CN107739327A - A kind of method for preparing peroxyacetic acid disinfectant - Google Patents
A kind of method for preparing peroxyacetic acid disinfectant Download PDFInfo
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- CN107739327A CN107739327A CN201710951980.7A CN201710951980A CN107739327A CN 107739327 A CN107739327 A CN 107739327A CN 201710951980 A CN201710951980 A CN 201710951980A CN 107739327 A CN107739327 A CN 107739327A
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- acid
- attapulgite
- catalyst
- disinfectant
- glacial acetic
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C407/00—Preparation of peroxy compounds
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N37/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
- A01N37/16—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing the group; Thio analogues thereof
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- 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
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- Pest Control & Pesticides (AREA)
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- Agronomy & Crop Science (AREA)
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Abstract
The invention discloses a kind of method for preparing peroxyacetic acid disinfectant, and using glacial acetic acid and hydrogen peroxide as raw material, it is catalyst that attapulgite, which strengthens polystyrene resin solid acid, and peroxyacetic acid disinfectant is directly prepared by solid super acid reaction.Peracetic acid heterogeneous catalysis new technology disclosed in this invention, the peroxyacetic acid disinfectant produced with the method is free of the concentrated sulfuric acid, realize that Peracetic acid high concentration produces in factory's centralization, eliminate potential safety hazard during traditional mode of production stores, and product is corrosion-free to material surface using process, it is that one kind meets that peroxyacetic acid disinfectant industrializes demand, the very strong new method of practicality.
Description
Technical field
The invention belongs to chemical field, is related to a kind of method for preparing peroxyacetic acid disinfectant, specifically strong with attapulgite
It is catalyst to change polystyrene resin solid acid, uses glacial acetic acid and aqueous hydrogen peroxide solution as raw material, and solid super acid obtains
The method of peroxyacetic acid disinfectant
Background technology
Peracetic acid as a kind of wide spectrum, efficient, quick-acting, the nontoxic noresidue of catabolite environment-friendlydisinfectant disinfectant,
There is killing action to various microorganisms, including fungi, bacterium, gemma and virus, its liquids and gases all has very strong kill
Bacterium ability, it is relatively low plus price, therefore it is widely used in the sterilization of the industries such as food, medicine, medicine equipment.
In recent years, Peracetic acid achieves larger hair in terms of China's food processing machinery and medical apparatus sterilizing sterilization
Exhibition.Peroxyacetic acid disinfectant is limited in food processing machinery and medical apparatus sterilizing, a major reason of germicidal applications, be by
There is stronger corrosivity in Peracetic acid, so as to limit its further genralrlization and application.And traditional peracetic acid disinfectant
Agent is produced using the concentrated sulfuric acid as catalyst, and the concentrated sulfuric acid of residual not only causes the corrosion of sterilisation purpose thing, and due to remaining in production
The concentrated sulfuric acid in product system can be catalyzed the synthesis and decomposition reaction of Peracetic acid, result in product storage and easily sent out with transportation
The accidents such as raw leakage blast.
Disclosed in patent 201410216038.2 it is a kind of using acid cation exchange resin or perfluorinated sulfonic resin or
Immobilized sulfuric acid is catalyst, the method for being continuously synthesizing to Peracetic acid.But immobilized sulfuric acid is there is being easy to run off inactivating, the sulphur of loss
Acid group enters Peracetic acid product, no fundamentally to solve the problems, such as that sulfuric acid is brought.Cationic ion-exchange resin or perfluorinated sulfonic acid
Easily swelling inactivates resin under the strong oxidizing property environment of Peracetic acid building-up process.
Strengthen sulfonated polystyrene ion exchange resin solid acid catalyst the invention discloses a kind of attapulgite and be used for Peracetic acid
Synthesis technique, using batch reaction or the continuous synthesis technique of fixed bed, fundamentally solves resin catalyst in strong oxidizing property
The problems such as stability, immobilized sulfuric acid under environment are easily lost in.
