CN115363029A - Polyquaternary ammonium salt composite disinfectant and preparation method thereof - Google Patents
Polyquaternary ammonium salt composite disinfectant and preparation method thereof Download PDFInfo
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N33/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic nitrogen compounds
- A01N33/02—Amines; Quaternary ammonium compounds
- A01N33/12—Quaternary ammonium compounds
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/22—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing ingredients stabilising the active ingredients
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/30—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests characterised by the surfactants
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01P—BIOCIDAL, PEST REPELLANT, PEST ATTRACTANT OR PLANT GROWTH REGULATORY ACTIVITY OF CHEMICAL COMPOUNDS OR PREPARATIONS
- A01P1/00—Disinfectants; Antimicrobial compounds or mixtures thereof
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Abstract
The application relates to the technical field of disinfection, and particularly discloses a polyquaternium composite disinfectant and a preparation method thereof, wherein the polyquaternium composite disinfectant comprises the following raw materials in parts by weight: 2-15 parts of water-soluble polyquaternium, 4-8 parts of surfactant, 0.2-1 part of synergist, 0.01-0.05 part of pH regulator, 0.5-1.5 parts of softening agent and 65-100 parts of deionized water; the polyquaternium composite disinfectant prepared by the application has a good antibacterial property.
Description
Technical Field
The application relates to the technical field of disinfection, in particular to a polyquaternium composite disinfectant and a preparation method thereof.
Background
In daily life, people always come into contact with various bacteria and viruses, especially in crowded places with many people, such as buses, subways, entertainment places and the like. These pathogens pose a great threat to our health and wellness. Therefore, various disinfection solutions have been produced in the market. The use of the disinfectant can eliminate harmful microorganisms causing diseases of people and animals in various external environments, and control other microorganisms causing economic loss, thereby achieving the purposes of blocking the spread of infectious diseases, preventing nosocomial infection, reducing the damage of microorganisms to foods and articles, and promoting the production of industry and agriculture.
Common disinfectant in the market at present comprises cresol soap, 84 disinfectant, iodophor, hydrogen peroxide, alcohol, benzalkonium bromide and the like. They have excellent sterilizing and disinfecting effects, but still have various defects, such as pungent odor, strong irritation, high price and the like. Quaternary ammonium salt disinfectant is a disinfectant which is researched more in recent years, and especially, high molecular quaternary ammonium salt becomes a hotspot of current research and development due to the advantages of strong antibacterial property, small irritation, environmental protection and the like.
In view of the above-mentioned related technologies, the inventor considers that the existing quaternary ammonium salt disinfectant has insufficient adsorption capacity on bacteria, and the antibacterial performance is yet to be further improved.
Disclosure of Invention
In order to improve the antibacterial property of quaternary ammonium salt disinfectant, the application provides a polyquaternary ammonium salt composite disinfectant and a preparation method thereof.
In a first aspect, the application provides a polyquaternium composite disinfectant, which adopts the following technical scheme:
a polyquaternium composite disinfectant comprises the following raw materials in parts by weight: 2-15 parts of water-soluble polyquaternium, 4-8 parts of surfactant, 0.2-1 part of synergist, 0.01-0.05 part of pH regulator, 0.5-1.5 parts of softening agent and 65-100 parts of deionized water.
By adopting the technical scheme, the polyquaternary ammonium salt compound disinfectant prepared by the application has the advantages that the water-soluble polyquaternary ammonium salt is added into the surfactant, the synergist, the pH regulator, the softening agent and the deionized water, so that the antibacterial property of the disinfectant is improved. The antibacterial process of quaternary ammonium salts can be divided into several steps, i.e., adsorption to the surface of bacteria, penetration of cell walls, binding to cell membranes, disturbing the cell membrane composition, causing leakage of intracellular substances, and finally death of the bacteria. The quaternary ammonium salt molecules are positively charged, after the high molecular weight treatment, the relative molecular weight is increased, the charge density is improved, and as the surfaces of microbial cells are negatively charged and phospholipid and membrane protein hydrolysate contained in cell membranes are also negatively charged, compared with small molecular monomers with the same structure, the water-soluble polyquaternary ammonium salt prepared by the method has the advantages that the molecular weight is increased, the adsorption of bacteria and the combination with the cell membranes are facilitated, and the antibacterial performance and the stability of the disinfectant are improved.
Preferably, the polyquaternium composite disinfectant comprises the following raw materials in parts by weight: 5-10 parts of water-soluble polyquaternium, 5.5-6.5 parts of surfactant, 0.4-0.8 part of synergist, 0.02-0.04 part of pH regulator, 0.8-1.2 parts of softening agent and 80-90 parts of deionized water.
By adopting the technical scheme, the antibacterial property of the prepared polyquaternium composite disinfectant is better when the raw material dosage of the polyquaternium composite disinfectant is in the range by optimizing the raw material dosage of the polyquaternium composite disinfectant.
Preferably, the water-soluble polyquaternium is prepared by reacting tetramethylethylenediamine, dichloroethyl ether and a catalyst; the mass ratio of the tetramethylethylenediamine to the dichloroethyl ether is 1-2.
By adopting the technical scheme, tetramethylethylenediamine and dichloroethyl ether are used as raw materials, a polymerization reaction is carried out under the condition of a catalyst to synthesize the high-molecular water-soluble polyquaternium containing long-chain alkyl, and the prepared water-soluble polyquaternium is used as a raw material and added into the preparation process of the disinfectant, so that the adsorption of thalli is facilitated, and the antibacterial property of the disinfectant is improved.
Preferably, the preparation method of the water-soluble polyquaternium comprises the following steps: mixing tetramethylethylenediamine, dichloroethyl ether and a catalyst, continuously stirring and uniformly mixing, wherein the reaction temperature is 80-100 ℃, and the reaction time is 4-8h.
By adopting the technical scheme, the preparation method of the water-soluble polyquaternium is simple and easy to implement, is convenient to operate, and can effectively improve the production efficiency; the reaction temperature and the reaction time in the preparation method have no obvious influence on the performance of the prepared water-soluble polyquaternium.
Preferably, the surfactant is a nonionic surfactant.
By adopting the technical scheme, the nonionic surfactant has certain wetting and sterilizing effects, and the stability of the disinfectant can be improved by adding the nonionic surfactant.
Preferably, the nonionic surfactant comprises one or more of fatty alcohol polyoxyethylene ether surfactants, polyol ester surfactants and span.
Preferably, the pH regulator comprises one or more of triethanolamine, citric acid, amino acid and lactic acid.
Preferably, the synergist is dodecyl dimethyl amine oxide.
By adopting the technical scheme, the dodecyl dimethyl amine oxide synergist is adopted, so that the bactericidal effect of the quaternary ammonium salt can be remarkably enhanced.
In a second aspect, the application provides a preparation method of a polyquaternium composite disinfectant, which adopts the following technical scheme: a preparation method of a polyquaternium composite disinfectant comprises the following steps:
1) Uniformly mixing a surfactant and a softening agent, heating to 60-80 ℃, and reacting for 1-3min to obtain a first mixture;
2) Uniformly mixing the synergist and deionized water to obtain a second mixture, and adding the second mixture into the first mixture to obtain a third mixture;
3) And sequentially adding the water-soluble polyquaternium and the pH regulator into the third mixture, and homogenizing for 5-15min at the speed of 4500-6000rpm to obtain the polyquaternium composite disinfectant.
By adopting the technical scheme, the water-soluble polyquaternium, the surfactant, the synergist, the pH regulator, the softening agent and the deionized water are blended in a certain sequence, so that the prepared polyquaternium composite disinfectant has better antibacterial property and stability.
In summary, the present application has the following beneficial effects:
1. according to the polyquaternium composite disinfectant prepared by the application, the water-soluble polyquaternium is added into the surfactant, the synergist, the pH regulator, the softening agent and the deionized water, so that the antibacterial property of the disinfectant is improved. The antibacterial process of quaternary ammonium salts can be divided into several steps, i.e., adsorption to the surface of bacteria, penetration of cell walls, binding to cell membranes, disturbing the cell membrane composition, causing leakage of intracellular substances, and finally death of the bacteria. The quaternary ammonium salt molecules are positively charged, after the high molecular weight treatment, the relative molecular weight is increased, the charge density is improved, and as the surfaces of microbial cells are negatively charged and phospholipid and membrane protein hydrolysate contained in cell membranes are also negatively charged, compared with small molecular monomers with the same structure, the water-soluble polyquaternary ammonium salt prepared by the method has the advantages that the molecular weight is increased, the adsorption of bacteria and the combination with the cell membranes are facilitated, and the antibacterial performance and the stability of the disinfectant are improved.
2. The polyquaternary ammonium salt composite disinfectant prepared by the application has good stability through antibacterial effect detection and stability test, and the phenomena of layered precipitation, peculiar smell and color change do not occur; the optimal antibacterial rate to escherichia coli reaches 99.98%, and the optimal antibacterial rate to staphylococcus aureus reaches 99.96%.
Detailed Description
The present application will be described in further detail with reference to examples.
Raw materials
The starting materials used in the present application are commercially available.
Preparation example
Preparation examples 1 to 3
The water-soluble polyquaternium of preparation examples 1 to 3, whose raw materials and amounts of the raw materials are shown in Table 1, was prepared by the following steps: mixing tetramethylethylenediamine, dichloroethyl ether and a catalyst, continuously stirring and uniformly mixing, wherein the reaction temperature is 80 ℃, and the reaction time is 4 hours, so as to obtain the water-soluble polyquaternium.
TABLE 1 raw materials and amounts (kg) of the raw materials of one of the water-soluble polyquaterniums of preparation examples 1 to 3
| Preparation example 1 | Preparation example 2 | Preparation example 3 | |
| Tetramethyl ethylene diamine | 10 | 15 | 20 |
| Dichloroethyl ether | 10 | 10 | 10 |
| Catalyst and process for producing the same | 1 | 1 | 1 |
Preparation example 4
A water-soluble polyquaternium which is different from that of preparation example 2 in that the reaction temperature is 90 ℃, and the rest steps are the same as those of preparation example 2.
Preparation example 5
A water-soluble polyquaternium which is different from that of preparation example 2 in that the reaction temperature is 100 ℃, and the rest steps are the same as those of preparation example 2.
Preparation example 6
A water-soluble polyquaternium which is different from that of preparation example 5 in that the reaction time is 6 hours, and the rest steps are the same as those of preparation example 5.
Preparation example 7
A water-soluble polyquaternium which is different from that of preparation example 5 in that the reaction time is 8h, and the rest steps are the same as those of preparation example 5.
Examples
Examples 1 to 4
The polyquaternium compound disinfectant of the embodiments 1 to 4 has the following preparation steps, wherein the raw materials and the use amounts of the raw materials are shown in table 2:
1) Uniformly mixing a surfactant and a softening agent, heating to 60 ℃, and reacting for 3min to obtain a first mixture;
2) Uniformly mixing the synergist and deionized water to obtain a second mixture, and adding the second mixture into the first mixture to obtain a third mixture;
3) And sequentially adding the water-soluble polyquaternium and the pH regulator into the third mixture, and homogenizing for 10min at the speed of 6000rpm to obtain the polyquaternium composite disinfectant.
Wherein the water-soluble polyquaternium is obtained from preparation example 1, the surfactant is fatty alcohol polyoxyethylene ether surfactant, and the pH regulator is triethanolamine.
TABLE 2 materials and amounts (kg) of materials of examples 1-4
| Example 1 | Example 2 | Example 3 | Example 4 | |
| Water-soluble polyquaternium | 2 | 2 | 2 | 2 |
| Surface active agent | 4 | 5.5 | 6.5 | 8 |
| Synergist | 1 | 0.8 | 0.4 | 0.2 |
| PH regulator | 0.01 | 0.02 | 0.04 | 0.05 |
| Softening and moistening agent | 1.5 | 1.2 | 0.8 | 0.5 |
| Deionized water | 65 | 80 | 90 | 100 |
Example 5
A polyquaternium compound disinfectant is different from that in example 3 in that water-soluble polyquaternium is obtained from preparation example 2, and the rest steps are the same as those in example 3.
Example 6
A polyquaternium compound disinfectant is different from that in example 3 in that water-soluble polyquaternium is obtained from preparation example 3, and the rest steps are the same as those in example 3.
Example 7
A polyquaternium compound disinfectant is different from that in example 5 in that water-soluble polyquaternium is obtained from preparation example 4, and the rest steps are the same as those in example 5.
Example 8
A polyquaternium compound disinfectant is different from the disinfectant in example 5 in that water-soluble polyquaternium is obtained from preparation example 5, and the rest steps are the same as those in example 5.
Example 9
A polyquaternium compound disinfectant is different from the disinfectant in the embodiment 7 in that water-soluble polyquaternium is obtained from the preparation 6, and the rest steps are the same as the embodiment 7.
Example 10
A polyquaternium compound disinfectant is different from the disinfectant in the embodiment 7 in that water-soluble polyquaternium is obtained from the preparation 7, and the rest steps are the same as the embodiment 7.
Example 11
A polyquaternium composite disinfectant is different from the disinfectant in the embodiment 10 in that the addition amount of water-soluble polyquaternium is 5kg, and the other steps are the same as the steps in the embodiment 10.
Example 12
A polyquaternium compound disinfectant is different from the disinfectant in the embodiment 10 in that the addition amount of water-soluble polyquaternium is 10kg, and the rest steps are the same as the steps in the embodiment 10.
Example 13
A polyquaternium composite disinfectant is different from the disinfectant in the embodiment 10 in that the addition amount of water-soluble polyquaternium is 15kg, and the other steps are the same as the steps in the embodiment 10.
Comparative example
Comparative example 1
The difference between the polyquaternium composite disinfectant and the embodiment 1 is that the mass ratio of the tetramethylethylenediamine to the dichloroethylether for preparing the water-soluble polyquaternium is 1:2, the rest of the steps are the same as in example 1.
Comparative example 2
The difference between the polyquaternium composite disinfectant and the embodiment 1 is that the mass ratio of the tetramethylethylenediamine to the dichloroethylether for preparing the water-soluble polyquaternium is 3:1, the rest of the procedure is the same as in example 1.
Comparative example 3
A polyquaternium compound disinfectant is different from the disinfectant in the embodiment 1 in that the reaction temperature is 50 ℃ when water-soluble polyquaternium is prepared, and the rest steps are the same as the steps in the embodiment 1.
Comparative example 4
A polyquaternium compound disinfectant is different from the disinfectant in the embodiment 1 in that the reaction temperature is 120 ℃ when water-soluble polyquaternium is prepared, and the rest steps are the same as the steps in the embodiment 1.
Comparative example 5
A polyquaternium compound disinfectant is different from the disinfectant in the embodiment 1 in that the addition amount of water-soluble polyquaternium is 0.5kg, and the rest steps are the same as the embodiment 1.
Comparative example 6
A polyquaternium compound disinfectant is different from the disinfectant in the embodiment 1 in that the addition amount of water-soluble polyquaternium is 20kg, and the rest steps are the same as the steps in the embodiment 1.
Performance test
Detection method/test method
The polyquaternium compound disinfectant was prepared according to the preparation methods of the polyquaternium compound disinfectant prepared in examples 1 to 13 and comparative examples 1 to 6, and then tested according to the following test methods, and the test results thereof are shown in table 3.
And (3) detecting the antibacterial effect: coli (8099) and staphylococcus aureus (ATCC 6538) were allowed to act for 30min according to "disinfection specifications", three times for each experiment, and the average was taken.
And (3) stability testing: the disinfectant prepared in the embodiment and the comparative example is placed at 25 ℃ for 10 days, then placed at-5 ℃ for 24 hours, placed at 40 ℃ for 24 hours, returned to room temperature, and observed whether layering, precipitation, peculiar smell and discoloration phenomena exist.
TABLE 3 test results of examples 1 to 13 and comparative examples 1 to 6
As can be seen from the data in Table 3, the polyquaternium composite disinfectant prepared by the method has better antibacterial property and stability by adding the prepared water-soluble polyquaternium.
According to the detection data of the embodiments 1 to 4, the ratio of the raw materials in the embodiment 3 is good, and the prepared polyquaternium composite disinfectant has no phenomena of layering precipitation and odor discoloration, and has good antibacterial property on escherichia coli and staphylococcus aureus.
According to the detection data of the embodiment 3, the embodiment 5-6 and the comparative example 1-2, the mass ratio of the tetramethylethylenediamine to the dichloroethyl ether in the water-soluble polyquaternium of the preparation example 2 is good, and the obtained polyquaternium composite disinfectant has good antibacterial property to escherichia coli and staphylococcus aureus and good stability when the water-soluble polyquaternium prepared by the preparation example 2 is used in the preparation process of the polyquaternium composite disinfectant.
As can be seen by combining the test data of example 5, examples 7 to 8 and comparative examples 3 to 4, the optimum reaction temperature of the water-soluble polyquaternium is 90 ℃; the detection data of the examples 9-10 are combined, so that the antibacterial property of the water-soluble polyquaternium on escherichia coli and staphylococcus aureus is gradually enhanced along with the increase of the reaction time during the preparation of the water-soluble polyquaternium; the optimal reaction temperature for preparing the water-soluble polyquaternium is 90 ℃, and the optimal reaction time is 8h.
The detection data of the embodiment 10, the embodiments 11 to 13 and the comparative examples 5 to 6 are combined, so that the antibacterial property of the finally obtained polyquaternary ammonium salt composite disinfectant is better along with the increase of the addition amount of the water-soluble polyquaternary ammonium salt, when the addition amount of the water-soluble polyquaternary ammonium salt is 15kg, the antibacterial rate of the obtained polyquaternary ammonium salt composite disinfectant on escherichia coli reaches 99.98%, the antibacterial rate on staphylococcus aureus reaches 99.96%, and the disinfectant also has better stability and does not have the phenomena of layering, precipitation and odor discoloration.
The specific embodiments are only for explaining the present application and are not limiting to the present application, and those skilled in the art can make modifications to the embodiments without inventive contribution as required after reading the present specification, but all the embodiments are protected by patent law within the scope of the claims of the present application.
Claims (9)
1. A polyquaternium composite disinfectant is characterized by comprising the following raw materials in parts by weight: 2-15 parts of water-soluble polyquaternium, 4-8 parts of surfactant, 0.2-1 part of synergist, 0.01-0.05 part of pH regulator, 0.5-1.5 parts of softening agent and 65-100 parts of deionized water.
2. The polyquaternium compound disinfectant as claimed in claim 1, wherein: the polyquaternium composite disinfectant comprises the following raw materials in parts by weight: 5-10 parts of water-soluble polyquaternium, 5.5-6.5 parts of surfactant, 0.4-0.8 part of synergist, 0.02-0.04 part of pH regulator, 0.8-1.2 parts of softening agent and 80-90 parts of deionized water.
3. The polyquaternium compound disinfectant as claimed in claim 1, wherein: the water-soluble polyquaternary ammonium salt is prepared by reacting tetramethylethylenediamine, dichloroethyl ether and a catalyst; the mass ratio of the tetramethylethylenediamine to the dichloroethyl ether is 1-2.
4. The polyquaternium compound disinfectant as claimed in claim 3, which is characterized in that: the preparation method of the water-soluble polyquaternium comprises the following steps: mixing tetramethylethylenediamine, dichloroethyl ether and a catalyst, continuously stirring and uniformly mixing, wherein the reaction temperature is 80-100 ℃, and the reaction time is 4-8h.
5. The polyquaternium compound disinfectant as claimed in claim 1, wherein: the surfactant is a nonionic surfactant.
6. The polyquaternium compound disinfectant as claimed in claim 5, wherein: the nonionic surfactant comprises one or more of fatty alcohol polyoxyethylene ether surfactant, polyalcohol ester surfactant and span.
7. The polyquaternium compound disinfectant as claimed in claim 1, wherein: the pH regulator comprises one or more of triethanolamine, citric acid, amino acid and lactic acid.
8. The polyquaternium compound disinfectant as claimed in claim 1, which is characterized in that: the synergist is dodecyl dimethyl amine oxide.
9. The method for preparing the polyquaternium composite disinfectant as claimed in any one of claims 1 to 8, which is characterized in that: the method comprises the following steps:
1) Uniformly mixing a surfactant and a softening agent, heating to 60-80 ℃, and reacting for 1-3min to obtain a first mixture;
2) Uniformly mixing the synergist and deionized water to obtain a second mixture, and adding the second mixture into the first mixture to obtain a third mixture;
3) And sequentially adding the water-soluble polyquaternium and the pH regulator into the third mixture, and homogenizing for 5-15min at the speed of 4500-6000rpm to obtain the polyquaternium composite disinfectant.
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| CN202211166833.6A CN115363029A (en) | 2022-09-23 | 2022-09-23 | Polyquaternary ammonium salt composite disinfectant and preparation method thereof |
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Application publication date: 20221122 |
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