CN113854313B - Potassium monopersulfate low-temperature disinfectant and preparation method thereof - Google Patents
Potassium monopersulfate low-temperature disinfectant and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of low-temperature disinfectants, and discloses a potassium monopersulfate low-temperature disinfectant and a preparation method thereof. The low-temperature disinfectant comprises a liquid single-component system or a two-component system consisting of powder and solution; the components of the potassium monopersulfate water-soluble emulsion comprise potassium monopersulfate composite salt, a surfactant, organic acid, inorganic buffer salt, calcium chloride, ethanol, ethylene glycol and water. The low-temperature disinfectant can be kept in a liquid state at the temperature of minus 40 ℃, is not solidified or frozen, can be still sterilized by spraying, and can still keep the sterilization effect. The sterilization test is respectively carried out at the normal temperature of 25 ℃, 18 ℃ and 40 ℃, and the average killing log value of bacteria and viruses is more than 4.00 after 10min of action time. The disinfectant has good disinfection capability under both normal temperature and low temperature conditions.
Description
Technical Field
The invention belongs to the technical field of low-temperature disinfectants, and particularly relates to a potassium monopersulfate low-temperature disinfectant and a preparation method thereof.
Background
In recent years, with the spread of infectious viruses such as new coronavirus, the safety problem of cold chain foods has attracted much attention. The disinfection of articles in the cold chain state is much more difficult than for articles at normal temperature, and disinfection at low temperature requires a safe and effective disinfectant and a reliable disinfection method.
The conventional disinfectant takes pure water as a solvent, under the condition of low-temperature freezing, the liquid disinfectant is condensed into a solid state, the disinfection effect is difficult to play, and even the disinfection products are completely ineffective. This becomes the technical difficulty that restricts virus and bacteria disinfection under cold chain condition and winter low temperature environment at present. Therefore, the development of high-efficiency, safe and low-temperature disinfection technology is also an urgent technical problem to be solved.
Low-temperature disinfectants prepared by adding anti-freeze solvents have been disclosed in the related art. For example, the Chinese disease control center starts a new low-temperature disinfection technology research from 6 months and 17 days in 2020, and develops two chlorine-containing low-temperature disinfectants. Wherein the disinfectant at-18 deg.C mainly comprises sodium dichloroisocyanurate, calcium chloride and ethanol. When the disinfectant is used on site, the effective chlorine concentration in the disinfectant at the low temperature of-18 ℃ is 0.3 percent (3000mg/L), the content of anhydrous calcium chloride is 25 percent, and the content of ethanol is 9.5 percent. The dosage form is binary package, powder and liquid. The agent A is sodium dichloroisocyanurate powder, and the agent B is a mixed solution of calcium chloride and ethanol. The low-temperature disinfectant at-40 deg.C mainly comprises sodium dichloroisocyanurate, calcium chloride, ethanol, ethylene glycol and benzalkonium chloride. When the disinfectant is used on site, the concentration of effective chlorine in the disinfectant at the low temperature of-40 ℃ is 0.5 percent (5000mg/L), the content of anhydrous calcium chloride is 30 percent, ethanol is 9.5 percent, glycol is 9.9 percent, and benzalkonium chloride is 0.09 percent. The dosage form is binary package, powder and liquid. The agent A is sodium dichloroisocyanurate powder; the agent B is a mixed solution of calcium chloride, ethanol, glycol and benzalkonium chloride.
The key technology of the low-temperature disinfectant needs to select a proper anti-freezing solvent or an auxiliary agent, and also needs to consider the compatibility and stability of effective disinfection components and the easiness in spraying of the whole formula. Compatibility is the compatibility of the disinfecting active ingredient with the solvent system, and the proper solvent system should not adversely affect the disinfecting efficacy of the disinfecting active ingredient. Stability refers to the storage stability of the disinfecting active ingredient and the stability of the disinfecting activity in the system formulation. The existing low-temperature disinfectant is generally in binary package and is divided into powder and liquid, and the reason is that the corresponding disinfection activity cannot last for a long time after the low-temperature disinfectant is prepared into a solution, and the low-temperature disinfectant needs to be prepared for use. However, the problem with binary packaging is that powders tend to cake during storage and still suffer some loss of activity. The easy spraying property means that the whole formula can be kept in a low-viscosity liquid state, can not be solidified and frozen at low temperature (such as minus 40 ℃), and can be sprayed for disinfection, so that the effect of quick disinfection at low temperature is achieved.