The content of the invention
The technical problem to be solved in the invention is, in prior synthesizing method system, concentrated sulfuric acid residual, and cation exchange
Resin or perfluorinated sulfonic resin easily swelling etc..
In order to solve the technical problem, the invention provides a kind of method for preparing peroxyacetic acid disinfectant.This method with
It is catalyst that attapulgite, which strengthens sulfonated polystyrene ion exchange resin solid acid, uses glacial acetic acid and aqueous hydrogen peroxide solution as material liquid
Solid catalysis obtains peroxyacetic acid disinfectant.
Attapulgite of the present invention, which strengthens sulfonated polystyrene ion exchange resin solid acid catalyst, to be changed with silane coupler
Property attapulgite be stabilizer, pass through Pickering emulsion polymerisation process obtain attapulgite strengthen polystyrene resin
Microballoon, under the sulfonation of the concentrated sulfuric acid, obtain attapulgite and strengthen sulfonated polystyrene ion exchange resin solid acid catalyst.
Specifically, the present invention program is：
A kind of method for preparing peroxyacetic acid disinfectant, using glacial acetic acid and hydrogenperoxide steam generator as raw material, pass through fixed bed
Flow reactor, heterogeneous catalysis prepare peroxyacetic acid disinfectant, wherein, the catalyst that this method uses is that attapulgite strengthens sulphur
Change polystyrene resin solid acid, carried out in a manner of continuous fixed bed reaction or continuous.
Method of the present invention, wherein, the continuous fixed bed reaction or continuous mode comprises the following steps:
Attapulgite is strengthened into sulfonated polystyrene ion exchange resin solid acid catalyst and loads fixed bed reactors, beds
It is incubated in 30-70 degree, preferably 40-60 degree, reactant glacial acetic acid and aqueous hydrogen peroxide solution is injected into reactor with constant speed, passed through
Adjust flow velocity so that the reaction time of described glacial acetic acid and the mixed solution of hydrogen peroxide in fixed bed reactors is 1-
10h, the product that reactor outlet is collected is peroxyacetic acid disinfectant product.
Method of the present invention, wherein, the aqueous hydrogen peroxide solution concentration is 30-50%.
Method of the present invention, wherein, the volume flow rate ratio of glacial acetic acid and hydrogen peroxide is 1：1-1：5.
A kind of method for preparing peroxyacetic acid disinfectant, it is anti-by autoclave using glacial acetic acid and hydrogenperoxide steam generator as raw material
Device is answered, heterogeneous catalysis prepares peroxyacetic acid disinfectant, wherein, the catalyst that this method uses is that attapulgite strengthens sulfonated polyphenyl
Vinyl solid acid, carried out with batch reactive mode.
Method of the present invention, wherein, the addition of catalyst for total reactant quality than 2-10%.
Method of the present invention, wherein, the time of the batch reaction is 2-24h.
Attapulgite of the present invention strengthens sulfonated polystyrene ion exchange resin solid acid, and its preparation method is, even with silane
It is stabilizer to join the attapulgite that agent is modified, and the polyphenyl second of attapulgite reinforcing is obtained by Pickering emulsion polymerisation process
Olefine resin microballoon, under the sulfonation of the concentrated sulfuric acid, obtain attapulgite and strengthen sulfonated polystyrene ion exchange resin solid acid catalyst.
In a currently preferred embodiment,
It is tubular fixed-bed anti-that the attapulgite of 30-50 mesh is strengthened into sulfonated polystyrene ion exchange resin solid acid catalyst 2g loadings
The constant temperature zone of device is answered, remainder is filled with quartz sand.It is 3h in volume space velocity-1Nitrogen flow rate under by beds constant temperature
It is then that 30% aqueous hydrogen peroxide solution is injected separately into system with glacial acetic acid by constant flow pump by concentration to 40 degree, glacial acetic acid
Mass space velocity is 1.2h-1, the mass space velocity of hydrogen peroxide is 0.8h-1, reaction mass enters after being mixed by three-way connection to react
Device, reacted mixture are collected.
