CN113105380A - Novel process for preparing peroxyacetic acid by using acetic acid as raw material through microreactor - Google Patents
Novel process for preparing peroxyacetic acid by using acetic acid as raw material through microreactor Download PDFInfo
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- CN113105380A CN113105380A CN202110409150.8A CN202110409150A CN113105380A CN 113105380 A CN113105380 A CN 113105380A CN 202110409150 A CN202110409150 A CN 202110409150A CN 113105380 A CN113105380 A CN 113105380A
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- acid
- acetic acid
- microreactor
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- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 title claims abstract description 147
- KFSLWBXXFJQRDL-UHFFFAOYSA-N Peracetic acid Chemical compound CC(=O)OO KFSLWBXXFJQRDL-UHFFFAOYSA-N 0.000 title claims abstract description 92
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 22
- 239000002994 raw material Substances 0.000 title claims abstract description 18
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 32
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000012528 membrane Substances 0.000 claims abstract description 22
- 239000006185 dispersion Substances 0.000 claims abstract description 21
- 239000011259 mixed solution Substances 0.000 claims abstract description 19
- 239000000243 solution Substances 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- 239000000463 material Substances 0.000 claims abstract description 3
- PZAGQUOSOTUKEC-UHFFFAOYSA-N acetic acid;sulfuric acid Chemical compound CC(O)=O.OS(O)(=O)=O PZAGQUOSOTUKEC-UHFFFAOYSA-N 0.000 claims abstract 2
- 238000002360 preparation method Methods 0.000 claims description 11
- 229910001220 stainless steel Inorganic materials 0.000 claims description 6
- 239000010935 stainless steel Substances 0.000 claims description 6
- 230000014759 maintenance of location Effects 0.000 claims 1
- 238000007254 oxidation reaction Methods 0.000 abstract description 5
- 238000010924 continuous production Methods 0.000 abstract description 3
- 239000003054 catalyst Substances 0.000 abstract 1
- 239000000047 product Substances 0.000 description 5
- 238000001514 detection method Methods 0.000 description 4
- 238000005070 sampling Methods 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000001954 sterilising effect Effects 0.000 description 2
- 238000004659 sterilization and disinfection Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- 150000000180 1,2-diols Chemical class 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 241000700605 Viruses Species 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000003899 bactericide agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000645 desinfectant Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 150000002118 epoxides Chemical class 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 150000007524 organic acids Chemical class 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
- 125000000864 peroxy group Chemical group O(O*)* 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- 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
-
- 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
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00781—Aspects relating to microreactors
- B01J2219/00891—Feeding or evacuation
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- 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 novel process for preparing peroxyacetic acid by taking acetic acid as a raw material through a membrane dispersion microstructure reactor, which comprises the following main raw materials: acetic acid, hydrogen peroxide and sulfuric acid. The process comprises the steps of adding sulfuric acid into acetic acid in advance for mixing, adding acetic acid-sulfuric acid mixed solution and hydrogen peroxide solution into a membrane dispersion micro-channel reactor through two pumps respectively, enabling the acetic acid solution and the hydrogen peroxide solution to be efficiently and fully mixed for oxidation reaction under the condition of taking the sulfuric acid as a catalyst to obtain peroxyacetic acid, and directly connecting the obtained peroxyacetic acid to a material using point through a pipeline. Compared with the traditional kettle type reactor, the process for preparing the peroxyacetic acid can more accurately control various conditions in the production, improve the mass transfer rate, realize a fine, quick and controllable continuous production mode, improve the production efficiency, reduce the stock of on-line dangerous goods in the reaction process and reduce the production safety risk.
Description
Technical Field
The invention relates to the technical field of preparation of peroxyacetic acid, in particular to a novel process for preparing peroxyacetic acid by taking acetic acid as a raw material through a microreactor.
