CN107602435A - The method that glyceryl triacetate prepares Peracetic acid - Google Patents
The method that glyceryl triacetate prepares Peracetic acid Download PDFInfo
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- CN107602435A CN107602435A CN201610541813.0A CN201610541813A CN107602435A CN 107602435 A CN107602435 A CN 107602435A CN 201610541813 A CN201610541813 A CN 201610541813A CN 107602435 A CN107602435 A CN 107602435A
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- peracetic acid
- acid
- glyceryl triacetate
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C409/00—Peroxy compounds
- C07C409/24—Peroxy compounds the —O—O— group being bound between a >C=O group and hydrogen, i.e. peroxy acids
- C07C409/26—Peracetic acid
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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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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The present invention relates to the technology of preparing of Peracetic acid, a kind of method of glyceryl triacetate preparation Peracetic acid.Prior art prepare Peracetic acid the shortcomings that be：The Peracetic acid product of preparation has strong acetic acid penetrating odor；Product stability is poor.The inventive method is as follows：Take following raw material：The parts by weight of 95% glyceryl triacetate 10-50, the parts by weight of 50% hydrogen peroxide 10 50, the parts by weight of 98% concentrated sulfuric acid 1-3, the parts by weight of 95% ethanol 5-15, the parts by weight of stabilizer 0.1-0.5, addition purified water to 100 parts by weight；Concentrated sulfuric acid catalyst is added in hydrogenperoxide steam generator and stirred, while sequentially adds ethanol, glyceryl triacetate and stabilizer and purified water, at the uniform velocity stirs one hour and is made.Advantages of the present invention：The Peracetic acid product of preparation is without acetic acid penetrating odor；Product stability is good, production and storage safety.
Description
Technical field
The present invention relates to a kind of preparation method of Peracetic acid, specifically glyceryl triacetate prepares Peracetic acid
Method.
Background technology
Peracetic acid, molecular formula C2H4O3, colourless liquid, there is the typical scent of acetic acid.
Structural formula is：
Peracetic acid is strong oxidizer, there is severe corrosive.Peracetic acid has important purposes in multiple technologies field.Example
Such as：As paper, paraffin, timber, fabric, grease, starch bleaching agent；Organic industry be used as manufacture expoxy propane, glycerine, oneself
The oxidant and epoxidizing agent of lactams；Plastics industry is used to manufacture epoxy resin and plasticizer；It is used as chemistry in analytical chemistry
Reagent；Also act as preservative etc..
Peracetic acid or a kind of wide spectrum, efficient, cheap disinfectant and bactericidal agent, to bacterial propagule, fungi, virus
There is very strong killing action with gemma etc..Suitable for hospital, restaurant, public place, infectious disease disinfection of epidemic focus, sanitary ware
Sterilization and non-metal medical apparatus, amenities sterilization and sterilizing.Peracetic acid using rear residue be water, carbon dioxide and
Oxygen, residue is safe and non-toxic, is clean, free of contamination oxidizing biocide.
Prior art prepare Peracetic acid method be：Using acetic acid, hydrogen peroxide as raw material, using inorganic acid as catalyst system
Standby Peracetic acid.Because the reaction that acetic acid, hydrogen peroxide prepare Peracetic acid is reversible reaction, so can not be kept away in final products
Exempt from hydrogen peroxide, acetic acid and Peracetic acid simultaneously be present.
The shortcomings that prior art is：
1. product has strong acetic acid penetrating odor.
2. Peracetic acid product stability is poor, explosion limit is low, especially in the presence of a large amount of metal ions, production
Potential safety hazard be present with storage.
3. under low concentration use state, product easily decomposes, and stability is poor, can be used the time limit not lasting enough.
Therefore invent a kind of Peracetic acid product has no irritating odor, stability is good, production and storage safety, useful life
The method that long glyceryl triacetate prepares Peracetic acid is very necessary.
The content of the invention
Had no irritating odor it is an object of the invention to provide one kind, stability is good, production and storage are safe, validity period limit for length
Glyceryl triacetate prepare Peracetic acid method.