The beneficial effects of the present invention are：By screening, obtain and strengthen sulfonated polyphenyl second for the attapulgite of catalysis
Olefine resin solid acid catalyst.
The catalyst effect is preferable, the sulfonation strengthened at concentrations up to 25% using inorganic nano material of Peracetic acid
Polystyrene resin catalyst, traditional concentrated sulfuric acid catalyst can be substituted so that residual without the concentrated sulfuric acid in peroxide ethylene sterilization agent
Stay, not only eliminate potential safety hazard in peroxyacetic acid disinfectant product storage and transportation process, and eliminate traditional Peracetic acid
Severe corrosive during disinfectant use, so as to so that peroxyacetic acid disinfectant is applied to more wide field.
Meanwhile the catalyst belongs to heterogeneous catalyst, after the completion of reaction, it can separate and reclaim from reaction system, can
It is used for multiple times with circulation, obtains more superior economic benefit.The present invention strengthens sulfonated polystyrene ion exchange resin using attapulgite
Solid acid is catalyst, and peroxyacetic acid disinfectant synthesis, and the technique are carried out as reactor using fixed bed or batch reactor
Route is there is not yet document report.
Brief description of the drawings
The attapulgite of Fig. 1 embodiments 6 strengthens sulfonated polystyrene ion exchange resin solid acid catalyst cyclical stability.
Embodiment
Embodiment 1
It is tubular fixed-bed anti-that the attapulgite of 30-50 mesh is strengthened into sulfonated polystyrene ion exchange resin solid acid catalyst 2g loadings
The constant temperature zone of device is answered, remainder is filled with quartz sand.It is 3h in volume space velocity-1Nitrogen flow rate under by beds constant temperature
It is then that 30% aqueous hydrogen peroxide solution is injected separately into system with glacial acetic acid by constant flow pump by concentration to 40 degree, glacial acetic acid
Mass space velocity is 1.2h-1, the mass space velocity of hydrogen peroxide is 0.8h-1, reaction mass enters after being mixed by three-way connection to react
Device, reacted mixture are collected, and through concentration determination, peroxyacetic acid concentration can reach 20.85%.
Embodiment 2
It is tubular fixed-bed anti-that the attapulgite of 30-50 mesh is strengthened into sulfonated polystyrene ion exchange resin solid acid catalyst 2g loadings
The constant temperature zone of device is answered, remainder is filled with quartz sand.It is 3h in volume space velocity-1Nitrogen flow rate under by beds constant temperature
It is then that 30% aqueous hydrogen peroxide solution is injected separately into system with glacial acetic acid by constant flow pump by concentration to 60 degree, glacial acetic acid
Mass space velocity is 2.0h-1, the mass space velocity of hydrogen peroxide is 1.5h-1, reaction mass enters after being mixed by three-way connection to react
Device, reacted mixture are collected, and through concentration determination, peroxyacetic acid concentration can reach 19.63%.
Embodiment 3
It is tubular fixed-bed anti-that the attapulgite of 30-50 mesh is strengthened into sulfonated polystyrene ion exchange resin solid acid catalyst 2g loadings
The constant temperature zone of device is answered, remainder is filled with quartz sand.It is 3h in volume space velocity-1Nitrogen flow rate under by beds constant temperature
It is then that 50% aqueous hydrogen peroxide solution is injected separately into system with glacial acetic acid by constant flow pump by concentration to 60 degree, glacial acetic acid
Mass space velocity is 5.0h-1, the mass space velocity of hydrogen peroxide is 3.0h-1, reaction mass enters after being mixed by three-way connection to react
Device, reacted mixture are collected, and through concentration determination, peroxyacetic acid concentration can reach 22.76%.