Background
Peracetic acid is an organic peroxide with a wide range of uses. In the organic acid containing peroxy, the chemical structure is simple, and the synthesis process and equipment are relatively simple. The aqueous solution of peroxyacetic acid has excellent bactericidal performance, and is a high-efficiency, quick-acting and broad-spectrum chemical bactericidal agent. The residual liquid after the sterilization of the effective components is acetic acid, oxygen and water, and the problem of secondary pollution is avoided.
In the period of the sars virus bouquet in 2003, the masterforce army as a disinfectant is widely applied to sterilization and detoxication in hospitals and other public places. In the chemical industry, the product can be used as an initiator of high molecular polymers, for preparing epoxide, synthesizing 1, 2-diol and important compounds such as glycerol, grease, phenol, brewing and the like.
Because of the wide application of the peroxyacetic acid, the synthesis device is simple, and many enterprises or hospitals try to produce the peroxyacetic acid, but the peroxyacetic acid is only limited to the reaction in the traditional stirred tank mode. The traditional reaction for synthesizing peroxyacetic acid needs to completely add sulfuric acid, acetic acid and hydrogen peroxide into a stirring kettle, and react for a long time in a stirring or static mode, wherein 3-5 hours are needed at about 30 ℃, and more than 2 hours are needed at about 0 ℃ to meet the use requirement (more than or equal to 25%). The whole reaction process and storage have certain potential safety hazards.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the technical defects and provide a novel process for preparing peroxyacetic acid by taking acetic acid as a raw material through a microreactor, wherein the continuous preparation overcomes the defects of the preparation process of the traditional peroxyacetic acid stirring kettle, the reaction time is changed, the peroxyacetic acid with the same content as the traditional stirring kettle is obtained, the continuous production can be realized, the fine, quick and controllable production mode is realized, and the safety risk of the peroxyacetic acid preparation is reduced.
In order to achieve the purpose of the invention, the invention adopts the technical scheme that: a new process for preparing peroxyacetic acid by taking acetic acid as a raw material through a microreactor comprises the following steps:
(1) preparing acetic acid and sulfuric acid mixed liquor: firstly, preparing an acetic acid and sulfuric acid mixed solution with a certain concentration;
(2) preparation of peracetic acid solution: then the acetic acid mixed solution is used as a mobile phase, the hydrogen peroxide solution is used as a dispersion phase, the mixture is uniformly and rapidly mixed through a membrane dispersion micro-reactor, and the reaction is carried out at a certain temperature to prepare the peroxyacetic acid solution.
Further, in the step (1), the concentration of the acetic acid solution is more than or equal to 99.0 percent, and the concentration of the sulfuric acid solution is 98 percent.
Further, the proportion of the two-phase solution in the step (1) is acetic acid: sulfuric acid = 100: 3-10 (V/V).
Further, the concentration of hydrogen peroxide in the step (2) is more than or equal to 50%, the temperature in the reaction process is 20-80 ℃, the flow rate of the acetic acid mixed solution is 10-20 ml/min, and the flow rate of the hydrogen peroxide is 10-20 ml/min.
Furthermore, a dispersion membrane in the membrane dispersion microreactor is a stainless steel membrane, and the aperture of the dispersion membrane is 1-50 mu m.
The invention has the beneficial effects that: the method takes acetic acid, sulfuric acid and hydrogen peroxide as raw materials, generates no by-products, improves the utilization rate of the hydrogen peroxide, realizes the continuous preparation of the peroxyacetic acid, reduces the consumption of subsequent stored energy, reduces the storage process and reduces the production safety risk. For the process, the equipment adopts a membrane dispersion micro-reactor, the dispersed phase hydrogen peroxide is divided into uniform small droplets after passing through a membrane, and the droplets are uniformly contacted and reacted with the mixed solution of acetic acid, so that the contact area of two phases is increased, the mass transfer process is strengthened, the reaction rate is increased, and the peroxyacetic acid solution with the uniform content is obtained. And the process can accurately control the material ratio, and realizes a rapid, controllable and safe continuous production mode.
Drawings
FIG. 1 is a schematic diagram of a microreactor to produce peroxyacetic acid.
FIG. 2 is a table of the data for detecting peracetic acid produced by the microreactor.