What the object of the invention was realized in：
A kind of method that glyceryl triacetate prepares Peracetic acid, step are as follows：
(1) following raw material for standby is accurately weighed：
(2) hydrogenperoxide steam generator is prepared, it is standby；
(3) 98% concentrated sulfuric acid is added in step (2) product, stirring；
(4) ethanol, glyceryl triacetate, stabilizer, purified water are added into step (3) product successively；
(5) at the uniform velocity stir one hour and be made.
Stabilizer is one kind in potassium dihydrogen phosphate, dipotassium hydrogen phosphate, sodium pyrophosphate, 1-hydroxy ethylidene-1,1-diphosphonic acid.
98% concentrated sulfuric acid in step (1) of the present invention is catalyst.
The present invention is characterized by:Concentrated sulfuric acid catalyst is added in hydrogenperoxide steam generator and stirred, while is added successively again
Enter ethanol, glyceryl triacetate and stabilizer and purified water, at the uniform velocity stir one hour and be made.
The raw material that prior art prepares Peracetic acid is hydrogen peroxide, acetic acid and catalyst.It is anti-due to preparing Peracetic acid
Should be reversible reaction, so hydrogen peroxide, acetic acid and Peracetic acid in final products unavoidably be present.Because acetic acid has by force
Strong penetrating odor, so the Peracetic acid of prior art production has strong impulse smell, so as to influence to use.This hair
It is bright to use glyceryl triacetate to replace acetic synthesis Peracetic acid for raw material.Course of reaction is as follows：1. glyceryl triacetate is being urged
Reversible reaction generation glycerine and acetic acid in the presence of agent；2. the acetic acid of generation is reversible with hydrogen peroxide in the presence of catalyst
Reaction generation Peracetic acid.Because the equilibrium constant of second step reaction is big compared with the equilibrium constant that the first step is reacted, so reacting
When being finally reached balance, the acetic acid of physical presence is seldom in solution.The Peracetic acid intense stimulus smell prepared with prior art
Compare, Peracetic acid prepared by the present invention eliminates the acetic acid penetrating odor in product, simultaneously because glyceryl triacetate has
There is the fragrant pleasant smell of ester, plus the alcohol taste of ethanol so that Peracetic acid product odour mellowness of the present invention.
Based on above-mentioned reaction mechanism and process, due to two step balanced reactions, the step with prior art Peracetic acid be present
Balanced reaction is compared, and the molecular acid to dissociate in peracetic acid soln prepared by the present invention is few；Simultaneously because ethanol is in catalyst
In the presence of reversible balanced reaction can be formed with acetic acid so that the stability of Peracetic acid greatly improves.In same transport, storage
Under conditions of, Peracetic acid rate of descent is low, stablizes, and production, storing and transporting security greatly improve.
Existing peracetic acid soln in the case where being diluted to low concentration solution, accelerate by decomposition of peracetic acid, general low
Strength solution effective life, is no more than 3 days.The present invention provides because glyceryl triacetate can be stablized in the case of low concentration
Acetic acid molecule, suppress balanced reaction and elapsed to hydrogen peroxide, acetic acid direction so that peracetic acid soln of the present invention is diluted to low dense
Stable peroxyacetic acid concentration can be kept when spending solution for a long time, low concentration peracetic acid soln validity period extends, up to 6-
10 days, compared with existing peracetic acid soln, peracetic acid soln prepared by the present invention had good persistence.
Experiment proves that Peracetic acid can strengthen the killing action to bacterium, virus under the ethanol effect of low concentration.This hair
The ethanol of raw material 95% in bright can also increase product bactericidal effect in addition to product odour and increase stability purposes is improved.
Product of the present invention is widely used in disinfection field, has and efficiently kills bacterium, the effect of virus.
The present invention can also select 27.5%, 30% hydrogen peroxide raw material according to the separate sources of raw material, but will need to make
The hydrogen peroxide that dosage is converted into 50% calculates.When using 27.5% or 30% hydrogen peroxide, according to the proportioning of each raw material,
It can also less add or be not added with purified water.
