CN1029401C - Preparation method for solid-state amyldiacid peroxide - Google Patents
Preparation method for solid-state amyldiacid peroxide Download PDFInfo
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- CN1029401C CN1029401C CN 92106152 CN92106152A CN1029401C CN 1029401 C CN1029401 C CN 1029401C CN 92106152 CN92106152 CN 92106152 CN 92106152 A CN92106152 A CN 92106152A CN 1029401 C CN1029401 C CN 1029401C
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- perglutaric acid
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Abstract
The present invention relates to a preparation method for solid perglutaric acid. Hydrogen peroxide, glutaric anhydride and water are used as raw materials and stirred for a certain period of time at certain temperature, and the solid perglutaric acid is obtained through sucking filtration, washing and drying. The content of the solid perglutaric acid can reach 98%, the solid perglutaric acid has high stability, low toxicity and no irritative odor, a diluted water solution of the solid perglutaric acid has good killing effect on various bacteria, bacterial spores, viruses and fungi, and the disinfecting liquid can be repeatedly used. The preparation method for solid perglutaric acid has the advantages of simple technology, mild reaction conditions, high active component content and low construction investment; thus, the method is suitable for industrial production.
Description
The present invention relates to a kind of method for preparing sterilizing agent, the preparation method of the solid-state amyldiacid peroxide that particularly a kind of high-content is stable.
As everyone knows, peroxy acid is good oxygenant and sterilizing agent.Lower peroxy acid such as Peracetic Acid can form comparatively stable solution with certain content, but higher volatility and stronger pungent taste are arranged, and this makes its management and use and has all run into difficulty.German patent DE 2654164(the coexist U.S., Japanese publication patent) a kind of method of utilizing Pyroglutaric acid and the synthetic state amyldiacid peroxide liquid dosage form of hydrogen peroxide disclosed, its product content reaches as high as 60%(and calculates with single state amyldiacid peroxide), overcome the shortcoming that Peracetic Acid exists, this sterilizing agent germicidal action is strong, more stable, toxicity is low, non-stimulated flavor, basic non-volatility is a kind of comparatively ideal sterilizing agent.But this sterilizing agent state amyldiacid peroxide content not high (about 50%), and be the aqueous solution, stability is not ideal enough, is not easy to transportation and preservation, influences the widespread use of this sterilizing agent.
The preparation method who the purpose of this invention is to provide a kind of solid-state amyldiacid peroxide, its technology is simple, the reaction conditions gentleness, operation easily, final product active constituent content height, good stability is convenient to transportation and preservation.
The object of the present invention is achieved like this: this method adopts the weight percent of raw material to be respectively hydrogen peroxide 10-50, Pyroglutaric acid 22-48, water 1-66, take by weighing according to quantity and put into reactor and stir, temperature is controlled at 5-30 ℃, and pH value is at 1-12, and the reaction times was at 5-120 minute, carry out conventional suction filtration, washing, drying after the reaction, promptly get the solid-state amyldiacid peroxide finished product.
Because it is promotor that the present invention adopts water, make the hydrogen peroxide oxidation Pyroglutaric acid, so obtain solid-state amyldiacid peroxide unexpectedly, its content (weight percent) is about the 61-98% state amyldiacid peroxide, the 1-50% pentanedioic acid, water 1-10% compares (being water-soluble state amyldiacid peroxide concentrated solution) with prior art, this method need not be added stablizer can obtain the highly stable solid dosage product of performance, this product state amyldiacid peroxide content (calculating with two state amyldiacid peroxides) 61-98%.Suitably control reaction temperature, pH value, time, can improve the yield of product and the content of state amyldiacid peroxide.Therefore, this method compared with prior art, not only technology is simple, raw material is easy to get, low cost of manufacture, and final product active constituent content height, good stability is convenient to transportation and is preserved, and helps wide popularization and application.