Detailed Description
In order to make the content of the present invention more clearly understood, the technical solutions in the embodiments of the present invention are clearly and completely described below.
Example one
A new process for preparing peroxyacetic acid by taking acetic acid as a raw material through a microreactor comprises the following steps:
1) the preparation proportion is acetic acid: sulfuric acid = 100: 10 (V/V) acetic acid mixed solution;
2) the acetic acid mixed solution is used as a mobile phase, flows at a flow rate of 20ml/min through a flask-heat exchanger-microreactor-heat exchanger, hydrogen peroxide is used as a dispersion phase, is mixed with the acetic acid mixed solution through a stainless steel membrane in a membrane dispersion microreactor at a flow rate of not higher than 16ml/min, an oxidation reaction is carried out at 65 ℃, and sampling is carried out at the interval of a microreactor outlet for 10min to detect the content of finished products of peracetic acid.
According to the above process steps, the peroxyacetic acid detection result shown in fig. 2 is obtained.
Example two
A new process for preparing peroxyacetic acid by taking acetic acid as a raw material through a microreactor comprises the following steps:
1) the preparation proportion is acetic acid: sulfuric acid = 100: 10 (V/V) acetic acid mixed solution;
2) the acetic acid mixed solution is used as a mobile phase, flows at a flow rate of 20ml/min through a flask-heat exchanger-microreactor-heat exchanger, hydrogen peroxide is used as a dispersion phase, is mixed with the acetic acid mixed solution through a stainless steel membrane in a membrane dispersion microreactor at a flow rate of not higher than 16ml/min, an oxidation reaction is carried out at 55 ℃, and sampling is carried out at the interval of a microreactor outlet for 10min to detect the content of finished products of peracetic acid.
According to the above process steps, the peroxyacetic acid detection result shown in fig. 2 is obtained.
EXAMPLE III
A new process for preparing peroxyacetic acid by taking acetic acid as a raw material through a microreactor comprises the following steps:
1) the preparation proportion is acetic acid: sulfuric acid = 100: 10 (V/V) acetic acid mixed solution;
2) the acetic acid mixed solution is used as a mobile phase, flows at a flow rate of 20ml/min through a flask-heat exchanger-microreactor-heat exchanger, hydrogen peroxide is used as a dispersion phase, is mixed with the acetic acid mixed solution through a stainless steel membrane in a membrane dispersion microreactor at a flow rate of not higher than 16ml/min, an oxidation reaction is carried out at 30 ℃, and sampling is carried out at the interval of a microreactor outlet for 10min to detect the content of finished products of peracetic acid.
According to the above process steps, the peroxyacetic acid detection result shown in fig. 2 is obtained.
Example four
A new process for preparing peroxyacetic acid by taking acetic acid as a raw material through a microreactor comprises the following steps:
1) the preparation proportion is acetic acid: sulfuric acid = 100: 5 (V/V) acetic acid mixed solution;
2) the acetic acid mixed solution is used as a mobile phase, flows at a flow rate of 20ml/min through a flask-heat exchanger-microreactor-heat exchanger, hydrogen peroxide is used as a dispersion phase, is mixed with the acetic acid mixed solution through a stainless steel membrane in a membrane dispersion microreactor at a flow rate of not higher than 16ml/min, an oxidation reaction is carried out at 65 ℃, and sampling is carried out at the interval of a microreactor outlet for 10min to detect the content of finished products of peracetic acid.
According to the above process steps, the peroxyacetic acid detection result shown in fig. 2 is obtained.
The present invention and the embodiments thereof have been described above, but the description is not limited to the embodiments, but only one of the embodiments of the present invention, and the actual embodiments are not limited thereto. In conclusion, those skilled in the art should appreciate that they can readily use the disclosed conception and specific embodiments as a basis for designing or modifying other structures for carrying out the same purposes of the present invention without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (6)
1. A new process for preparing peroxyacetic acid by taking acetic acid as a raw material through a microreactor is characterized in that: the method comprises the following steps:
(1) preparing acetic acid and sulfuric acid mixed liquor: firstly, preparing an acetic acid-sulfuric acid mixed solution;
(2) preparation of peracetic acid solution: then the acetic acid mixed solution is used as a mobile phase, the hydrogen peroxide solution is used as a dispersion phase, and the peroxyacetic acid solution is prepared by uniform, rapid mixing and reaction of a membrane dispersion micro-reactor.