Embodiment 4
The attapulgite of 30-50 mesh is strengthened into sulfonated polystyrene ion exchange resin solid acid catalyst 2g and loads round-bottomed flask, is added
Enter glacial acetic acid 60ml, concentration is 30% aqueous hydrogen peroxide solution 40ml, and magnetic agitation is well mixed, and reaction is maintained under 40 degree
Carry out, react catalyst filtration after terminating, produce Peracetic acid product, through concentration determination, react 24 hours, Peracetic acid is dense
Degree can reach 19.48%.
Embodiment 5
The attapulgite of 30-50 mesh is strengthened into sulfonated polystyrene ion exchange resin solid acid catalyst 2g and loads round-bottomed flask, is added
Enter glacial acetic acid 60ml, concentration is 50% aqueous hydrogen peroxide solution 40ml, and magnetic agitation is well mixed, and reaction is maintained under 60 degree
Carry out, react catalyst filtration after terminating, produce Peracetic acid product, through concentration determination, react 24 hours, Peracetic acid is dense
Degree can reach 25.37%.
Embodiment 6
The attapulgite of 30-50 mesh is strengthened into sulfonated polystyrene ion exchange resin solid acid catalyst 2g and loads round-bottomed flask, even
It is continuous to carry out ten batch reactions, the recycling stability of catalyst is investigated, the reactant rate of charge per batch is as follows：Glacial acetic acid
60ml, concentration be 50% aqueous hydrogen peroxide solution 40ml, 40 degree of reaction temperature.As a result as shown in Figure 1, catalyst circulation ten
Secondary, stable in catalytic performance, peroxyacetic acid concentration can maintain more than 24%.
The metal protection testing experiment of embodiment 7 is tested：
In the present embodiment, the equipment used is：
Sheet metal：Copper sheet, carbon steel coupon, aluminium flake, stainless steel substrates.
Assay balance：Sartorius GL124-2SCN.
Disinfectant：The high concentration unitary peroxyacetic acid disinfectant obtained with embodiment in the present invention 1.
Experimental method is as follows：
Test basis：The Ministry of Public Health《Disinfection technology standard》(2002 editions) 2.2.4 metal protections determine
Test condition：25 DEG C of environment temperature, relative humidity 50%
It is that Peracetic acid content is 2000mg/L dilutions to test decontaminant concentration.
Disinfectant is as shown in table 1 to corrosion of metal degree result.
The disinfectant of table 1 is to corrosion of metal degree
According to result it can be seen that：The present invention high concentration unitary peroxyacetic acid disinfectant Peracetic acid content be
2000mg/L dilution is to carbon steel coupon, aluminium flake moderate corrosion, to copper sheet mild corrosion, to stainless steel no corrosion.
Claims (9)
1. a kind of method for preparing peroxyacetic acid disinfectant, using glacial acetic acid and hydrogenperoxide steam generator as raw material, connected by fixed bed
Continuous reactor, heterogeneous catalysis prepare peroxyacetic acid disinfectant, it is characterised in that the catalyst that this method uses is that attapulgite is strong
Change sulfonated polystyrene ion exchange resin solid acid, carried out in a manner of continuous fixed bed reaction or continuous.
2. according to the method for claim 1, it is characterised in that the continuous fixed bed reaction or continuous mode comprises the following steps:
Attapulgite is strengthened into sulfonated polystyrene ion exchange resin solid acid catalyst and loads fixed bed reactors, beds insulation
In 40-60 degree, reactant glacial acetic acid and aqueous hydrogen peroxide solution are injected into reactor with constant speed, by adjusting flow velocity so that institute
Reaction time of the glacial acetic acid and the mixed solution of hydrogen peroxide stated in fixed bed reactors is 1-10h, and reactor outlet is received
The product of collection is peroxyacetic acid disinfectant product.
3. according to the method for claim 2, it is characterised in that the aqueous hydrogen peroxide solution concentration is 30-50%.
4. according to the method for claim 2, it is characterised in that the volume flow rate ratio of glacial acetic acid and hydrogen peroxide is 1：1-1：5.
