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CN113994969A - Sodium pyrithione compound preservative, preparation method and application thereof - Google Patents

Sodium pyrithione compound preservative, preparation method and application thereof Download PDF

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CN113994969A
CN113994969A CN202111247803.3A CN202111247803A CN113994969A CN 113994969 A CN113994969 A CN 113994969A CN 202111247803 A CN202111247803 A CN 202111247803A CN 113994969 A CN113994969 A CN 113994969A
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sodium pyrithione
preservative
spt
stirring
sodium
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CN113994969B (en
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侯玉波
杨澄钶
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Shanghai Mccann Biotechnology Co ltd
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    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
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    • A01N43/34Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom
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    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
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    • A01N43/72Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms
    • A01N43/80Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms five-membered rings with one nitrogen atom and either one oxygen atom or one sulfur atom in positions 1,2
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    • A61P31/00Antiinfectives, i.e. antibiotics, antiseptics, chemotherapeutics
    • A61P31/02Local antiseptics
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    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
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    • A61P31/00Antiinfectives, i.e. antibiotics, antiseptics, chemotherapeutics
    • A61P31/04Antibacterial agents
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P31/00Antiinfectives, i.e. antibiotics, antiseptics, chemotherapeutics
    • A61P31/10Antimycotics

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Abstract

The invention relates to a preservative, in particular to a sodium pyrithione compound preservative, a preparation method and application thereof, belonging to the technical field of inorganic chemistry. The sodium pyrithione compound preservative comprises the following components in percentage by weight: 2.5-20.0 percent of Sodium Pyrithione (SPT), 0.1-9.5 percent of Benzisothiazolinone (BIT), 0.0-10.0 percent of Methylisothiazolinone (MIT), 0.1-10.0 percent of chelating agent, 0.1-10.0 percent of antifreezing agent, 0.01-5.0 percent of pH regulator and the balance of water. The invention effectively solves the problem of product discoloration caused by the reaction of SPT and iron ions when the iron ion content is 1ppm in the prior art.

Description

Sodium pyrithione compound preservative, preparation method and application thereof
Technical Field
The invention relates to a preservative, in particular to a sodium pyrithione compound preservative, a preparation method and application thereof, belonging to the technical field of inorganic chemistry.
Background
Sodium pyrithione, alternative name: pyrithiofamid; sodium α -mercaptopyridine-N-oxide; SPT; sodium olmesartan, english name: sodium Pyrithione, CAS number: 3811-73-2, structural formula:
Figure BDA0003321681780000011
SPT is mainly used for mildew resistance and bacteria resistance of products in the fields of daily chemical industry (shampoo and hair care products), building coatings, adhesives, sealants, pesticides, textiles, leather products, metal working fluids and the like. Can also be used for preparing disinfectant, cleaning agent and broad-spectrum antifungal dermatologic medicine. Meanwhile, the disinfectant is an effective disinfectant for crops such as fruit trees, peanuts, wheat and vegetables and an excellent disinfectant for silkworms. SPT and its similar products are widely used in the related fields due to their excellent properties of high efficiency, broad spectrum and low toxicity.
SPT will react with Fe in aqueous systems2+、Fe3+Complexation occurs, resulting in discoloration of the system, especially in white emulsions, which can result in the white emulsion turning purple, as shown in FIG. 1. When the content of iron ions is 1ppm, SPT can cause the color of the product to change; at an iron ion content of 3ppm, SPT causes significant discoloration of the product. Complete removal of iron ions is almost impossible in industrial production, thus limiting the use of SPT in industrial production.
Disclosure of Invention
The invention aims to provide a sodium pyrithione compound preservative to solve the problem of product discoloration caused by the reaction of SPT and iron ions.