It is an advantage of the invention that：
1. product is without acetic acid penetrating odor.
2. Peracetic acid product stability prepared by the present invention is good, production and storage safety.
3. Peracetic acid product prepared by the present invention is when being diluted to low concentration liquid, validity period limit for length.
Embodiment：
Below by embodiment, the present invention will be further described.
Embodiment 1：
Prepare 500kg Peracetic acid：
Stirred 1. the 15kg concentrated sulfuric acids are added in 175kg30% hydrogenperoxide steam generators；
2. sequentially adding 75kg95% ethanol, 125kg95% glyceryl triacetates, 1kg sodium pyrophosphates, add purified water
109kg；
3. at the uniform velocity stirring 1 hour, 3.5% peracetic acid soln is made.
Embodiment 2：
Prepare 500kg Peracetic acid：
1. the 15kg concentrated sulfuric acids are added in 255kg30% hydrogenperoxide steam generators, stir；
2. sequentially add 54kg95% ethanol, 175kg95% glyceryl triacetates, 1kg 1-hydroxy ethylidene-1,1-diphosphonic acids；
3. at the uniform velocity stir the peracetic acid soln of 1 hour obtained 7.5%.
Embodiment 3：
Prepare 500kg Peracetic acid：
1. the 10kg concentrated sulfuric acids are added in 215kg50% hydrogenperoxide steam generators, stir；
2. sequentially add 60kg95% ethanol, 214kg95% glyceryl triacetates, 1kg sodium pyrophosphates；
3. at the uniform velocity stir the peracetic acid soln of 1 hour obtained 15%.
Peracetic acid soln performance prepared by the embodiment of the present invention is as follows:
1. product stability test result:
Table 1:
| Initial content | 1 year content | 1 year rate of descent | |
| Embodiment 1 | 3.62% | 3.43% | 5.2% |
| Embodiment 2 | 7.90% | 7.53% | 4.7% |
| Embodiment 3 | 16.4% | 15.7% | 4.3% |
The stability data of the present invention means the data that the cool dark place of product preserves.Content is pressed《GB 19104-2008 peroxide second
Acid solution》Middle determination of peracetic acid item is measured.
Measurement result shows that product stability of the present invention is good, and 1 year rate of descent is 4.3%--5.2%.Existing similar peroxide
1 year rate of descent of acetic acid product is more than 18%.
2. low concentration solution persistence detects：
Table 2:0.3% peracetic acid soln 3 days, 6 days, content on the 10th
| Initial content | Content on the 3rd | Content on the 6th | Content on the 10th | |
| The dilution of embodiment 1 | 0.30% | 0.27% | 0.24% | 0.21% |
| The dilution of embodiment 2 | 0.31% | 0.27% | 0.23% | 0.22% |
| The dilution of embodiment 3 | 0.28% | 0.25% | 0.22% | 0.20% |
Table 2 detects for low concentration solution persistence.Detection method:Peracetic acid prepared by different embodiments adds purifying
Water is diluted to the solution of concentration 0.3%, and room temperature is placed, and its content is determined respectively at 3 days, 6 days, 10 days.It is of the invention as seen from the above table
Product configuration low concentration solution, Peracetic acid content met requirement in 10 days, more than existing 3 day effective life.
3.0.30% peracetic acid soln sterilization test：Press《Disinfection technology standard 2002 editions》Peracetic acid disinfectant is entered
Row sterilization test.Product of the present invention is diluted to 0.3% strength solution, test result is：Bacterial propagule can be killed within 1 minute；5
Minute kills tubercle bacillus and fungi；Kill spores of bacillus subtilin within 30 minutes.
Above-described embodiment is only the preference of the present invention, is not intended to limit the present invention, all within the principle of the present invention,
Any modifications and variations done, within protection scope of the present invention.