5. a kind of method for preparing peroxyacetic acid disinfectant, using glacial acetic acid and hydrogenperoxide steam generator as raw material, pass through still reaction
Device, heterogeneous catalysis prepare peroxyacetic acid disinfectant, it is characterised in that the catalyst that this method uses is that attapulgite strengthens sulfonation
Polystyrene resin solid acid, carried out with batch reactive mode.
6. according to the method for claim 5, it is characterised in that the addition of catalyst be total reactant quality than 2-
10%。
7. according to the method for claim 5, it is characterised in that the time of the batch reaction is 2-24h.
8. the attapulgite described in any of the above-described method strengthens sulfonated polystyrene ion exchange resin solid acid, it is characterised in that it is prepared
Method is, using silane coupler modified attapulgite as stabilizer, concave convex rod is obtained by Pickering emulsion polymerisation process
The polystyrene resin microballoon that soil is strengthened, under the sulfonation of the concentrated sulfuric acid, obtain attapulgite and strengthen sulfonated polystyrene tree
Fat solid acid catalyst.
9. the attapulgite described in any of the above-described method strengthens sulfonated polystyrene ion exchange resin solid acid catalyst, it is characterised in that
Its granule size is 30-50 mesh.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201710951980.7A CN107739327A (en) | 2017-10-13 | 2017-10-13 | A kind of method for preparing peroxyacetic acid disinfectant |
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| CN201710951980.7A CN107739327A (en) | 2017-10-13 | 2017-10-13 | A kind of method for preparing peroxyacetic acid disinfectant |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020028657A1 (en) * | 2018-08-02 | 2020-02-06 | Evonik Corporation | Stabilized peroxyacid solutions |
| CN114409582A (en) * | 2022-02-23 | 2022-04-29 | 兰州助剂厂有限责任公司 | Method for preparing peroxyacetic acid and improving stability of peroxyacetic acid by adopting heterogeneous catalyst |
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| CN101284809A (en) * | 2008-04-21 | 2008-10-15 | 江苏九九久科技股份有限公司 | Production method for acetic hyctro peroxide of high concentration by tower type and continuous process |
| CN104193662A (en) * | 2014-05-22 | 2014-12-10 | 上海应用技术学院 | Preparing method of peracetic acid |
| CN106824283A (en) * | 2017-01-16 | 2017-06-13 | 南京工业大学 | A kind of attapulgite reinforced resin solid acid catalyst and preparation method thereof |
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2017
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| CN101284809A (en) * | 2008-04-21 | 2008-10-15 | 江苏九九久科技股份有限公司 | Production method for acetic hyctro peroxide of high concentration by tower type and continuous process |
| CN104193662A (en) * | 2014-05-22 | 2014-12-10 | 上海应用技术学院 | Preparing method of peracetic acid |
| CN106824283A (en) * | 2017-01-16 | 2017-06-13 | 南京工业大学 | A kind of attapulgite reinforced resin solid acid catalyst and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020028657A1 (en) * | 2018-08-02 | 2020-02-06 | Evonik Corporation | Stabilized peroxyacid solutions |
| CN112512320A (en) * | 2018-08-02 | 2021-03-16 | 赢创有限公司 | Stabilized peroxyacid solutions |
| CN112512320B (en) * | 2018-08-02 | 2022-07-08 | 赢创有限公司 | Stabilized peroxyacid solutions |
| US11779013B2 (en) | 2018-08-02 | 2023-10-10 | Evonik Corporation | Stabilized peroxyacid solutions |
| CN114409582A (en) * | 2022-02-23 | 2022-04-29 | 兰州助剂厂有限责任公司 | Method for preparing peroxyacetic acid and improving stability of peroxyacetic acid by adopting heterogeneous catalyst |
| CN114409582B (en) * | 2022-02-23 | 2024-05-14 | 兰州助剂厂股份有限公司 | Method for preparing peroxyacetic acid by heterogeneous catalyst and improving stability of peroxyacetic acid |
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Application publication date: 20180227 |