The technical scheme adopted by the invention for solving the technical problems is as follows:
the sodium pyrithione compound preservative comprises the following components in percentage by weight:
Figure BDA0003321681780000012
Figure BDA0003321681780000021
preferably, the chelating agent is one or more selected from sodium tripolyphosphate, diethylenetriamine pentaacetic acid, ethylene diamine tetraacetic acid disodium, ethylene diamine tetraacetic acid tetrasodium, hydroxyethylidene diphosphonic acid tetrasodium, and ethylene diamine tetramethylene phosphoric acid.
Preferably, the antifreezing agent is one or more selected from ethylene glycol, propylene glycol, glycerol and isopropanol.
Preferably, the pH regulator is one selected from the group consisting of sodium hydroxide, potassium hydroxide, lithium hydroxide, 2-amino-2-methyl-1-propanol (AMP-95), and aqueous ammonia.
Preferably, the pH value of the sodium pyrithione compound preservative is 9.0 to 9.5.
Preferably, the weight percentage formula of each component of the sodium pyrithione compound preservative is as follows:
Figure BDA0003321681780000022
a preparation method of the sodium pyrithione compound preservative comprises the following steps:
s1, adding the water with the formula amount into a container, adding the SPT with the formula amount into the container under the condition of stirring at a low speed of not more than 100r/min, and uniformly dispersing;
s2, adding the chelating agent with the formula amount under the low-speed stirring of not more than 100r/min, and dispersing uniformly;
s3, slowly adding BIT with the formula amount under the condition of low-speed stirring of not more than 100r/min, and adding a pH regulator in the process of dissolution after the BIT is completely added to keep the pH value of the system between 9.0 and 9.5;
and S4, after the BIT is completely dissolved, adding MIT in the formula amount, fully dispersing, and uniformly stirring to obtain the product.
The application of the sodium pyrithione compound preservative in the aspects of mildew prevention, antibiosis and corrosion prevention in industrial production. The sodium pyrithione compound preservative is suitable for mildew prevention and antibiosis of products in the fields of daily chemical industry (shampoo and hair care products), building coatings, adhesives, sealants, pesticides, textiles, leather products, metal working fluids and the like with the concentration of iron ions less than or equal to 40ppm, can also be used for preparing products such as disinfectants, cleaning agents, medical broad-spectrum antifungal dermatology medicines and the like, and effective bactericides of crops such as fruit trees, peanuts, wheat, vegetables and the like and excellent disinfectants for silkworms.
Compared with the prior art, the sodium pyrithione compound preservative and the preparation method thereof have the following beneficial effects:
1. experiments prove that when the concentration of iron ions is less than or equal to 40ppm, the system can not change color by adding the sodium pyrithione compound preservative, and the invention effectively solves the problem of product color change caused by the reaction of SPT and iron ions when the content of iron ions is 1ppm in the prior art;
2. the sodium pyrithione compound preservative disclosed by the invention generates a synergistic effect by compounding a plurality of sterilization components, effectively improves the antibacterial effect, has lower Minimum Inhibitory Concentration (MIC) compared with the single use of SPT and BIT with the same concentration, is more balanced to the MIC of a plurality of strains, and has broad sterilization spectrum;
3. the sodium pyrithione compound preservative disclosed by the invention uses water as a main carrier, and is safe to operate.
4. The sodium pyrithione compound preservative has high flash point, is not easy to burn and explode, and is safe to store and transport.
5. The sodium pyrithione compound preservative has the advantages of simple process, normal temperature and pressure, convenient industrial production, low cost, environmental protection and easy operation.
Drawings
FIG. 1 is a photograph of a prior art SPT reacted with iron ions to cause discoloration.
Detailed Description
The technical solution of the present invention will be further specifically described below by way of specific examples. It is to be understood that the practice of the invention is not limited to the following examples, and that any variations and/or modifications may be made thereto without departing from the scope of the invention.
In the present invention, all parts and percentages are by weight, unless otherwise specified, and the equipment and materials used are commercially available or commonly used in the art. The methods in the following examples are conventional in the art unless otherwise specified.
Example 1: 2.5% SPT compound preservative
The formulation of the 2.5% SPT formulated preservative of this example is shown in Table 1.