The chemical formula C10H14O8 of the solid-state amyldiacid peroxide that makes with this method, molecular weight 262, structural formula HOOC(CH2) 3COOOCO(CH2) 3COOH, outward appearance is white bulky powder, dissolving is very fast in 50 ℃ of warm water, dissolves in the organic solvent such as ethanol basic non-volatility, non-stimulated flavor.Its good stability was at room temperature placed 2.5 years, and state amyldiacid peroxide content rate of descent is about 13-15%.Toxicity test, its mouse oral LD50 are 2483 milligrams/kilogram, are low toxicity material, no cumulative toxicity, no mutagenesis.2% concentration has slight stimulation to the skin nonirritant to mucous membrane.Corrosion test shows that textiles is had fading function, but its quality is not had obvious influence.Chromium plating, nickel plating metal, stainless steel there is not corrosion phenomenon.
Sterilization effect, be the action time that bacterial inactivation rate is reached the state amyldiacid peroxide different concns aqueous solution more than 99.9%: 0.05% concentration was to intestinal bacteria, Staphylococcus albus 2 minutes; To bacterium anthracoides brood cell 1.0% concentration 30 minutes, 0.5% concentration 90 minutes; To Candida albicans 1.0% concentration 120 minutes.Under 20% calf serum protection, to intestinal bacteria and Staphylococcus albus 0.05% concentration 5 minutes; To bacterium anthracoides brood cell 1.0% concentration 30 minutes.1.0% concentration placed for three weeks 25 ℃ of conditions, its density loss to 0.87%, and brood cell's effect is constant substantially extremely.To the HBsAg(hepatitis B surface antigen(HBsAg)) deactivation, 1.0% concentration 5 minutes; Deactivation HBsAg in serum, 1.0% concentration 30 minutes.1.0% concentration is used for nonmetal instrument soaking sterilization can be used 20 days continuously, and HBsAg is still had deactivation.0.5% concentration is used for the tableware soaking disinfection, can use continuously 30 days, still can kill intestinal bacteria and phage F2 thereof.
The minimum inhibitory concentration of state amyldiacid peroxide is: intestinal bacteria 0.031%; Staphylococcus albus 0.016%; Bacterium anthracoides brood cell 0.031%; Candida albicans 0.125%.
The state amyldiacid peroxide mother liquor also has sterilization effect preferably, also can be used for various sterilisation purposes.
Entire reaction course is simple, and no waste produces, and free from environmental pollution, state amyldiacid peroxide solid dosage and mother liquor all can utilize.Raw materials used being easy to get, low cost of manufacture.Wherein raw materials used is that 70-98%, concentration of hydrogen peroxide are that distilled water is advisable for industrial hydrogen peroxide, the water greater than 30% with Pyroglutaric acid content.Its reaction conditions is preferentially selected temperature 8-25 ℃ for use, pH value 2-5, time 40-100 minute.
The invention will be further described below in conjunction with embodiment.
Embodiment 1
80% Pyroglutaric acid, 57 grams, 3,0%H,2O2 50 grams, H2O 100 grams, 98,%H2,SO4 5 grams.Above-mentioned substance is put in the reactor, started stirrer, carry out vigorous stirring, temperature is controlled at 8-25 ℃, surveys PH less than 2.React comparatively slow, whole synthesising reacting time is 120 minutes.Carry out conventional suction filtration, washing, drying then.Get state amyldiacid peroxide solid 36.7 grams, yield is 64.4%.Survey state amyldiacid peroxide content 81.2% with iodimetry,iodometry.
Embodiment 2
80% Pyroglutaric acid, 57 grams, 3,0%H,2O2 50 grams, H2O 100 grams, sodium acetate 2 grams.Above-mentioned substance is put in the reactor, started stirrer, carry out vigorous stirring, temperature is controlled at 8-25 ℃, surveys PH greater than 12.Building-up reactions is very fast, and whole synthesising reacting time is 5-15 minute.Carry out suction filtration, washing, drying then.Get state amyldiacid peroxide solid 30.7 grams, yield is 53.8%.State amyldiacid peroxide content 68.3%.