The patent CN113439758A discloses a low-temperature potassium monopersulfate disinfectant formula, which comprises an agent A and an agent B, wherein the agent A is powder, the agent A contains 65-95% of potassium monopersulfate composite salt, 1-25% of sodium hexametaphosphate or sodium tripolyphosphate, 0-5% of polyvinylpyrrolidone, 0-5% of sodium dodecyl benzene sulfonate and 0.5-25% of sulfamic acid in percentage by mass. The agent B exists in the form of powder or liquid, chemical components of the agent B are sodium chloride, calcium chloride or a mixture of the sodium chloride and the calcium chloride when the powder exists, the content of the sodium chloride is 0.5-99%, the content of the calcium chloride is 0.1-99%, the content of magnesium chloride is not higher than 5%, and when the agent B exists in the form of liquid, the content of the sodium chloride is 0.5-23.5%, the content of the calcium chloride is 0.1-35%, the content of the magnesium chloride is not higher than 2%, and the total content is 15-35%. The patent is suitable for disinfection in different low-temperature environments by adding a large amount of greening sodium, calcium chloride and the like into an aqueous solution. In addition, the common potassium monopersulfate composite salt is adopted, and the storage anti-caking performance and the activity stability of the potassium monopersulfate composite salt are required to be further improved.
Disclosure of Invention
Aiming at the defects and shortcomings of the prior art, the invention aims to provide the oxone low-temperature disinfectant. The low-temperature disinfectant can be kept in a liquid state at the temperature of minus 40 ℃, is not solidified or frozen, can be still sterilized by spraying, and can still keep the sterilization effect. The sterilization test is respectively carried out at the normal temperature of 25 ℃, 18 ℃ and 40 ℃, and the average killing log value of bacteria and viruses is more than 4.00 after 10min of action time. The disinfectant has good disinfection capability under both normal temperature and low temperature conditions. Meets the requirements of disinfection technical specification (2002 edition).
The invention also aims to provide a preparation method of the potassium monopersulfate low-temperature disinfectant.
The purpose of the invention is realized by the following technical scheme:
a low-temperature potassium monopersulfate disinfectant comprises a liquid single-component system or a two-component system consisting of powder and solution; the liquid single-component system comprises potassium monopersulfate complex salt, a surfactant, organic acid, inorganic buffer salt, calcium chloride, ethanol, ethylene glycol and water; the powder in the two-component system comprises potassium monopersulfate composite salt, and the solution comprises a surfactant, organic acid, inorganic buffer salt, calcium chloride, ethanol, ethylene glycol and water.
Further, the low-temperature disinfectant comprises the following components in percentage by mass:
further, the surfactant is at least one of sodium alkyl benzene sulfonate and sodium alkyl sulfonate; the organic acid is at least one of malic acid, citric acid and tartaric acid; the inorganic buffer salt is sodium polyphosphate.
Further, the potassium monopersulfate composite salt is an anti-caking high-stability potassium monopersulfate composite salt and is prepared by the following method:
(1) adding hydrogen peroxide and a stabilizer into a reactor, controlling the temperature to be 0-5 ℃, dropwise adding fuming sulfuric acid under the stirring condition, and controlling the temperature to be below 15 ℃ for heat preservation reaction to obtain peroxidation reaction liquid;
(2) dropwise adding a potassium carbonate or potassium hydroxide solution into the peroxidation reaction liquid in the step (1) to carry out neutralization reaction to obtain a neutralization liquid;
(3) and (3) adding liquid sodium silicate into the neutralized liquid obtained in the step (2), stirring and dissolving uniformly, concentrating in vacuum, cooling and crystallizing, and centrifugally drying to obtain the anti-caking high-stability potassium monopersulfate composite salt.