TABLE 1 formulation of 2.5% SPT Compound preservative
Raw materials Mass percent%
SPT 2.5
BIT 2.5
MIT 2.5
Hydroxy ethylidene diphosphoric acid 5.0
Propylene glycol 0.1
50% sodium hydroxide aqueous solution Adjusting the pH value to 9.0-9.5
Deionized water Adding to 100 percent
The preparation method of the 2.5% SPT compound preservative comprises the following steps: adding deionized water calculated according to a formula into a stirring container, and adding 0.1% glycol under the condition of low-speed stirring at a speed of not more than 100r/min, so that the dispersion is uniform. Respectively adding 2.5 percent of SPT under the low-speed stirring of not more than 100r/min, and fully stirring. Thirdly, adding 5.0% of hydroxyl ethylene-diphosphonic acid under low-speed stirring of not more than 100r/min, fully stirring, uniformly dispersing, slowly adding calculated 2.5% of BIT powder, and increasing the rotating speed to 300-500 r/min until the BIT powder is not dissolved any more. And fifthly, slowly adding a pH regulator, keeping the pH value between 9.0 and 9.5, and stirring for 15min after the BIT powder is fully dissolved until the solution is completely clear. Sixthly, adding the calculated 2.5% MIT under the condition of stirring at a low speed of not more than 100r/min, fully stirring, and uniformly dispersing.
Example 2: 5.0% SPT compounded preservative
The formulation of the 5.0% SPT formulated preservative of this example is shown in Table 2.
TABLE 2 formulation of 5.0% BIT SPT COMPLEX STABILIZER
Figure BDA0003321681780000041
Figure BDA0003321681780000051
The preparation method of the 5.0% SPT compound preservative comprises the following steps: adding deionized water calculated according to a formula into a stirring container, adding 1.0% of glycol under the condition of low-speed stirring at a speed of not more than 100r/min, and uniformly dispersing. Respectively adding 5.0 percent of SPT under the low-speed stirring of not more than 100r/min, and fully stirring. Thirdly, adding 6.25% of tetrasodium ethylenediamine tetraacetate under low-speed stirring of not more than 100r/min, fully stirring, uniformly dispersing, slowly adding calculated 5.0% of BIT powder, and increasing the rotating speed to 300-500 r/min until the BIT powder is not dissolved any more. And fifthly, slowly adding a pH regulator, keeping the pH value between 9.0 and 9.5, and stirring for 15min after the BIT powder is fully dissolved until the solution is completely clear. Sixthly, adding the calculated 2.5% MIT under the condition of stirring at a low speed of not more than 100r/min, fully stirring, and uniformly dispersing.
Example 3: 8.0% SPT compound preservative
The formulation of the 8.0% SPT formulated preservative of this example is shown in Table 3.
TABLE 3 formulation of 8.0% BIT SPT compounded preservative
Raw materials Mass percent%
SPT 8.0
BIT 5.0
MIT 2.5
Ethylenediaminetetra (methylene) phosphoric acid 8.0
Isopropanol (I-propanol) 2.0
50% sodium hydroxide aqueous solution Adjusting the pH value to 9.0-9.5
Deionized water Adding to 100 percent
The preparation method of the 8.0% SPT compound preservative comprises the following steps: adding deionized water calculated according to a formula into a stirring container, adding 2.0% of isopropanol under the condition of low-speed stirring at a speed of not more than 100r/min, and uniformly dispersing. And adding 8.0% of SPT respectively under the low-speed stirring of not more than 100r/min, and fully stirring. Thirdly, adding 8.0% of ethylenediamine tetramethylene phosphoric acid under low-speed stirring of not more than 100r/min, fully stirring, uniformly dispersing, slowly adding calculated 5.0% of BIT powder, and increasing the rotating speed to 300-500 r/min until the BIT powder is not dissolved any more. And fifthly, slowly adding the pH regulator, keeping the pH value between 9.0 and 9.5, and stirring for 15min after the BIT powder is fully dissolved until the solution is completely clear. Sixthly, adding the calculated 2.5% MIT under the condition of stirring at a low speed of not more than 100r/min, fully stirring, and uniformly dispersing.
Example 4: 10.0% SPT compounded preservative
The formulation of the 10.0% SPT formulated preservative of this example is shown in Table 4.
TABLE 4 formulation of 10.0% BIT SPT reconstituted preservative
Raw materials Mass percent%
SPT 10.0
BIT 8.0
MIT 5.0
Tetrasodium hydroxy ethylidene diphosphate 10.0
Ethylene glycol 5.0
50% sodium hydroxide aqueous solution Adjusting the pH value to 9.0-9.5
Deionized water Adding to 100 percent
The preparation method of the 10.0% SPT compound preservative comprises the following steps: adding deionized water calculated according to a formula into a stirring container, adding 5.0% of glycol under the condition of low-speed stirring at a speed of not more than 100r/min, and uniformly dispersing. And adding 10.0% of SPT respectively under the low-speed stirring of not more than 100r/min, and fully stirring. Thirdly, 10.0% of hydroxyethylidene tetrasodium diphosphate is added under the low-speed stirring of not more than 100r/min, the mixture is fully stirred and uniformly dispersed, 8.0% of calculated BIT powder is slowly added, the rotating speed is increased to 300-500 r/min, and the BIT powder is not dissolved any more. And fifthly, slowly adding the pH regulator, keeping the pH value between 9.0 and 9.5, and stirring for 15min after the BIT powder is fully dissolved until the solution is completely clear. Sixthly, adding the calculated MIT of 5.0% under the condition of stirring at a low speed of not more than 100r/min, fully stirring and uniformly dispersing.
Example 5: 15.0% SPT compounded preservative
The formulation of the 15.0% SPT formulated preservative of this example is shown in Table 5.
TABLE 5 formulation of 15.0% BIT SPT reconstituted preservative
Figure BDA0003321681780000061
Figure BDA0003321681780000071
The preparation method of the 10.0% SPT compound preservative comprises the following steps: adding deionized water calculated according to a formula into a stirring container, adding 2.5% of glycol under the condition of low-speed stirring at a speed of not more than 100r/min, and uniformly dispersing. And adding 15.0% of SPT respectively under the low-speed stirring of not more than 100r/min, and fully stirring. Thirdly, 10.0% of hydroxyethylidene tetrasodium diphosphate is added under the low-speed stirring of not more than 100r/min, the mixture is fully stirred and uniformly dispersed, 5.0% of calculated BIT powder is slowly added, the rotating speed is increased to 300-500 r/min, and the BIT powder is not dissolved any more. And fifthly, slowly adding the pH regulator, keeping the pH value between 9.0 and 9.5, and stirring for 15min after the BIT powder is fully dissolved until the solution is completely clear. Sixthly, adding the calculated 2.5% MIT under the condition of stirring at a low speed of not more than 100r/min, fully stirring, and uniformly dispersing.
Example 6: 20.0% SPT compounded preservative
The 20.0% SPT formulated preservative formulation of this example is shown in Table 6.
TABLE 6 formulation of 20.0% SPT Compound preservative
Raw materials Mass percent%
SPT 20.0
BIT 5.0
MIT 2.5
Tetrasodium hydroxy ethylidene diphosphate 10.0
Ethylene glycol 2.5
50% sodium hydroxide aqueous solution Adjusting the pH value to 9.0-9.5
Deionized water Adding to 100 percent
The preparation method of the 20.0% SPT compound preservative comprises the following steps: adding deionized water calculated according to a formula into a stirring container, adding 2.5% of glycol under the condition of low-speed stirring at a speed of not more than 100r/min, and uniformly dispersing. And adding 20.0 percent of SPT respectively under the low-speed stirring of not more than 100r/min, and fully stirring. Thirdly, adding 10.0% of tetrasodium ethylenediamine tetraacetate while stirring at a low speed of not more than 100r/min, fully stirring, uniformly dispersing, slowly adding calculated 5.0% of BIT powder, and increasing the rotating speed to 300-500 r/min until the BIT powder is not dissolved any more. And fifthly, slowly adding the pH regulator, keeping the pH value between 9.0 and 9.5, and stirring for 15min after the BIT powder is fully dissolved until the solution is completely clear. Sixthly, adding the calculated 2.5% MIT under the condition of stirring at a low speed of not more than 100r/min, fully stirring, and uniformly dispersing.