Embodiment 3
90% Pyroglutaric acid, 57 grams, 3,0%H,2O2 30 grams, H2O 165 grams.Above-mentioned substance is put in the reactor, started stirrer, carry out vigorous stirring, PH is controlled at 2-5, temperature 8-25 ℃, in 80 minutes reaction times, carries out suction filtration, washing, drying then.Get state amyldiacid peroxide solid 35 grams, yield is 61.4%.State amyldiacid peroxide content 64.4%.
Embodiment 4
95-98% Pyroglutaric acid 114 grams, 3,0%H,2O2 89 grams, H2O 125 grams.Above-mentioned substance is put in the reactor.Start stirrer and stir, measure starting temperature and pH value, and perform record.Temperature is controlled between 8-25 ℃, and PH is controlled between the 2-5, and the reaction times only is 80 minutes, carries out suction filtration, washing, drying then.Get state amyldiacid peroxide solids component receipts amount 82 grams, yield 71.9%, state amyldiacid peroxide content 98.2%.
To sum up example explanation, synthesising reacting time is long under acidic medium, its yield and content all not high (example 1); Fast in the following reaction times of alkaline medium, its yield and content lower (example 2); Under the situation that does not add any medium, change formula rate, reduce the H2O2 consumption, strengthen the H2O consumption, synthetic its yield and content lower (example 3) as a result; Under the situation that does not add any medium, formula rate is suitable, and temperature is controlled between 8-25 ℃, PH is controlled between the 2-5, reaction times moderate (80 minutes), its yield higher (71.9%), state amyldiacid peroxide content is higher 98.2%, is more satisfactory synthesizing formula and condition (example 4).
Claims (3)
1, a kind of preparation method of solid-state amyldiacid peroxide, it is characterized in that adopting the weight percent of raw material to be respectively concentration greater than 30% hydrogen peroxide 10-50%, Pyroglutaric acid 22-48%, the water 1-66% that concentration is 70-98%, take by weighing according to quantity and put into reactor and stir, temperature is controlled at 5-30 ℃, pH value is at 2-5, reaction times was carried out conventional suction filtration, washing, drying at 5-120 minute after the reaction, promptly get the solid-state amyldiacid peroxide goods.
2, method according to claim 1 is characterized in that raw materials used water is distilled water.
3, method according to claim 1 is characterized in that reaction conditions selects temperature 8-25 ℃, time 40-100 minute for use.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 92106152 CN1029401C (en) | 1992-05-08 | 1992-05-08 | Preparation method for solid-state amyldiacid peroxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 92106152 CN1029401C (en) | 1992-05-08 | 1992-05-08 | Preparation method for solid-state amyldiacid peroxide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1067882A CN1067882A (en) | 1993-01-13 |
| CN1029401C true CN1029401C (en) | 1995-08-02 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN 92106152 Expired - Fee Related CN1029401C (en) | 1992-05-08 | 1992-05-08 | Preparation method for solid-state amyldiacid peroxide |
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| CN (1) | CN1029401C (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107973734A (en) * | 2017-11-30 | 2018-05-01 | 江西理文化工有限公司 | A kind of preparation method of disuccinic acid peroxide |
| CN111892524A (en) * | 2020-09-09 | 2020-11-06 | 感控卫士(山东)医疗科技有限公司 | Preparation method of disinfectant peroxyglutaric acid |
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1992
- 1992-05-08 CN CN 92106152 patent/CN1029401C/en not_active Expired - Fee Related
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| CN1067882A (en) | 1993-01-13 |
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| C15 | Extension of patent right duration from 15 to 20 years for appl. with date before 31.12.1992 and still valid on 11.12.2001 (patent law change 1993) | ||
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| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |