CN117736129A - Preparation method based on stability of peroxyacetic acid - Google Patents
Preparation method based on stability of peroxyacetic acid Download PDFInfo
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- CN117736129A CN117736129A CN202311741371.0A CN202311741371A CN117736129A CN 117736129 A CN117736129 A CN 117736129A CN 202311741371 A CN202311741371 A CN 202311741371A CN 117736129 A CN117736129 A CN 117736129A
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- acid
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- peroxyacetic
- phosphoric acid
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- KFSLWBXXFJQRDL-UHFFFAOYSA-N Peracetic acid Chemical compound CC(=O)OO KFSLWBXXFJQRDL-UHFFFAOYSA-N 0.000 title claims abstract description 316
- 238000002360 preparation method Methods 0.000 title abstract description 15
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 212
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 141
- 238000006243 chemical reaction Methods 0.000 claims abstract description 137
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 106
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 98
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 82
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims abstract description 78
- ZGTMUACCHSMWAC-UHFFFAOYSA-L EDTA disodium salt (anhydrous) Chemical compound [Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O ZGTMUACCHSMWAC-UHFFFAOYSA-L 0.000 claims abstract description 63
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims abstract description 54
- 229920000056 polyoxyethylene ether Polymers 0.000 claims abstract description 51
- 229940051841 polyoxyethylene ether Drugs 0.000 claims abstract description 50
- OKBMCNHOEMXPTM-UHFFFAOYSA-M potassium peroxymonosulfate Chemical compound [K+].OOS([O-])(=O)=O OKBMCNHOEMXPTM-UHFFFAOYSA-M 0.000 claims abstract description 49
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 claims abstract description 44
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- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 claims abstract description 39
- 239000000645 desinfectant Substances 0.000 claims abstract description 27
- 230000004913 activation Effects 0.000 claims abstract description 20
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- 150000003254 radicals Chemical class 0.000 claims description 39
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- 229910021645 metal ion Inorganic materials 0.000 claims description 20
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- 230000009467 reduction Effects 0.000 claims description 3
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- FQENQNTWSFEDLI-UHFFFAOYSA-J sodium diphosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])([O-])=O FQENQNTWSFEDLI-UHFFFAOYSA-J 0.000 description 4
- 229940048086 sodium pyrophosphate Drugs 0.000 description 4
- 235000019818 tetrasodium diphosphate Nutrition 0.000 description 4
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 239000005725 8-Hydroxyquinoline Substances 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- 229920001661 Chitosan Polymers 0.000 description 1
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 235000021355 Stearic acid Nutrition 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
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- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
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- MPNNOLHYOHFJKL-UHFFFAOYSA-N peroxyphosphoric acid Chemical compound OOP(O)(O)=O MPNNOLHYOHFJKL-UHFFFAOYSA-N 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
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- MCJGNVYPOGVAJF-UHFFFAOYSA-N quinolin-8-ol Chemical compound C1=CN=C2C(O)=CC=CC2=C1 MCJGNVYPOGVAJF-UHFFFAOYSA-N 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a preparation method based on the stability of peroxyacetic acid, which is used for adapting the peroxyacetic acid product, placing acetic acid, sulfuric acid and hydrogen peroxide into a reaction kettle and fully stirring for more than 6 hours to obtain a solution A; the solution A is a monobasic peroxyacetic acid solution; checking the solution A in the reaction kettle, ensuring that the solution A is uniformly distributed and has no solid residue under visual conditions, and transferring the solution A into an activation container for activation for more than 24 hours to obtain the solution A; taking a sample in the solution A to detect the content of the peracetic acid, and determining the content of the peracetic acid in the reagent A; pouring the solution A into a reaction kettle, and adding phosphoric acid, disodium ethylenediamine tetraacetate, polyoxyethylene ether, propionic acid, diethylenetriamine penta-subunit phosphoric acid and potassium hydrogen peroxymonosulfate into the solution A; stirring and mixing to obtain a unitary peracetic acid disinfectant; it is desirable to ameliorate the problem of decreased concentration of peracetic acid sanitizing products over extended shelf life.
Description
Technical Field
The invention relates to a peroxyacetic acid disinfectant, in particular to a preparation method based on the stability of peroxyacetic acid.
Background
Peracetic acid is a strong oxidizing agent that kills a variety of microorganisms including viruses, bacteria, fungi, and spores, and thus is often used as a disinfectant. The current application range of the peroxyacetic acid comprises air, environment disinfection and preventive disinfection; generally, a 0.2% solution of peracetic acid can substantially achieve sterilization purposes about 10 minutes in contact with an object. In the actual storage process, the peracetic acid is relatively stable under normal use conditions, but in a preservation environment, the peracetic acid disinfectant can be influenced by external environment, so that an unstable phenomenon occurs in the peracetic acid disinfectant, such as a rapid concentration drop occurs in the concentration of the peracetic acid disinfectant along with the extension of the preservation time. The characteristic of peracetic acid is unstable because the chemical structure of peracetic acid has a peroxide bond, and the peroxide bond contains two oxygen atoms, so that the peroxide bond is easier to break compared with a common carbon-oxygen bond, and the peracetic acid is easy to decompose and release oxygen under specific conditions; resulting in peroxyacetic acid with a certain risk of being exposed to the naked eye.
In the actual application process, the stabilizer is introduced into the peracetic acid at present, so that the stability of the peracetic acid disinfectant is improved, and the explosion risk is reduced. However, in the process of storing the peracetic acid, besides natural decomposition, factors influencing the decomposition of the peracetic acid include light, concentration, temperature, acidity and metal ions in the solution, and the addition of a stabilizer is commonly adopted at present to influence the storage of the peracetic acid solution, so that the concentration reduction period of the peracetic acid disinfectant in the process of storing is shorter, but the use effect of the peracetic acid may be insufficient when the peracetic acid disinfectant is stored for a certain period of time. Therefore, how to optimize the stability of the peroxyacetic acid disinfection product is worth studying.
Disclosure of Invention
The object of the present invention is to provide a preparation method based on the stability of peracetic acid, in order to desirably improve the problem that the concentration of peracetic acid sterilizing products decreases with prolonged storage time.
In order to solve the technical problems, the invention adopts the following technical scheme:
a method of preparing a peroxyacetic acid based stability, the method for adapting a peroxyacetic acid product comprising: according to the weight portions, 20 to 30 portions of hydrogen peroxide, 60 to 70 portions of acetic acid, 2 to 4 portions of sulfuric acid, 5 to 6 portions of phosphoric acid, 0.5 to 1 portion of disodium ethylenediamine tetraacetate, 0.2 to 0.3 portion of polyoxyethylene ether, 0.5 to 1 portion of propionic acid, 0.25 to 0.5 portion of diethylenetriamine pentasubunit phosphoric acid and 0.5 to 1 portion of potassium hydrogen peroxymonosulfate are taken for standby.
Placing the acetic acid, sulfuric acid and hydrogen peroxide into a reaction kettle and fully stirring for more than 6 hours to obtain a solution A; the solution A is a monobasic peroxyacetic acid solution; checking the solution A in the reaction kettle, ensuring that the solution A is uniformly distributed and has no solid residue under visual conditions, and transferring the solution A into an activation container for activation for more than 24 hours to obtain the solution A; taking a sample in the solution A to detect the content of the peracetic acid, and determining the content of the peracetic acid in the reagent A; pouring the solution A into a reaction kettle, and adding phosphoric acid, disodium ethylenediamine tetraacetate, polyoxyethylene ether, propionic acid, diethylenetriamine penta-subunit phosphoric acid and potassium hydrogen peroxymonosulfate into the solution A; stirring and mixing to obtain a unitary peracetic acid disinfectant; the disodium ethylenediamine tetraacetate, phosphoric acid, polyoxyethylene ether, propionic acid, diethylenetriamine penta-subunit phosphoric acid and potassium hydrogen peroxymonosulfate are used for being in balance and combination with each other in a reaction system to inhibit decomposition of peracetic acid.
Preferably, the acetic acid is placed in a reaction kettle; sulfuric acid and hydrogen peroxide are slowly added into the container in sequence, and the temperature range of the reaction kettle is below 25 ℃.
Preferably, the activation temperature of the solution A in the activation vessel is in the range of 65-70 ℃.
Preferably, the hydrogen peroxide has an electron-grade purity and a concentration of 36%; the concentration of the acetic acid is 99.8%, and the quality grade of the acetic acid is pharmaceutical grade; the concentration of the sulfuric acid is 98%; the purity of the sulfuric acid is electronic grade; the acetic acid and hydrogen peroxide produce peroxyacetic acid, and the sulfuric acid catalyzes the peroxyacetic acid to produce monoperoxyacetic acid.
Preferably, the quality grade of the phosphoric acid is food grade, and the purity of the phosphoric acid is 99.8%, and the phosphoric acid is used for adjusting the pH value of the reaction system and maintaining the acid-base balance of the reaction system.
Preferably, the disodium edetate is of pharmaceutical grade and has a purity of 99.6%, and as a chelating agent, the disodium edetate is used in combination with potassium hydrogen monosulfate to promote radical reaction and inhibit the reaction of metal ions with peroxyacetic acid.
Preferably, the polyoxyethylene ether is polyoxyethylene ether Aeo-9, and the purity of the polyoxyethylene ether is 96.5%; the polyoxyethylene ether is used for adjusting the surface tension of the solution A, and disodium ethylenediamine tetraacetate, phosphoric acid, propionic acid, diethylenetriamine pentasubunit phosphoric acid and potassium hydrogen peroxymonosulfate are uniformly distributed in the solution A by the polyoxyethylene ether.
Preferably, the quality grade of the diethylenetriamine penta-subunit phosphoric acid is pharmaceutical grade, the purity of the diethylenetriamine penta-subunit phosphoric acid is 98%, the diethylenetriamine penta-subunit phosphoric acid is used for combining with the active site of the peroxyacetic acid, and the diethylenetriamine penta-subunit phosphoric acid is matched with potassium hydrogen peroxymonosulfate to inhibit the concentration of the monoperoxyacetic acid from rapidly decreasing.
Preferably, the quality grade of the potassium hydrogen peroxymonosulfate is pharmaceutical grade, and the purity of the potassium hydrogen peroxymonosulfate is 99.5 percent; the potassium hydrogen peroxymonosulfate is used for reacting residual hydrogen peroxide with acetic acid and sulfuric acid as a stabilizer and triggering reaction free radicals in organic molecules in disodium ethylenediamine tetraacetate, phosphoric acid, polyoxyethylene ether, propionic acid and diethylenetriamine penta-subunit phosphoric acid and promoting the formation of polymer chains.
Preferably, the purity of the propionic acid is 99.6%, and the propionic acid is mixed with phosphoric acid in the mixing process to maintain acid-base balance, so that the growth of microorganisms in the monoperoxyacetic acid disinfectant is inhibited by the propionic acid.
Compared with the prior art, the invention has the beneficial effects that at least one of the following is adopted:
the invention adopts the acetic acid, the sulfuric acid and the hydrogen peroxide as basic reaction materials, and the reaction materials are all high-purity raw materials, thereby being beneficial to improving the quality stability and the safety of products. By adding disodium ethylenediamine tetraacetate, phosphoric acid, polyoxyethylene ether, propionic acid, diethylenetriamine pentasubunit phosphoric acid, potassium hydrogen peroxymonosulfate and other substances, organic molecules in the system are balanced with each other, and decomposition of peracetic acid is inhibited, so that the stability and activity of the product are improved. The solution A is transferred into an activation container for activation, and the activation temperature is controlled within 65-70 ℃, so that the activity and the sterilization effect of the product are further improved. Meanwhile, through the combined action of substances such as disodium ethylenediamine tetraacetate, phosphoric acid, polyoxyethylene ether, propionic acid, diethylenetriamine pentasubunit phosphoric acid, potassium hydrogen peroxymonosulfate and the like, the rapid decrease of the concentration of the peroxyacetic acid can be inhibited, and the stability and the durability of the product are improved. And the polyoxyethylene ether is uniformly distributed in the solution, so that the uniformity and stability of the solution are ensured. The disodium edetate and the metal ions form a coordination compound, so that the coordination compound and the metal ions in the peroxyacetic acid are chelated, the reaction between the metal ions and the peroxyacetic acid is reduced, the stability of the monoperoxyacetic acid is improved, and simultaneously, the disodium edetate is matched with the potassium peroxymonosulfate to accelerate the generation of free radicals and the reaction process, so that the formation of the monoperoxyacetic acid is further promoted.
Detailed Description
The present invention will be described in further detail with reference to the following background and examples in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
The existing peroxyacetic acid belongs to a strong oxidant, so that the peroxyacetic acid has very good disinfection capability, but the peroxyacetic acid is easy to cause poor stability and easy to decompose. The existing stabilizer can reduce the decomposition speed of the peroxyacetic acid, improve the stability of the peroxyacetic acid and reduce the explosion risk. However, the stabilizer may react with the peroxyacetic acid to regulate its decomposition process, but does not stop completely. Thus, the concentration of peracetic acid gradually decreases over time even if a stabilizer is added. When a certain low concentration value is reached, the disinfection effect may no longer be evident.