2. The novel process for preparing peroxyacetic acid from acetic acid as a raw material through a microreactor as claimed in claim 1, wherein: in the step (1), the concentration of the acetic acid solution is more than or equal to 99.0 percent, the concentration of the sulfuric acid solution is 98 percent, and the proportion of the two-phase solution is acetic acid: sulfuric acid = 100: 3-10 (V/V).
3. The novel process for preparing peroxyacetic acid from acetic acid as a raw material through a microreactor as claimed in claim 1, wherein: the temperature of the two-phase reaction in the step (2) is 20-80 ℃.
4. The novel process for preparing peroxyacetic acid from acetic acid as a raw material through a microreactor as claimed in claim 1, wherein: the material retention time in the microreactor in the step (2) is less than or equal to 5 min.
5. The novel process for preparing peroxyacetic acid from acetic acid as a raw material through a microreactor as claimed in claim 1, wherein: in the step (2), the content of peracetic acid at the outlet of the microreactor channel is more than or equal to 25%.
6. The novel process for preparing peroxyacetic acid from acetic acid as a raw material through a microreactor as claimed in claim 1, wherein: the dispersion membrane in the membrane dispersion microreactor is a stainless steel membrane, and the aperture of the dispersion membrane is 1-50 mu m.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110409150.8A CN113105380A (en) | 2021-04-16 | 2021-04-16 | Novel process for preparing peroxyacetic acid by using acetic acid as raw material through microreactor |
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| CN202110409150.8A CN113105380A (en) | 2021-04-16 | 2021-04-16 | Novel process for preparing peroxyacetic acid by using acetic acid as raw material through microreactor |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114984878A (en) * | 2022-05-24 | 2022-09-02 | 沈阳化工研究院有限公司 | A kind of microreaction continuous synthesis method and device of peracetic acid |
| CN115947441A (en) * | 2023-01-17 | 2023-04-11 | 哈尔滨工业大学 | Method for removing organic pollutants in industrial wastewater by using peracetic acid in cooperation with Fe (II) and hydroxylamine |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103204793A (en) * | 2013-03-05 | 2013-07-17 | 嘉兴学院 | Process and device for synthesizing peroxyacetic acid |
| CN111333559A (en) * | 2020-03-18 | 2020-06-26 | 中国天辰工程有限公司 | Method for rapidly preparing peroxyacetic acid by continuous flow |
| CN111825589A (en) * | 2019-04-17 | 2020-10-27 | 上海朴颐化学科技有限公司 | A kind of method for preparing anhydrous peracetic acid solution with microchannel reactor |
-
2021
- 2021-04-16 CN CN202110409150.8A patent/CN113105380A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103204793A (en) * | 2013-03-05 | 2013-07-17 | 嘉兴学院 | Process and device for synthesizing peroxyacetic acid |
| CN111825589A (en) * | 2019-04-17 | 2020-10-27 | 上海朴颐化学科技有限公司 | A kind of method for preparing anhydrous peracetic acid solution with microchannel reactor |
| CN111333559A (en) * | 2020-03-18 | 2020-06-26 | 中国天辰工程有限公司 | Method for rapidly preparing peroxyacetic acid by continuous flow |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114984878A (en) * | 2022-05-24 | 2022-09-02 | 沈阳化工研究院有限公司 | A kind of microreaction continuous synthesis method and device of peracetic acid |
| CN115947441A (en) * | 2023-01-17 | 2023-04-11 | 哈尔滨工业大学 | Method for removing organic pollutants in industrial wastewater by using peracetic acid in cooperation with Fe (II) and hydroxylamine |
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