Claims (2)
1. a kind of method that glyceryl triacetate prepares Peracetic acid, step are as follows：
(1) following raw material for standby is accurately weighed：
(2) 50% hydrogenperoxide steam generator is taken to load container, it is standby；
(3) 98% concentrated sulfuric acid is added in step (2) product, stirring；
(4) 95% ethanol, 95% glyceryl triacetate, stabilizer, purifying are added into step (3) product successively while stirring
Water；
(5) at the uniform velocity stir one hour and be made.
2. the method that glyceryl triacetate according to claim 1 prepares Peracetic acid, it is characterised in that：Stabilizer is phosphorus
One kind in acid dihydride potassium, dipotassium hydrogen phosphate, sodium pyrophosphate, 1-hydroxy ethylidene-1,1-diphosphonic acid.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610541813.0A CN107602435A (en) | 2016-07-12 | 2016-07-12 | The method that glyceryl triacetate prepares Peracetic acid |
| CN202211651168.XA CN116102481A (en) | 2016-07-12 | 2016-07-12 | Method for preparing peracetic acid from glyceryl triacetate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610541813.0A CN107602435A (en) | 2016-07-12 | 2016-07-12 | The method that glyceryl triacetate prepares Peracetic acid |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211651168.XA Division CN116102481A (en) | 2016-07-12 | 2016-07-12 | Method for preparing peracetic acid from glyceryl triacetate |
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| Publication Number | Publication Date |
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| CN107602435A true CN107602435A (en) | 2018-01-19 |
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| CN201610541813.0A Pending CN107602435A (en) | 2016-07-12 | 2016-07-12 | The method that glyceryl triacetate prepares Peracetic acid |
| CN202211651168.XA Pending CN116102481A (en) | 2016-07-12 | 2016-07-12 | Method for preparing peracetic acid from glyceryl triacetate |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202211651168.XA Pending CN116102481A (en) | 2016-07-12 | 2016-07-12 | Method for preparing peracetic acid from glyceryl triacetate |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB803159A (en) * | 1956-07-31 | 1958-10-22 | Union Carbide Corp | Process for producing peracids from aliphatic carboxylic acids |
| EP0125781A1 (en) * | 1983-04-14 | 1984-11-21 | Interox Chemicals Limited | Peroxygen compounds |
| JPH10330357A (en) * | 1997-05-28 | 1998-12-15 | Arakawa Chem Ind Co Ltd | Production of peracid |
| CN102197025A (en) * | 2008-10-31 | 2011-09-21 | 埃科莱布有限公司 | Enhanced stability peracid compositions |
| WO2012090124A2 (en) * | 2010-12-29 | 2012-07-05 | Ecolab Usa Inc. | IN SITU GENERATION OF PEROXYCARBOXYLIC ACIDS AT ALKALINE pH, AND METHODS OF USE THEREOF |
| CN104364384A (en) * | 2012-03-30 | 2015-02-18 | 纳幕尔杜邦公司 | Enzymes useful for peracid production |
-
2016
- 2016-07-12 CN CN201610541813.0A patent/CN107602435A/en active Pending
- 2016-07-12 CN CN202211651168.XA patent/CN116102481A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB803159A (en) * | 1956-07-31 | 1958-10-22 | Union Carbide Corp | Process for producing peracids from aliphatic carboxylic acids |
| EP0125781A1 (en) * | 1983-04-14 | 1984-11-21 | Interox Chemicals Limited | Peroxygen compounds |
| JPH10330357A (en) * | 1997-05-28 | 1998-12-15 | Arakawa Chem Ind Co Ltd | Production of peracid |
| CN102197025A (en) * | 2008-10-31 | 2011-09-21 | 埃科莱布有限公司 | Enhanced stability peracid compositions |
| WO2012090124A2 (en) * | 2010-12-29 | 2012-07-05 | Ecolab Usa Inc. | IN SITU GENERATION OF PEROXYCARBOXYLIC ACIDS AT ALKALINE pH, AND METHODS OF USE THEREOF |
| CN104364384A (en) * | 2012-03-30 | 2015-02-18 | 纳幕尔杜邦公司 | Enzymes useful for peracid production |
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| CN116102481A (en) | 2023-05-12 |
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