Further, the stabilizer in the step (1) is trisodium phosphate or sodium polyphosphate; the addition amount of the stabilizer is 0.5 to 2 percent of the mass of the hydrogen peroxide.
Further, the hydrogen peroxide and the oleum in the step (1) are diluted to the mass concentration of 20-50% before reaction.
Further, the molar ratio of the hydrogen peroxide to the fuming sulfuric acid in the step (1) is (1-3) to 1.
Furthermore, in the step (2), the molar ratio of the addition amount of the potassium carbonate or the potassium hydroxide to the oleum (calculated as sulfate radicals) is (4.8-5.2): 4, wherein the molar amount of the potassium carbonate or the potassium hydroxide is calculated as the molar amount of potassium.
Further, the adding amount of the liquid sodium silicate in the step (3) is 0.2-4% of the mass of the neutralizing liquid.
Further, the vacuum concentration in the step (3) is to perform vacuum concentration to saturation at the temperature of 45-55 ℃; the cooling crystallization refers to standing crystallization after cooling to-4 ℃.
The preparation method of the potassium monopersulfate low-temperature disinfectant comprises the following preparation steps:
adding a surfactant, an organic acid, an inorganic buffer salt, calcium chloride, ethanol and glycol into water, stirring and dissolving uniformly, then adding a potassium monopersulfate composite salt, stirring and dissolving uniformly to obtain a liquid single-component system low-temperature disinfectant; or adding the surfactant, the organic acid, the inorganic buffer salt, the calcium chloride, the ethanol and the glycol into water, stirring and dissolving uniformly to obtain a solution, and respectively packaging the solution and the potassium monopersulfate composite salt powder to obtain the double-component system low-temperature disinfectant.
Compared with the prior art, the invention has the beneficial effects that:
(1) the low-temperature disinfectant can be kept in a liquid state at the temperature of minus 40 ℃, is not solidified or frozen, can be still sterilized by spraying, and can still keep the sterilization effect. The sterilization and disinfection tests are respectively carried out at the normal temperature of 25 ℃, 18 ℃ and 40 ℃, and the average killing log values of bacteria and viruses are all greater than 4.00 after 10min of action time. The disinfectant has good disinfection capability under both normal temperature and low temperature conditions. Meets the requirements of disinfection technical specification (2002 edition).
(2) The invention adopts the potassium monopersulfate composite salt as the active component of the low-temperature disinfectant, and has the advantages of good disinfection effect, safety and environmental protection.
(3) The anti-caking high-stability potassium monopersulfate composite salt prepared by a specific method is used as an active ingredient of a low-temperature disinfectant. When the nano-silver-containing nano-silver particles are used as a liquid single-component system, the stability of the disinfection activity of the nano-silver-containing nano-silver particles is good, and the retention rate of active oxygen can still be maintained above 80% after the nano-silver-containing nano-silver particles are stored at normal temperature in a sealed manner for 6 months. When the potassium monopersulfate composite salt powder is applied as a two-component system consisting of powder and solution, the active component potassium monopersulfate composite salt powder has good anti-caking performance and high storage stability. Compared with the prior low-temperature disinfectant, the flexibility of the using mode is greatly improved when the low-temperature disinfectant is only used in the existing preparation.
(4) In the preparation process of the anti-caking high-stability potassium monopersulfate composite salt, a certain amount of liquid sodium silicate is added in the concentration and crystallization process of the potassium monopersulfate composite salt, so that the crystallization and precipitation of the potassium monopersulfate composite salt in a solution are facilitated, and the utilization rate of raw materials and the yield of products are improved. And the anti-caking performance and stability of the potassium monopersulfate composite salt can be obviously improved.
(5) The invention adopts inorganic buffer salt to replace the prior sodium chloride or calcium chloride which is used in large quantity, and has the advantages of low irritation and wide application range.
(6) The low-temperature disinfectant disclosed by the invention is beneficial to improving the spraying easiness and stability of the disinfectant by adding a certain amount of surfactant and organic acid, and achieves the effect of quickly disinfecting under a low-temperature condition.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto.
Example 1
The potassium monopersulfate low-temperature disinfectant comprises the following components in percentage by mass:
the low-temperature potassium monopersulfate disinfectant is prepared by the following method: adding sodium dodecyl benzene sulfonate, citric acid, sodium polyphosphate, calcium chloride, ethanol and ethylene glycol into water, stirring and dissolving uniformly, then adding potassium monopersulfate composite salt, stirring and dissolving uniformly to obtain a liquid single-component system low-temperature disinfectant; or adding the surfactant, the organic acid, the inorganic buffer salt, the calcium chloride, the ethanol and the glycol into water, stirring and dissolving uniformly to obtain a solution, and respectively packaging the solution and the potassium monopersulfate composite salt powder to obtain the double-component system low-temperature disinfectant.
The potassium monopersulfate composite salt of the embodiment adopts anti-caking high-stability potassium monopersulfate composite salt, which is prepared by the following method:
(1) adding 30% of hydrogen peroxide and 1% of stabilizer sodium tripolyphosphate by mass of the hydrogen peroxide into a reactor, controlling the temperature to be about 0 ℃, dropwise adding 30% of fuming sulfuric acid under the stirring condition, controlling the molar ratio of the hydrogen peroxide to the fuming sulfuric acid to be 2:1, and controlling the temperature to be below 15 ℃ for heat preservation reaction to obtain peroxidation reaction liquid.
(2) And (2) dropwise adding a potassium carbonate solution into the peroxidation reaction liquid in the step (1) to perform a neutralization reaction, wherein the molar ratio of the added potassium carbonate to fuming sulfuric acid (calculated as sulfate radicals) is 5:4 based on the molar amount of potassium, so as to obtain a neutralized liquid.
(3) And (3) adding liquid sodium silicate (crystal coprecipitator) with the mass concentration of 1.0% into the neutralized liquid obtained in the step (2), stirring and dissolving uniformly, concentrating in vacuum at about 50 ℃ until the solution is saturated, cooling to 0 ℃ for crystallization, and centrifugally drying to obtain the anti-caking high-stability potassium monopersulfate composite salt.
The low-temperature disinfectant of the embodiment can keep liquid, non-freezing and non-freezing at the temperature of minus 40 ℃. The sterilization and disinfection tests are respectively carried out at the normal temperature of 25 ℃, 18 ℃ and 40 ℃. The liquid single component system is directly used, and the double component system is used after potassium monopersulfate composite salt powder is added into the solution and evenly mixed.
1. The test was carried out according to the technical Specification for Disinfection (2002 edition) 2.1.1.10, technical requirement for evaluation of sanitary safety of Low temperature disinfectant.
2. The quantitative killing effect test on the staphylococcus aureus-pre-existing carrier: the action time is 10min, and the action temperature is 25 ℃, 18 ℃ and 40 ℃. The experiment was repeated three times.
3. Quantitative inactivation assay for poliovirus type I (vaccine strain) vectors: the action time is 10min, and the action temperature is 25 ℃, 18 ℃ and 40 ℃. The experiment was repeated three times.
The measurement result shows that the low-temperature disinfectant has the average killing logarithm value of being more than 4.00 to bacteria and viruses within 10min of action time. The disinfectant has good disinfection capability under both normal temperature and low temperature conditions. Meets the requirements of disinfection technical specification (2002 edition).
The stability of the disinfection activity of the liquid single-component system low-temperature disinfectant obtained in the example was tested (stored hermetically at 25 ℃ C. for 6 months) and the result showed that the retention rate of active oxygen was 89%. And the determination result of the retention rate of active oxygen of the low-temperature disinfectant prepared by the common potassium monopersulfate (compared with the preparation method of the anti-caking high-stability potassium monopersulfate composite salt, liquid sodium silicate is not added, and the rest is completely the same) is 62%. The potassium monopersulfate composite salt prepared by the specific method has the advantages of remarkably improved stability of disinfection activity, certain storage stability period, capability of being stored for later use as a liquid product and good use flexibility. The anti-caking performance of the potassium monopersulfate composite salt powder in the two-component system low-temperature disinfectant of the present example was tested (the ratio of the weight of particles passing through a 10-mesh sieve after being packaged and stored in a sealed bag at normal temperature for 6 months to the weight of particles passing through a 10-mesh sieve before storage) to obtain a result of 0.86, while the anti-caking performance of the common potassium monopersulfate composite salt (compared with the preparation method of the anti-caking high-stability potassium monopersulfate composite salt of the present invention, no liquid sodium silicate was added, and the rest were completely the same) was tested to obtain a result of 0.47. When the low-temperature disinfectant is applied as a two-component system consisting of powder and solution, the potassium monopersulfate composite salt powder as the active ingredient has good anti-caking performance and high storage stability. In addition, in the preparation process of the anti-caking high-stability potassium monopersulfate composite salt, the liquid sodium silicate is added, so that the product yield is obviously improved. The test shows that the product yield is improved from 72.3% to 91.1% compared with the common potassium monopersulfate composite salt prepared without adding liquid sodium silicate. The improvement effects of the anti-caking high-stability potassium monopersulfate composite salt on the product yield, the anti-caking performance and the stability are described in detail in the earlier application CN 2021111382584, an anti-caking high-stability potassium monopersulfate active salt disinfectant and a preparation method thereof. The results of the product yield, anti-caking properties and stability tests (based on the results of the determination of the retention of active oxygen after 7 days in a 1% solution at 20 ℃ in 300ppm hard water) obtained by adding different crystal co-precipitants during the preparation of the oxone complex salt are shown in table 1 below.
TABLE 1
| Different crystal coprecipitates | Product yield | Anti-caking Properties | Stability of |
| Blank control | 72.3％ | 0.47 | 83.8％ |
| Liquid sodium silicate | 91.1％ | 0.86 | 92.3％ |
| Sodium chloride | 77.7％ | 0.52 | 83.4％ |
| Sodium sulfate | 78.2％ | 0.36 | 84.1％ |
| Nano calcium silicate powder | 72.1％ | 0.89 | 86.7％ |
| Nano silicon dioxide powder | 72.5％ | 0.87 | 88.0％ |
As can be seen from the results in table 1, the product yield can be improved to some extent by adding soluble sodium salt as co-precipitation, but the improvement effect is significantly different from that of liquid sodium silicate, and the anti-caking property and stability are not significantly improved. The common inorganic anti-caking additive (nano calcium silicate powder and nano silicon dioxide powder) is added to achieve good anti-caking performance, but the product yield is not obviously improved. And the liquid sodium silicate adopted by the invention has more remarkable effect of improving the stability of the product.
Example 2
The potassium monopersulfate low-temperature disinfectant comprises the following components in percentage by mass:
the low-temperature potassium monopersulfate disinfectant is prepared by the following method: adding sodium dodecyl sulfate, tartaric acid, sodium polyphosphate, calcium chloride, ethanol and ethylene glycol into water, stirring and dissolving uniformly, then adding potassium monopersulfate composite salt, stirring and dissolving uniformly to obtain a liquid single-component system low-temperature disinfectant; or adding the surfactant, the organic acid, the inorganic buffer salt, the calcium chloride, the ethanol and the glycol into water, stirring and dissolving uniformly to obtain a solution, and respectively packaging the solution and the potassium monopersulfate composite salt powder to obtain the double-component system low-temperature disinfectant.
The potassium monopersulfate composite salt of the present example was an anti-caking high-stability potassium monopersulfate composite salt, and the preparation method thereof was the same as that of example 1.
The low-temperature disinfectant of the embodiment can keep liquid, non-freezing and non-freezing at the temperature of minus 40 ℃. The sterilization and disinfection tests are respectively carried out at the normal temperature of 25 ℃, 18 ℃ and 40 ℃. The liquid single component system is directly used, and the double component system is used after potassium monopersulfate composite salt powder is added into the solution and evenly mixed.
1. The test was carried out according to the technical Specification for Disinfection (2002 edition) 2.1.1.10, technical requirement for evaluation of sanitary safety of Low temperature disinfectant.
2. The quantitative killing effect test on the staphylococcus aureus-pre-existing carrier: the action time is 10min, and the action temperature is 25 ℃, 18 ℃ and 40 ℃. The test was repeated three times.
3. Quantitative inactivation assay for poliovirus type I (vaccine strain) vectors: the action time is 10min, and the action temperature is 25 ℃, 18 ℃ and 40 ℃. The experiment was repeated three times.
The measurement result shows that the low-temperature disinfectant has the average killing logarithm value of being more than 4.00 to bacteria and viruses within 10min of action time. The disinfectant has good disinfection capability under both normal temperature and low temperature conditions. Meets the requirements of disinfection technical specification (2002 edition).
The stability of the disinfection activity of the liquid single-component system low-temperature disinfectant obtained in the example was tested (stored hermetically at 25 ℃ C. for 6 months) and the result showed that the retention rate of active oxygen was 81%. And the determination result of the retention rate of active oxygen of the low-temperature disinfectant prepared by the common potassium monopersulfate (compared with the preparation method of the anti-caking high-stability potassium monopersulfate composite salt, liquid sodium silicate is not added, and the rest is completely the same) is 56%. The potassium monopersulfate composite salt prepared by the specific method has the advantages of remarkably improved stability of disinfection activity, certain storage stability period, capability of being stored for later use as a liquid product and good use flexibility.
Example 3
The potassium monopersulfate low-temperature disinfectant comprises the following components in percentage by mass:
the low-temperature potassium monopersulfate disinfectant is prepared by the following method: adding sodium dodecyl benzene sulfonate, malic acid, sodium polyphosphate, calcium chloride, ethanol and ethylene glycol into water, stirring and dissolving uniformly, then adding potassium monopersulfate composite salt, stirring and dissolving uniformly to obtain a liquid single-component system low-temperature disinfectant; or adding the surfactant, the organic acid, the inorganic buffer salt, the calcium chloride, the ethanol and the glycol into water, stirring and dissolving uniformly to obtain a solution, and respectively packaging the solution and the potassium monopersulfate composite salt powder to obtain the double-component system low-temperature disinfectant.
The potassium monopersulfate composite salt used in this example was an anti-caking high-stability potassium monopersulfate composite salt, and the preparation method was the same as in example 1.
The low-temperature disinfectant of the embodiment can keep liquid, non-freezing and non-freezing at the temperature of minus 40 ℃. The sterilization and disinfection tests were carried out at normal temperature of 25 deg.C, -18 deg.C, -40 deg.C, respectively. The liquid single component system is directly used, and the double component system is used after potassium monopersulfate composite salt powder is added into the solution and evenly mixed.
1. The test was carried out according to specification of Disinfection (2002 edition) 2.1.1.10, specification of Low temperature disinfectant sanitation evaluation technical requirement.
2. The quantitative killing effect test on the staphylococcus aureus-pre-existing carrier: the action time is 10min, and the action temperature is 25 ℃, 18 ℃ and 40 ℃. The experiment was repeated three times.
3. Quantitative inactivation assay for poliovirus type I (vaccine strain) vectors: the action time is 10min, and the action temperature is 25 ℃, 18 ℃ and 40 ℃. The experiment was repeated three times.
The measurement result shows that the average killing logarithm value of the low-temperature disinfectant on bacteria and viruses is more than 4.00 after the low-temperature disinfectant is applied for 10 min. The disinfectant has good disinfection capability under both normal temperature and low temperature conditions. Meets the requirements of disinfection technical specification (2002 edition).
The stability of the disinfection activity of the liquid single-component system low-temperature disinfectant obtained in the embodiment is tested (the liquid single-component system low-temperature disinfectant is stored hermetically at the normal temperature of 25 ℃ for 6 months), and the result shows that the retention rate of active oxygen is 91%. And the determination result of the active oxygen retention rate of the low-temperature disinfectant prepared by the common potassium monopersulfate (compared with the preparation method of the anti-caking high-stability potassium monopersulfate composite salt, liquid sodium silicate is not added, and the other parts are completely the same) is 73%. The potassium monopersulfate composite salt prepared by the specific method has the advantages of remarkably improved stability of disinfection activity, certain storage stability period, capability of being stored for later use as a liquid product and good use flexibility.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (6)
1. The low-temperature potassium monopersulfate disinfectant is characterized by comprising a liquid single-component system or a double-component system consisting of powder and solution; the liquid single-component system comprises potassium monopersulfate complex salt, a surfactant, organic acid, inorganic buffer salt, calcium chloride, ethanol, ethylene glycol and water; the powder in the two-component system comprises potassium monopersulfate composite salt, and the solution comprises a surfactant, organic acid, inorganic buffer salt, calcium chloride, ethanol, ethylene glycol and water;
the potassium monopersulfate composite salt is an anti-caking high-stability potassium monopersulfate composite salt and is prepared by the following method:
(1) adding hydrogen peroxide and a stabilizer into a reactor, controlling the temperature to be 0-5 ℃, dropwise adding fuming sulfuric acid under the stirring condition, and controlling the temperature to be below 15 ℃ for heat preservation reaction to obtain peroxidation reaction liquid;
(2) dropwise adding a potassium carbonate or potassium hydroxide solution into the peroxidation reaction liquid in the step (1) to carry out neutralization reaction to obtain a neutralization liquid;
(3) adding liquid sodium silicate into the neutralized solution obtained in the step (2), stirring and dissolving uniformly, concentrating in vacuum, cooling and crystallizing, and centrifugally drying to obtain anti-caking high-stability potassium monopersulfate composite salt;
the stabilizer in the step (1) is trisodium phosphate or sodium polyphosphate; the addition amount of the stabilizer is 0.5-2% of the mass of the hydrogen peroxide;
in the step (2), the molar ratio of the addition amount of the potassium carbonate or the potassium hydroxide to the fuming sulfuric acid is (4.8-5.2): 4;
in the step (3), the addition amount of the liquid sodium silicate is 0.2-4% of the mass of the neutralizing liquid.
2. The oxone low-temperature disinfectant according to claim 1, wherein the low-temperature disinfectant comprises the following components by mass percent:
0.2-3% of potassium monopersulfate composite salt;
0.5% -5% of a surfactant;
0.3% -2% of organic acid;
5% -15% of inorganic buffer salt;
1% -5% of calcium chloride;
5% -20% of ethanol;
6% -15% of ethylene glycol;
the balance of water.
3. The oxone low temperature disinfectant according to claim 1 or 2, wherein the surfactant is at least one of sodium alkyl benzene sulfonate and sodium alkyl sulfonate; the organic acid is at least one of malic acid, citric acid and tartaric acid; the inorganic buffer salt is sodium polyphosphate.
4. The low-temperature potassium monopersulfate disinfectant as claimed in claim 1, wherein in the step (1), the hydrogen peroxide and the oleum are diluted to 20-50% by mass before reaction; the molar ratio of the hydrogen peroxide to the fuming sulfuric acid is (1-3) to 1.
5. The low-temperature potassium monopersulfate disinfectant as set forth in claim 1, wherein in the step (3), the vacuum concentration is performed at 45-55 ℃ until saturation; the cooling crystallization refers to standing crystallization at the temperature of minus 4-4 ℃.
6. The preparation method of the oxone low-temperature disinfectant as claimed in any one of claims 1 to 5, which comprises the following preparation steps:
adding a surfactant, an organic acid, an inorganic buffer salt, calcium chloride, ethanol and glycol into water, stirring and dissolving uniformly, then adding a potassium monopersulfate composite salt, stirring and dissolving uniformly to obtain a liquid single-component system low-temperature disinfectant; or adding the surfactant, the organic acid, the inorganic buffer salt, the calcium chloride, the ethanol and the glycol into water, stirring and dissolving uniformly to obtain a solution, and respectively packaging the solution and the potassium monopersulfate composite salt powder to obtain the double-component system low-temperature disinfectant.
Priority Applications (1)
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| CN114794091A (en) * | 2022-03-15 | 2022-07-29 | 北京可佳永好科贸有限公司 | Low-temperature disinfection powder and preparation method and application thereof |
| CN114984736A (en) * | 2022-05-12 | 2022-09-02 | 惠州市栢诗新材料有限公司 | Application of potassium monopersulfate composite salt in formaldehyde removal preparation |
| CN114711250A (en) * | 2022-05-23 | 2022-07-08 | 山东润兴环保科技有限公司 | Potassium monopersulfate compound cleaning disinfectant and preparation method thereof |
| CN114847289B (en) * | 2022-06-16 | 2024-05-31 | 深圳市质量安全检验检测研究院 | Acid virus nucleic acid degradation disinfection method |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1545883A (en) * | 2003-12-15 | 2004-11-17 | 韶山大北农动物药业有限公司 | Water soluble composite potassium monopersulfate powder disinfectant |
| CN102265904A (en) * | 2011-06-03 | 2011-12-07 | 宋海鹏 | Compound potassium hydrogen persulfate disinfectant and manufacturing process thereof |
| CN106973939A (en) * | 2017-05-11 | 2017-07-25 | 江苏苏沃尚新材料科技有限公司 | A kind of monopersulfate hydrogen potassium composite disinfectant |
| CN108041073A (en) * | 2018-01-23 | 2018-05-18 | 广东贝特涞生物科技有限公司 | Potassium peroxymonosulfate disinfectant |
| CN109730086A (en) * | 2019-02-28 | 2019-05-10 | 湘潭大学 | A kind of preparation method of potassium peroxymonosulfate and the application sterilized in water process |
| CN112640912A (en) * | 2020-12-07 | 2021-04-13 | 泰安宏孚化工有限公司 | Active oxygen composite bactericide and preparation method thereof |
| CN113287627A (en) * | 2021-05-25 | 2021-08-24 | 中山市迈微环保科技有限公司 | Cleaning disinfectant containing potassium hydrogen persulfate compound, and use method and application thereof |
| CN113439758A (en) * | 2021-06-29 | 2021-09-28 | 上海泰缘生物科技股份有限公司 | Formula and use scheme of potassium monopersulfate low-temperature disinfectant |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050035066A1 (en) * | 2003-08-13 | 2005-02-17 | Martin Perry L. | Combining a solvent-activated reactor and a halogen for enhanced oxidation |
-
2021
- 2021-11-08 CN CN202111311734.8A patent/CN113854313B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1545883A (en) * | 2003-12-15 | 2004-11-17 | 韶山大北农动物药业有限公司 | Water soluble composite potassium monopersulfate powder disinfectant |
| CN102265904A (en) * | 2011-06-03 | 2011-12-07 | 宋海鹏 | Compound potassium hydrogen persulfate disinfectant and manufacturing process thereof |
| CN106973939A (en) * | 2017-05-11 | 2017-07-25 | 江苏苏沃尚新材料科技有限公司 | A kind of monopersulfate hydrogen potassium composite disinfectant |
| CN108041073A (en) * | 2018-01-23 | 2018-05-18 | 广东贝特涞生物科技有限公司 | Potassium peroxymonosulfate disinfectant |
| CN109730086A (en) * | 2019-02-28 | 2019-05-10 | 湘潭大学 | A kind of preparation method of potassium peroxymonosulfate and the application sterilized in water process |
| CN112640912A (en) * | 2020-12-07 | 2021-04-13 | 泰安宏孚化工有限公司 | Active oxygen composite bactericide and preparation method thereof |
| CN113287627A (en) * | 2021-05-25 | 2021-08-24 | 中山市迈微环保科技有限公司 | Cleaning disinfectant containing potassium hydrogen persulfate compound, and use method and application thereof |
| CN113439758A (en) * | 2021-06-29 | 2021-09-28 | 上海泰缘生物科技股份有限公司 | Formula and use scheme of potassium monopersulfate low-temperature disinfectant |
Non-Patent Citations (2)
| Title |
|---|
| 过一硫酸氢钠复合盐的合成;王铭佳 等;《无机盐工业》;20180411;第50卷(第4期);第40-42页 * |
| 过一硫酸氢钾复合消毒剂的制备及工艺设计;王铭佳;《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》;20190115(第1期);第B016-818页 * |
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