For example, conventional phenolic compounds, in which the phenolic compound and peracetic acid may produce an adduct of hydrogen peroxide and a phenolic compound, such as a phenolic ether, may be effective in delaying the decomposition of peracetic acid and improving its stability, due to the slower reaction involved in the phenolic compound compared to the decomposition of peracetic acid itself. However, peracetic acid is consumed during the reaction, and the concentration of peracetic acid may be reduced during long-term preservation.
For example, in the preparation process of peroxyacetic acid, more 8-hydroxyquinoline or sodium pyrophosphate is added as a stabilizer for use, but due to the characteristic of sodium pyrophosphate, a certain corrosion inhibitor is usually added to reduce the corrosiveness of the prepared body fluid product to instruments. Secondly, although sodium pyrophosphate has a better stabilizing effect, the decomposition speed of the peroxyacetic acid can be slowed down, and the service life of the sodium pyrophosphate is prolonged, the peroxyacetic acid still has higher instability, and the peroxyacetic acid can be gradually decomposed along with the time, so that the concentration is reduced.
One embodiment of the invention is a preparation method based on the stability of peroxyacetic acid, which is used for adapting the peroxyacetic acid product, preparing a disinfectant by raw materials, taking 30g of hydrogen peroxide, 68g of acetic acid, 2g of sulfuric acid, 5g of phosphoric acid, 0.5g of disodium ethylenediamine tetraacetate, 0.2g of polyoxyethylene ether, 0.5g of propionic acid, 0.2g of diethylenetriamine penta-subunit phosphoric acid and 0.5g of potassium hydrogen peroxymonosulfate for standby.
Placing the acetic acid, sulfuric acid and hydrogen peroxide into a reaction kettle and fully stirring for more than 6 hours to obtain a solution A; the solution A is a monobasic peroxyacetic acid solution; the solution A is a monobasic peracetic acid solution, the peracetic acid is obtained by the reaction of acetic acid and hydrogen peroxide, and the monobasic peracetic acid is obtained by catalyzing the peracetic acid with sulfuric acid. Wherein, acetic acid, sulfuric acid and hydrogen peroxide are fully stirred for more than 6 hours in a reaction kettle, so that the acetic acid and the hydrogen peroxide can be converted into monoperoxyacetic acid for a sufficient reaction time. Compared with the method that acetic acid and hydrogen peroxide react normally to obtain monoperoxyacetic acid, the monoperoxyacetic acid is more stable and safer through a sulfuric acid catalysis mode. The principle is as follows: sulfuric acid is used as a catalyst in the reaction, so that the reaction rate of acetic acid and peracetic acid is accelerated, specifically, sulfuric acid promotes migration of oxygen atoms through participation in the reaction, so that one oxygen atom in acetic acid and hydroxyl in peracetic acid react to generate monoperoxyacetic acid, the reaction rate and the yield of products are objectively improved, and the reaction time is shortened.
Checking the solution A in the reaction kettle, ensuring that the solution A is uniformly distributed and has no solid residue under visual conditions, namely determining the maintenance concentration of the peracetic acid, and checking whether the solution A is completely reacted, wherein the purpose of checking the solution A is to ensure the completeness of the reaction, and avoiding the conditions that unreacted complete products possibly appear in the reaction process, the subsequent stability is reduced and the like. By checking the solution A, the reaction degree and the stability of the product can be verified, so that the accuracy of the experiment and the reliability of the result are ensured. In the process of preparing the unitary peroxyacetic acid, the adiabatic temperature rise is in direct proportion to the reaction heat release amount, and if the condition of large decomposition heat release amount occurs, the efficiency of the adiabatic temperature rise can be increased, so that a certain explosion risk exists in the preparation process. Strict temperature control and monitoring of the reaction is therefore required.
The solution A is used for checking and helping to judge whether the reaction reaches an equilibrium state, and if the reaction is complete, the solution A is completely reacted. If unreacted acetic acid or peracetic acid is still present in the solution A, this indicates that the reaction has not been completed, and the reaction time is prolonged or the reaction conditions are adjusted. Wherein, checking whether there is a solid residue in the solution A can also judge whether the reaction is abnormal or a reaction by-product exists.
Since peracetic acid contains one hydroxyl peroxy group, the chemical property of the peracetic acid is strong in oxidizing property. And the molecule of acetic acid contains a carboxylic acid group, when acetic acid reacts with peracetic acid, an oxygen atom is withdrawn from a hydroxyl group in peracetic acid to replace an oxygen atom in acetic acid, so that the one oxygen atom in acetic acid and the hydroxyl group in peracetic acid are combined to form peracetic acid, and the molecule of the monoperoxyacetic acid simultaneously contains a structural unit of peracetic acid. Thus, transferring the solution A to an activation container for more than 24 hours for activation to obtain the solution A; taking a sample in the solution A to detect the content of the peracetic acid, and determining the content of the peracetic acid in the reagent A; and (3) taking a sample in the solution A for detecting the content of the peracetic acid, and determining the content of the peracetic acid in the solution A. The content of peracetic acid in the solution a is determined by selecting a suitable analytical method, such as titration or high performance liquid chromatography.
Pouring the solution A into a reaction kettle, and adding phosphoric acid, disodium ethylenediamine tetraacetate, polyoxyethylene ether, propionic acid, diethylenetriamine penta-subunit phosphoric acid and potassium hydrogen peroxymonosulfate into the solution A; stirring and mixing to obtain a unitary peracetic acid disinfectant; the disodium ethylenediamine tetraacetate, phosphoric acid, polyoxyethylene ether, propionic acid, diethylenetriamine penta-subunit phosphoric acid and potassium hydrogen peroxymonosulfate are used for being in balance and combination with each other in a reaction system to inhibit decomposition of peracetic acid. Before the solution A is poured into a reaction kettle, the content of the peracetic acid in the solution A is ensured to be corresponding to the proportion, so as to ensure the balance of substances in a reaction system. The solution in the reaction kettle is stirred and mixed, so that different substances are fully mixed and react correspondingly. The addition of the disodium ethylenediamine tetraacetate, the phosphoric acid, the polyoxyethylene ether, the propionic acid, the diethylenetriamine pentasubunit phosphoric acid and the potassium hydrogen peroxymonosulfate can be balanced and combined in the reaction system to inhibit the decomposition of the peracetic acid. Therefore, the substances can chemically react with the peroxyacetic acid or provide stability so as to delay the decomposition speed of the peroxyacetic acid, thereby maintaining the stability within a certain time, and finally the obtained unitary peroxyacetic acid disinfectant can be applied to occasions needing disinfection or sterilization.
Based on the above examples, the comparative examples of the present invention are that the preparation method is carried out according to the above preparation method, except for the amount, the other parameters are the same, and the environmental conditions are the same, so that the preparation of the disinfectant is compared:
comparative example 1, 30g of hydrogen peroxide, 68g of acetic acid, 2g of sulfuric acid, 5g of phosphoric acid, 0.5g of disodium ethylenediamine tetraacetate, 0.2g of polyoxyethylene ether, 0.5g of propionic acid, 0.2g of diethylenetriamine penta-subunit phosphoric acid and 0.5g of potassium hydrogen peroxymonosulfate.
Comparative example 2, 65.92g of acetic acid, 2.5g of sulfuric acid, 23.85g of hydrogen oxide, 5.7g of phosphoric acid, 0.5g of disodium ethylenediamine tetraacetate, 0.23g of polyoxyethylene ether, 0.5g of propionic acid, 0.25g of diethylenetriamine penta-subunit phosphoric acid, and 0.55g of potassium hydrogen peroxymonosulfate.
Comparative example 3, 30g of hydrogen peroxide, 68g of acetic acid, 2g of sulfuric acid, 5g of phosphoric acid, 0.5g of disodium ethylenediamine tetraacetate, 0.2g of polyoxyethylene ether, 0.5g of propionic acid, 0.2g of diethylenetriamine penta-subunit phosphoric acid and 0.5g of potassium hydrogen peroxymonosulfate.
Comparative example 4, hydrogen peroxide 20g, acetic acid 40g, sulfuric acid 2g, phosphoric acid 5g, disodium edetate 1g, polyoxyethylene ether 0.2g, propionic acid 0.1g, diethylenetriamine penta-subunit phosphoric acid 0.5g, potassium hydrogen peroxymonosulfate 0.5g.
And (3) placing the solution A obtained in the comparative example under a phase condition, taking 12 months as a time node, and detecting the concentration content of the monobasic peroxyacetic acid disinfectant after detecting the time node. The preservation results of the parameters in the protocol were determined as follows:
| cycle: for 12 months | Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 |
| Concentration content (mol/L) | 167 | 175 | 153 | 144 |
In the above embodiment, the best mode is selected for preparation analysis, 65.92g of acetic acid, 2.5g of sulfuric acid and 23.85g of hydrogen oxide are placed in a reaction kettle and fully stirred for more than 6 hours to obtain solution A; wherein the solution A is a monobasic peroxyacetic acid solution; checking the solution A in the reaction kettle, ensuring that the solution A is uniformly distributed and has no solid residue under visual conditions, and transferring the solution A into an activation container for activation for more than 24 hours to obtain the solution A; taking a sample in the solution A to detect the content of the peracetic acid, and determining the content of the peracetic acid in the reagent A; pouring the solution A into a reaction kettle, and adding 5.7g of phosphoric acid, 0.5g of disodium ethylenediamine tetraacetate, 0.23g of polyoxyethylene ether, 0.5g of propionic acid, 0.25g of diethylenetriamine pentasubunit phosphoric acid and 0.55g of potassium hydrogen peroxymonosulfate into the solution A; stirring and mixing to finally obtain the unitary peroxyacetic acid disinfectant; the disodium ethylenediamine tetraacetate, phosphoric acid, polyoxyethylene ether, propionic acid, diethylenetriamine penta-subunit phosphoric acid and potassium hydrogen peroxymonosulfate are used for being in balance and combination with each other in a reaction system to inhibit decomposition of peracetic acid.
Wherein, phosphoric acid can be neutralized with the peracetic acid of the solution A, and the pH value of the whole reaction system is regulated while the decomposition of the peracetic acid of the solution A is inhibited. By maintaining a suitable pH, the decomposition of peracetic acid is prevented from accelerating or generating unintended reactions.
Subsequently, disodium edetate may undergo a chelation reaction with the metal ions of solution a to form a stable complex. Avoiding that metal ions can act as catalysts for the decomposition of peracetic acid in solution A or generate free radicals. Therefore, the disodium ethylenediamine tetraacetate can stabilize metal ions, reduce the reaction rate and reduce the occurrence rate of adverse reactions of the solution A in the fusion process.
Wherein, the polyoxyethylene ether can form a micelle structure in the reaction system. The polyoxyethylene ether can adsorb to the liquid and form a stable interfacial film, thereby reducing the surface tension of the liquid. The stable interface film formed by polyoxyethylene ether can prevent the decomposition of peroxyacetic acid molecules and the volatilization of reactants, thereby improving the stability of the reaction. The propionic acid can participate in esterification, and the integral product has better stability through esterification reaction, thereby being beneficial to further slowing down the decomposition of the peroxyacetic acid.
Wherein, diethylenetriamine penta-subunit phosphoric acid and metal ions undergo a complex reaction. Through the complexation reaction, the diethylenetriamine penta-subunit phosphoric acid can reduce the catalysis of metal ions on the peroxyacetic acid, thereby inhibiting the decomposition reaction of the peroxyacetic acid.
Wherein potassium hydrogen peroxymonosulfate reacts with peroxyacetic acid to form stable sulfate ion complexation of peroxyethane. The formation of the complex can inhibit the continued decomposition of the peracetic acid, thereby improving the stability of the peracetic acid.
In operation, 65.92g of peracetic acid, 2.5g of sulfuric acid and 23.85g of hydrogen oxide are proportionally added into the reaction device, and workers need to pay attention to maintain good ventilation conditions and wear appropriate protective equipment in the process. The reaction temperature was stirred and maintained constant by the apparatus. The reaction was carried out by being initially problematic at room temperature, and then starting to heat slightly to the reaction conditions. During the reaction, stirring was continued for 6 hours to ensure that the reaction was sufficiently proceeding. During the stirring process, the change of the reaction and the fluctuation of the environmental conditions are observed to ensure the stability of the reaction. After the stirring was completed, the solution A was allowed to react and decompose further by leaving it at room temperature for 24 hours to improve the stability of the product. And (5) performing central control detection on the content of the peroxyacetic acid. The content of peracetic acid in the reaction system is determined using a suitable analytical method, such as titration or high performance liquid chromatography. Then 5.7g of phosphoric acid, 0.5g of disodium ethylenediamine tetraacetate, 0.23g of polyoxyethylene ether, 0.5g of propionic acid, 0.25g of diethylenetriamine pentasubunit phosphoric acid and 0.55g of potassium hydrogen peroxymonosulfate are weighed and added into a reaction device according to a proportion, stirring and mixing are continued, the added substances are ensured to be uniformly dispersed, and the mixture is fully reacted with the peroxyacetic acid in the reaction system. After stirring until mixing is completed, the peroxyacetic acid is more stable. During this process, it is necessary to constantly observe and adjust the reaction conditions, such as temperature and stirring speed, to ensure the progress of the reaction and the stability of the product.
If necessary, a sampling experiment may be performed during the stirring process, and the experimental results may include the measurement result of the content of peracetic acid in the reaction system, and a series of physical and chemical property test results. For example, the stability, pH, oxidation performance, etc. of peracetic acid may be measured and analyzed. The product may also be further analyzed and identified, such as by existing mass spectrometry, infrared spectrometry, and the like.
Based on the above embodiment, another embodiment of the present invention is that, in order to improve the safety and stability of the reaction in the reaction kettle and to ensure the quality stability of the obtained product, the above acetic acid is placed in the reaction kettle; sulfuric acid and hydrogen peroxide are slowly added into the container in sequence, and the temperature range of the reaction kettle is below 25 ℃.
Acetic acid is used as an initial raw material, and intense heat release of the reaction and uncontrollable risk of reaction acceleration can be prevented through mild reaction conditions, so that the safety and stability of the reaction are ensured. The temperature of the reaction kettle is controlled below 25 ℃, so that side reactions and severe reactions in the reaction process can be reduced. The lower reaction temperature is favorable for reducing byproducts and adverse reactions of the reaction and improving the stability of a reaction system. Avoiding the degradation of monoperoxyacetic acid and irreversible reaction under the high temperature condition.
During operation, firstly acetic acid is put in, and then sulfuric acid and hydrogen peroxide are slowly added so as to better control the reaction speed and temperature, thereby ensuring the stability of the reaction system. By employing a reaction temperature of 25 degrees celsius, the quality stability of the resulting product is maintained. The controllable reaction rate is beneficial to maintaining the stability and activity of the product.
Based on the above embodiment, another embodiment of the present invention is that, in order to improve the activity and the sterilization effect of the monoperoxyacetic acid, the activating temperature of the solution a in the activating container ranges from 65 to 70 ℃. The A solution is in the range of 65-70 degrees Celsius, and the reaction rate generally increases with increasing temperature. Therefore, when the solution A is activated, the temperature of the solution A can be increased by heating the solution A to the temperature of 65-70 ℃, so that the reaction rate can be increased, the reaction is promoted, and the temperature of the solution A can be increased by heating the solution A in an activation container, thereby promoting the active substance peracetic acid in the solution A to be released from the solution more quickly. Thus, the peroxyacetic acid can participate in the reaction, and the concentration and activity of the monoperoxyacetic acid are improved.
It should be noted that the rate at which the reaction reaches equilibrium increases in the range of 65-70 degrees celsius for solution a based on temperature-affected reaction equilibrium considerations. Therefore, the solution A can be promoted to react to reach an equilibrium state rapidly by controlling the activation temperature to be between 65 and 70 ℃, so that the activity and the sterilization effect of the monoperoxyacetic acid are improved.
Based on the above embodiment, another embodiment of the present invention is that the hydrogen peroxide has a purity of electronic grade and a concentration of 36%; the concentration of the acetic acid is 99.8%, and the quality grade of the acetic acid is pharmaceutical grade; the concentration of the sulfuric acid is 98%; the purity of the sulfuric acid is electronic grade; the acetic acid and hydrogen peroxide produce peroxyacetic acid, and the sulfuric acid catalyzes the peroxyacetic acid to produce monoperoxyacetic acid. The hydrogen peroxide purity is selected to be electronic grade and 36% concentration, and the core is to ensure that the hydrogen peroxide used is of high purity and the concentration can meet the reaction requirements. The hydrogen peroxide with the concentration of 36 percent can improve the preparation quality and the safety of the monoperoxyacetic acid. The purpose of the arrangement of the concentration and quality grade of the acetic acid is to ensure that the used acetic acid has higher purity and quality, avoid the influence of other impurities on the reaction and ensure the stable quality of the prepared monoperoxyacetic acid. Since sulfuric acid is used as a catalyst, the formation of peracetic acid is promoted during the reaction. The 98% strength of electronic grade sulfuric acid on the one hand improves the catalytic effect and on the other hand reduces the fluctuating influence on the quality of the monoperoxyacetic acid.
The preparation method comprises the following steps: peracetic acid can be obtained by the reaction of acetic acid and hydrogen peroxide, and the catalysis of sulfuric acid can convert peracetic acid to monoperoxyacetic acid. The purity and the quality of the reaction materials can be ensured by utilizing the purity and the concentration of hydrogen oxide, the concentration and the quality grade of acetic acid and the concentration and the purity of sulfuric acid, and the preparation of the monoperoxyacetic acid with high efficiency and high purity can be realized.
Based on the above embodiment, another embodiment of the present invention is that the quality grade of the phosphoric acid is food grade and the purity of the phosphoric acid is 99.8%, and the phosphoric acid is used to adjust the pH value of the reaction system and maintain the acid-base balance of the reaction system. In one aspect, in the process of preparing the monobasic peroxyacetic acid disinfectant, the phosphoric acid can increase or decrease the acidity of the reaction system as required to ensure that the reaction is carried out under proper acid-base conditions, and the pH value of the reaction system is regulated by the acidic substance characteristics of the peroxyphosphoric acid. On the other hand, the phosphoric acid can be used as a temporary buffering agent in the reaction system, and has good acid-base balance capability. During the reaction, some acidic or basic byproducts or intermediates may be generated, which may affect the progress of the reaction and the quality stability of the product. The phosphoric acid can absorb or release H+ ions as a buffering agent, maintain the acid-base balance of the reaction system and prevent the severe change of the pH value.
The quality grade of phosphoric acid is food grade, the purity is 99.8%, and the quality stability and the activity of the unitary peroxyacetic acid disinfectant are improved when the pH value of a reaction system is regulated and the acid-base balance is maintained, specifically: phosphoric acid is a multi-acidic organic acid containing a plurality of ionizable hydrogen ions in its molecule. If too much hydrogen ions appear in the reaction system to cause too high acidity, phosphoric acid can neutralize the acidity through the hydrogen ions in the absorption part; if the acid is too low due to insufficient hydrogen ions in the reaction system, phosphoric acid can release hydrogen ions to increase the acid. Through neutralization and adjustment of phosphoric acid, the acid-base balance of a reaction system is maintained, and the stability and activity of the unitary peroxyacetic acid disinfectant are objectively improved.
Based on the above embodiment, another embodiment of the present invention is that the quality grade of the disodium edetate is pharmaceutical grade and the purity is 99.6%, and the disodium edetate is used as a chelating agent, and the disodium edetate is matched with potassium hydrogen sulfate to promote free radical reaction and inhibit the reaction of metal ions and peracetic acid.
On the one hand, disodium edetate can form a stable chelate ring with oxygen atoms in hydrogen peroxide, thereby inhibiting or slowing down the decomposition reaction of hydrogen peroxide and maintaining the concentration of hydrogen peroxide in a certain time range. In particular, disodium ethylenediamine tetraacetate inhibits the rapid decrease of the concentration of monoperoxyacetic acid within a certain time range and can help stabilize the decomposition of hydrogen peroxide. During long-term storage, disodium edetate can react continuously with hydrogen peroxide to form an exothermic process. However, the rate of decomposition of hydrogen peroxide is inhibited by the interaction of disodium ethylenediamine tetraacetate with hydrogen peroxide, thus eventually leading to a significant reduction in the rate of hydrogen peroxide concentration. The purpose of prolonging the shelf life is achieved.
On the other hand, disodium edetate is combined with potassium hydrogen peroxymonosulfate to promote the free radical reaction. The potassium hydrogen peroxymonosulfate can release free radicals in the reaction system, and the disodium ethylenediamine tetraacetate can react with the free radicals, so that the generation of the free radicals and the reaction process are accelerated, and the formation of the monoperoxyacetic acid is further promoted.
The specific method is as follows: the potassium hydrogen peroxymonosulfate can generate free radicals in a reaction system, and the disodium ethylenediamine tetraacetate can react with the free radicals due to the existence of amino groups and carboxyl groups to capture the free radicals. Meanwhile, the structural characteristics of the disodium ethylenediamine tetraacetate enable the disodium ethylenediamine tetraacetate to transfer the captured free radicals to other substances, so that the participation of the free radicals and the occurrence of the reaction are further promoted.
The mechanism is as follows: potassium hydrogen peroxymonosulfate can be decomposed in a reaction system to generate free radicals; the compound of the disodium ethylenediamine tetraacetate with amino and carboxyl enables the disodium ethylenediamine tetraacetate to react with free radicals and capture the free radicals. Disodium edetate has a structure of polyketone acid, so that the disodium edetate can react with free radicals and transfer the free radicals to other substances, promote new free radical reaction and complete free radical transfer.
Therefore, the generation and half-life of the peroxyacetic acid can be regulated and controlled through the activation and inhibition of the free radical reaction, and the monobasic peroxyacetic acid disinfectant can be better generated through improving the efficiency of the free radical reaction, so that the disinfection effect of the monobasic peroxyacetic acid disinfectant is enhanced, and meanwhile, the stability of the monobasic peroxyacetic acid disinfectant is improved.
It is emphasized that the pharmaceutical grade of disodium edetate is an indication of its compliance with stringent pharmaceutical quality requirements, higher purity and lower impurity levels. In the experimental and industrial production processes, the use of disodium ethylenediamine tetraacetate with guaranteed pharmaceutical grade quality can provide good safety and operability, and reduce unnecessary risks. Second, disodium edetate of 99.6% purity can ensure the purity and stability of the substances added in the reaction system. Avoiding that disodium edetate may contain impurities or impure compounds that may adversely affect the reaction products. The disodium ethylenediamine tetraacetate with the purity of 99.6% can avoid the interference of impurities on the catalyst or other additives in the reaction process and reduce the reaction efficiency.
More importantly, the limitation of purity is helpful to reduce the variable and uncertainty in the experiment and improve the repeatability of the experiment and the reliability of the result. Disodium edetate of 99.6% purity can provide more stable and controlled experimental conditions and reduce the formation of unintended reactions or degradation products, thereby facilitating subsequent product development.
Based on the embodiment, according to another embodiment of the invention, the polyoxyethylene ether is polyoxyethylene ether Aeo-9, and the purity of the polyoxyethylene ether is 96.5%; the polyoxyethylene ether is used for adjusting the surface tension of the solution A, and disodium ethylenediamine tetraacetate, phosphoric acid, propionic acid, diethylenetriamine pentasubunit phosphoric acid and potassium hydrogen peroxymonosulfate are uniformly distributed in the solution A by the polyoxyethylene ether. Wherein, the polyoxyethylene ether Aeo-9 can form the action mechanism of the surfactant, and the molecular structure of the polyoxyethylene ether has the characteristics of hydrophilicity and hydrophobicity, so that a stable interface film can be formed on the surface and the interface of the liquid. In the solution A, polyoxyethylene ether molecules can be adsorbed on the surface of liquid and the interface between the solution and the gas to form a structure similar to a film. The interfacial film can reduce the surface tension of the liquid, so that substances such as disodium ethylenediamine tetraacetate, phosphoric acid, propionic acid, diethylenetriamine penta-subunit phosphoric acid, potassium hydrogen peroxymonosulfate and the like are easier to disperse in the solution, and keep uniform distribution. By reducing the surface tension, polyoxyethylene ethers help reduce interactions between various substances in solution and gas or undissolved substances, thereby promoting uniform dispersion of the substances.
The uniform dispersion of disodium ethylenediamine tetraacetate, phosphoric acid, propionic acid, diethylenetriamine penta-subunit phosphoric acid and potassium peroxymonosulfate is aided by the polyoxyethylene ether by adjusting the surface tension of the solution. Thus, the efficiency and controllability of the reaction can be improved, which is beneficial to reducing the events of uneven distribution or overhigh local concentration.
Based on the above embodiment, another embodiment of the present invention is that the quality grade of the diethylenetriamine penta-subunit phosphoric acid is pharmaceutical grade, the purity of the diethylenetriamine penta-subunit phosphoric acid is 98%, the diethylenetriamine penta-subunit phosphoric acid is used for binding with the active site of peracetic acid, and the diethylenetriamine penta-subunit phosphoric acid is matched with potassium hydrogen peroxymonosulfate to inhibit the concentration of monoperoxyacetic acid from rapidly decreasing.
The solution A contains a certain amount of hydrogen peroxide, so that the solution A has unstable property. During long-term storage, the hydrogen peroxide in solution a can spontaneously decompose into water and oxygen and form an exothermic process. As the exotherm time increases, the rate of decomposition may also increase, resulting in a more rapid rate of hydrogen peroxide decomposition and ultimately a significant decrease in the concentration of hydrogen peroxide in solution a. The principle that diethylenetriamine penta-subunit phosphoric acid is used as a chelating agent and can inhibit the rapid decrease of the concentration of monoperoxyacetic acid is mainly that the diethylenetriamine penta-subunit phosphoric acid and metal ions in monoperoxyacetic acid form a stable complex.
The specific method is as follows: metal ions may be present in the monoperoxyacetic acid, and the presence of the metal ions may accelerate the decomposition reaction of the monoperoxyacetic acid, while the diethylenetriamine penta-subunit phosphoric acid has a phosphate group with a higher affinity, and the phosphate group of the diethylenetriamine penta-subunit phosphoric acid may form a complex with the metal ions. By complexing the diethylenetriamine pentasubunit phosphoric acid with metal ions, the diethylenetriamine pentasubunit phosphoric acid can inhibit the catalysis of the metal ions on the monoperoxyacetic acid, thereby slowing down or inhibiting the decomposition rate of the monoperoxyacetic acid.
More importantly, the complex formed between the phosphate radical of the diethylenetriamine penta-subunit phosphoric acid and the metal ion can be matched with potassium hydrogen peroxymonosulfate to further prevent the decomposition reaction of the monoperoxyacetic acid catalyzed by the metal ion, so that the diethylenetriamine penta-subunit phosphoric acid is matched with the potassium hydrogen peroxymonosulfate to have a repression effect in the solution A. Thereby preventing the unary peroxyacetic acid molecule of the solution A from generating adverse reaction, reducing the generation of free radicals and limiting the rapid decrease of the concentration of the unary peroxyacetic acid.
Based on the above embodiment, another embodiment of the present invention is that the quality grade of the potassium hydrogen peroxymonosulfate is pharmaceutical grade, and the purity of the potassium hydrogen peroxymonosulfate is 99.5%; the potassium hydrogen peroxymonosulfate is used for reacting residual hydrogen peroxide with acetic acid and sulfuric acid as a stabilizer and triggering reaction free radicals in organic molecules in disodium ethylenediamine tetraacetate, phosphoric acid, polyoxyethylene ether, propionic acid and diethylenetriamine penta-subunit phosphoric acid and promoting the formation of polymer chains.
Wherein, potassium hydrogen peroxymonosulfate is used for reacting residual hydrogen peroxide, acetic acid and sulfuric acid as a stabilizer and triggering reactive free radicals in organic molecules in disodium ethylenediamine tetraacetic acid, phosphoric acid, polyoxyethylene ether, propionic acid and diethylenetriamine penta-subunit phosphoric acid to promote the formation of polymer chains.
During operation, the potassium hydrogen peroxymonosulfate is used as a stabilizer to react residual reactants such as hydrogen peroxide, acetic acid, sulfuric acid and the like, and the concentration of the residual reactants is reduced, so that a reaction system is stabilized, and side reactions are prevented. This helps to improve the quality stability of the monoperoxyacetic acid disinfectant. Potassium hydrogen peroxymonosulfate then also generates free radicals in the reaction system. The free radical can react with organic molecules such as disodium ethylenediamine tetraacetate, phosphoric acid, polyoxyethylene ether, propionic acid, diethylenetriamine penta-subunit phosphoric acid and the like, so that the free radical chain reaction is initiated. Thereby forming free radical chain reaction, further promoting organic molecules to form polymer chains, and improving the stability and activity of the monoperoxyacetic acid disinfectant.
The free radical generated by potassium hydrogen peroxymonosulfate has high reactivity, can react with organic molecules such as disodium ethylenediamine tetraacetate, phosphoric acid, polyoxyethylene ether, propionic acid, diethylenetriamine penta-subunit phosphoric acid and the like to trigger free radical reaction between the two to form a stable free radical intermediate, and the free radical intermediate can react with disodium ethylenediamine tetraacetate, phosphoric acid, polyoxyethylene ether, propionic acid and diethylenetriamine penta-subunit phosphoric acid molecules to continuously form the free radical intermediate containing more polymerization units, and the free radicals are mutually consumed by collision of the plurality of free radical intermediates, so that the free radical reaction is ended to form a stable polymer chain.
For example, the present application can be applied to various situations, and in one embodiment of the present invention, on the premise that the monoperoxyacetic acid solution has higher stability, in order to prolong the shelf life of the monoperoxyacetic acid solution, biodegradable materials, such as silica gel, microcrystalline cellulose, and the like, may be selected as a matrix, and the monoperoxyacetic acid is mixed into the matrix. The monoperoxyacetic acid may be uniformly distributed in the matrix by mixing, dissolving or melting. The mixture is then cooled and solidified, sheared into particles of appropriate size, and optionally coated with a coating. The wrapper can be the existing polyvinyl alcohol, chitosan and stearic acid, on the basis of the above, the release time of the monoperoxyacetic acid is controlled, the preservation time of the monoperoxyacetic acid is effectively prolonged through the wrapper, and when the wrapper is required to release the monoperoxyacetic acid, the wrapper is added into an aqueous solution, so that the wrapper can be quickly dissolved, and the monoperoxyacetic acid is released. Since water is harmless to monoperoxyacetic acid, it does not destroy its oxidizing and disinfecting properties, and at the same time, it can dissolve most of the matrix and the coating, thereby rapidly releasing monoperoxyacetic acid to obtain monoperoxyacetic acid solution.
In order to ensure that the concentration of the monoperoxyacetic acid after the release of the wrapper corresponds to the concentration of the monoperoxyacetic acid solution, the total amount of the monoperoxyacetic acid is determined by setting the total weight of the particles, namely, the required amount of the monoperoxyacetic acid is reasonably calculated according to the concentration of the solution and the total weight of the particles, the required monoperoxyacetic acid is dissolved in a matrix with enough amount to be uniformly distributed, and then the monoperoxyacetic acid is solidified, sheared and wrapped according to the previous steps; some particle samples are collected and then analyzed for the level of monoperoxyacetic acid to determine if the desired concentration is achieved, if the monoperoxyacetic acid concentration is too high, it may be desirable to increase the amount of matrix or decrease the monoperoxyacetic acid ratio; if the concentration is insufficient, it may be necessary to increase the amount of monoperoxyacetic acid so that the monoperoxyacetic acid concentration in the particles corresponds to the concentration in the original solution, thereby ensuring that the desired effect can be obtained in the case where these particles are used.
Reference throughout this specification to "one embodiment," "another embodiment," "an embodiment," "a preferred embodiment," etc., means that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one embodiment described in general terms in the present application. The appearances of the phrase in various places in the specification are not necessarily all referring to the same embodiment. Further, when a particular feature, structure, or characteristic is described in connection with any embodiment, it is intended that such feature, structure, or characteristic be implemented within the scope of the invention.
Although the invention has been described herein with reference to a number of illustrative embodiments thereof, it should be understood that numerous other modifications and embodiments can be devised by those skilled in the art that will fall within the scope and spirit of the principles of this disclosure. More specifically, various variations and modifications may be made to the component parts and/or arrangements of the subject combination arrangement within the scope of the disclosure and claims of this application. In addition to variations and modifications in the component parts and/or arrangements, other uses will be apparent to those skilled in the art.
Claims (10)
1. A method of preparing a peroxyacetic acid based formulation for adapting a peroxyacetic acid product comprising: taking, by weight, 20-30 parts of hydrogen peroxide, 60-70 parts of acetic acid, 2-4 parts of sulfuric acid, 5-6 parts of phosphoric acid, 0.5-1 part of disodium ethylenediamine tetraacetate, 0.2-0.3 part of polyoxyethylene ether, 0.5-1 part of propionic acid, 0.25-0.5 part of diethylenetriamine pentasubunit phosphoric acid and 0.5-1 part of potassium hydrogen peroxymonosulfate for later use;
placing the acetic acid, sulfuric acid and hydrogen peroxide into a reaction kettle, and fully stirring for more than 6 hours to obtain a solution A; the solution A is a monobasic peroxyacetic acid solution; checking the solution A in the reaction kettle, ensuring that the solution A is uniformly distributed and has no solid residue under visual conditions, and transferring the solution A into an activation container for activation for more than 24 hours to obtain the solution A; taking a sample in the solution A to detect the content of the peracetic acid, and determining the content of the peracetic acid in the reagent A; pouring the solution A into a reaction kettle, and adding phosphoric acid, disodium ethylenediamine tetraacetate, polyoxyethylene ether, propionic acid, diethylenetriamine penta-subunit phosphoric acid and potassium hydrogen peroxymonosulfate into the solution A; stirring and mixing to obtain a unitary peracetic acid disinfectant; the disodium ethylenediamine tetraacetate, phosphoric acid, polyoxyethylene ether, propionic acid, diethylenetriamine penta-subunit phosphoric acid and potassium hydrogen peroxymonosulfate are used for being in balance combination with each other in a reaction system to inhibit decomposition of peracetic acid.
2. The method for preparing the peroxyacetic acid based on the stability according to claim 1 is characterized in that: the acetic acid is placed in a reaction kettle; sulfuric acid and hydrogen peroxide are slowly added into the container in sequence, and the temperature range of the reaction kettle is below 25 ℃.
3. The method for preparing the peroxyacetic acid based on the stability according to claim 1 is characterized in that: the activation temperature of the solution A in the activation container ranges from 65 ℃ to 70 ℃.
4. The method for preparing the peroxyacetic acid based on the stability according to claim 1 is characterized in that: the hydrogen peroxide has an electron-grade purity and a concentration of 36%; the concentration of the acetic acid is 99.8%, and the quality grade of the acetic acid is pharmaceutical grade; the concentration of sulfuric acid is 98%; the purity of the sulfuric acid is electronic grade; the acetic acid and hydrogen peroxide produce peroxyacetic acid, and the sulfuric acid catalyzes the peroxyacetic acid to produce monoperoxyacetic acid.
5. The method for preparing the peroxyacetic acid based on the stability according to claim 1 is characterized in that: the quality grade of the phosphoric acid is food grade, the purity of the phosphoric acid is 99.8%, and the phosphoric acid is used for adjusting the pH value of the reaction system and maintaining the acid-base balance of the reaction system.
6. The method for preparing the peroxyacetic acid based on the stability according to claim 1 is characterized in that: the quality grade of the disodium ethylenediamine tetraacetate is pharmaceutical grade, the purity is 99.6%, and the disodium ethylenediamine tetraacetate is used as a chelating agent, and the disodium ethylenediamine tetraacetate is matched with potassium hydrogen monosulfate to promote free radical reaction and inhibit the reaction of metal ions and peroxyacetic acid.
7. The method for preparing the peroxyacetic acid based on the stability according to claim 1 is characterized in that: the polyoxyethylene ether is polyoxyethylene ether Aeo-9, and the purity of the polyoxyethylene ether is 96.5%; the polyoxyethylene ether is used for adjusting the surface tension of the solution A, and the polyoxyethylene ether enables disodium ethylenediamine tetraacetate, phosphoric acid, propionic acid, diethylenetriamine penta-subunit phosphoric acid and potassium hydrogen peroxymonosulfate to be evenly distributed in the solution A.
8. The method for preparing the peroxyacetic acid based on the stability according to claim 1 is characterized in that: the quality grade of the diethylenetriamine pentasubunit phosphoric acid is medicinal grade, the purity of the diethylenetriamine pentasubunit phosphoric acid is 98%, the diethylenetriamine pentasubunit phosphoric acid is used for combining with the active site of the peroxyacetic acid, and the diethylenetriamine pentasubunit phosphoric acid is matched with potassium hydrogen peroxymonosulfate to inhibit the rapid reduction of the concentration of the monoperoxyacetic acid.
9. The method for preparing the peroxyacetic acid based on the stability according to claim 1 is characterized in that: the quality grade of the potassium hydrogen peroxymonosulfate is medicinal grade, and the purity of the potassium hydrogen peroxymonosulfate is 99.5%; the potassium hydrogen peroxymonosulfate is used for reacting residual hydrogen peroxide with acetic acid and sulfuric acid as a stabilizer and triggering reaction free radicals in organic molecules in disodium ethylenediamine tetraacetate, phosphoric acid, polyoxyethylene ether, propionic acid and diethylenetriamine penta-subunit phosphoric acid and promoting the formation of polymer chains.
10. The method for preparing the peroxyacetic acid based on the stability according to claim 1 is characterized in that: the purity of the propionic acid is 99.6%, the propionic acid is mixed with phosphoric acid in the mixing process to maintain acid-base balance, and the propionic acid inhibits the growth of microorganisms in the unitary peroxyacetic acid disinfectant.
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| CN202311741371.0A CN117736129A (en) | 2023-12-18 | 2023-12-18 | Preparation method based on stability of peroxyacetic acid |
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