2) and a discharging port (channel 3) on one side, the two feeding ports are communicated with a three-dimensional channel inlet with the length of 100 mu m after being converged in the micro mixer, and an outlet of the micro channel is connected with the outside through the channel 3. The inlet of the coil reactor is connected in series with the channel 3 of the micromixer, the coil reactor is placed in the refrigerating fluid, and the specification of the coil is that The outlet of the coil reactor is the crude product, with a length of 60 meters.
3. The specific operation is as follows:
Step 1, adding 990kg of butanone into the blending kettle 01, starting stirring, opening a cooling water inlet and outlet valve of the blending kettle 01, slowly adding 2 kg of 70% sulfuric acid into the blending kettle 01, and controlling the temperature to be about 15 ℃. After stirring for 15 minutes, the stirring was stopped, and the raw material in the preparation kettle 01 was set as the raw material A.
Step 2, transferring 1334kg of 70% hydrogen peroxide into the overhead tank 01, and cooling to about 15 ℃ to obtain a raw material B.
And 3, setting the temperature of a heat exchanger of the microreactor to 15 ℃, and opening a refrigerating fluid inlet and outlet valve of the heat exchanger.
Step 4, respectively setting the flow rate of the raw material A transfer pump: 4.76kg/min, raw material B transfer pump flow: 6.39kg/min, starting the raw material A and raw material B transfer pumps.
And 5, feeding the crude product into a dilution kettle 01, and sampling the crude product in a central control way at an outlet of the crude product.
And 6, switching the crude product to the dilution kettle 02 when the weight of the crude product of the dilution kettle 01 reaches 2290 kg.
Step 7, diluting the kettle 01, adding 11.5kg of 20% sodium hydroxide, transferring 1000kg of dimethyl phthalate and 1110kg of diethylene glycol.
And 8, stirring the dilution kettle 01 for half an hour, sampling, and transferring to a finished product tank for packaging and warehousing after the dilution kettle is qualified.
Comparative test
The products produced in example 1 and example 2 were subjected to crude active oxygen detection with the batch reaction product, and the results were as follows:
As can be seen from the comparison, compared with the traditional batch reaction production, the micro-reaction continuous production using the technical scheme has smaller difference of crude active oxygen of different batches of products and lower fluctuation of quality among batches.
By using the technical scheme, the time required for producing a batch of methyl ethyl ketone peroxide with the same quality can be reduced from 7-8 hours to about 4 hours in the traditional method, the production cost is reduced, and the production efficiency is improved.
Although the specific embodiments of the present invention have been described in detail, the present invention is not limited to the above embodiments, and various changes and modifications without inventive labor may be made within the scope of the present invention without departing from the spirit of the present invention, which is within the scope of the present invention.
Claims (9)
1. A continuous synthesis method of methyl ethyl ketone peroxide, comprising the following steps:
step1, pumping a raw material A and a raw material B into a microchannel reactor;
Step 2, discharging from an outlet of the microchannel reactor after full reaction to obtain a crude product C;
step 3, blending the crude product C obtained in the step 2;
The method is characterized in that: in the step 1, the raw material A is butanone, and the raw material B is hydrogen peroxide; the microchannel reactor further comprises a micromixer and a coil reactor, wherein the outlet of the micromixer is connected with the coil reactor in series; the coil reactor is placed in a chilled liquid.
2. The continuous synthesis method of methyl ethyl ketone peroxide according to claim 1, wherein:
the raw material A also comprises at least one of a solvent and an acid; the raw material B also comprises acid.
3. The continuous synthesis method of methyl ethyl ketone peroxide according to claim 2, wherein:
in the step 1, the solvent is one or a mixture of more than one of phthalate, 2, 4-trimethyl-1, 3-pentanediol diisobutyrate and polyol.
4. The continuous synthesis method of methyl ethyl ketone peroxide according to claim 2, wherein:
The acid is one or more mixed liquids of nitric acid, sulfuric acid, phosphoric acid, acetic acid and trichloroacetic acid.
5. The continuous synthesis method of methyl ethyl ketone peroxide according to claim 1 or 2, characterized in that: raw material A and raw material B are 1:0.2-2.0.
6. A continuous process for the synthesis of methyl ethyl ketone peroxide according to any one of claims 1 to 5,
The method is characterized in that: the mass concentration of butanone in the raw material A is 40-100%, the mass concentration of hydrogen peroxide in the raw material B is 50-80%, and the molar ratio of the butanone to the hydrogen peroxide is 1:1.0-3.0.
7. A continuous process for the synthesis of methyl ethyl ketone peroxide according to any one of claims 1 to 5,
The method is characterized in that: and the temperature of the raw materials A and B is reduced to 15 ℃ before the raw materials A and B are introduced into the microchannel reactor.
8. The continuous synthesis method of methyl ethyl ketone peroxide according to claim 1 or 2, characterized in that: the volume of the micromixer is 2.0-200 ml, the flow is 10-8000 l/h, and the residence time is 1.0-1000 ms.
9. The continuous synthesis method of methyl ethyl ketone peroxide according to claim 7, wherein:
the temperature of the microreactor is 0-60 ℃.
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| CN202410075544.8A CN117924136A (en) | 2024-01-18 | 2024-01-18 | Continuous synthesis method of methyl ethyl ketone peroxide |
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