The performance indices of the products obtained in examples 1 to 6 are shown in Table 7.
TABLE 7
Figure BDA0003321681780000081
Thermal stability verification conditions: whether the content of the substance is within a range of. + -. 5% after 7 days at 50 ℃.
Cold stability verification conditions: and at the temperature of-4 ℃, after the sample is completely frozen, the sample is placed at the temperature of 25 ℃ to judge whether the appearance of the sample can completely recover to the state before freezing.
Application example 1 color Change test
The SPT compound preservative prepared in the examples 1-6 is used for carrying out a color change experiment to verify the color change of the product under different iron ion concentrations, and the specific operation is as follows: first, anhydrous Fe3Diluting Cl into aqueous solutions with iron ion concentrations of 1ppm, 3ppm, 5ppm, 7ppm, 9ppm, 11ppm, 13ppm, 15ppm, 20ppm, 30ppm, 40ppm, 50ppm, 70ppm and 100ppm by deionized water respectively; the samples of the embodiments 1 to 6 are respectively added into aqueous solutions containing iron ions with different concentrations according to the concentration of 0.2 percent, the dispersion is uniform, and the color change of the aqueous solutions is observed.
TABLE 8
Figure BDA0003321681780000082
Figure BDA0003321681780000091
Table 8 (continuation)
Figure BDA0003321681780000092
As is clear from the data in Table 8, when the iron ion concentration exceeds 50ppm, the addition of examples 1 to 6 causes yellowing of the product, but when the iron ion concentration is less than 50ppm, the addition of examples 1 to 6 causes no discoloration of the product.Please note that: not changing into purple
Application example 2 MIC assay
In this example, the Minimum Inhibitory Concentrations (MICs) of 20% SPT, 20% BIT, the sample of example 1, the sample of example 2, the sample of example 3, and the sample of example 4 were measured using Escherichia coli (Escherichia coli), Staphylococcus aureus (Staphylococcus aureus), Bacillus subtilis, Aspergillus niger (Aspergillus niger), Aureobasidium pullulans (Aureobasidium pullulans), and Saccharomyces cerevisiae (Saccharomyces cerevisiae), respectively.
1. Preparation of samples of different concentrations
Accurately weighing, firstly preparing a test sample into a 0.5% deionized water solution, and then performing 2-time gradient dilution on the sterilized normal saline to obtain test samples with different concentrations.
2. Preparation of Medium plates containing samples of different concentrations
1ml of the sample containing the gradient concentration was added to the sterilized petri dish, 19ml of the sterilized medium was added, cooled for later use, and recorded.
3. Inoculation of test bacteria
Test strains are respectively inoculated in culture medium plates containing test samples with different concentrations, and streaking inoculation is carried out. Blank control was also performed. And three replicates were made.
Then, the culture medium plate inoculated with the bacteria is placed in an incubator at 37 ℃ for 2-3 days and then observed.
And (3) placing the culture medium plate inoculated with the mould and the microzyme in an incubator at 28 ℃ for 4-5 days, and observing.
4. Determination of Minimum Inhibitory Concentration (MIC)
Observing that the culture medium plate of the same test strain of the same test sample has colony growth in the test sample with lower concentration and no growth in the test sample with higher concentration under adjacent concentration, and determining that the Minimum Inhibitory Concentration (MIC) of the test sample to the strain is lower concentration.
The Minimum Inhibitory Concentration (MIC) results for examples 1-6 are shown in Table 9.
TABLE 9 (unit: mg/kg)
Figure BDA0003321681780000101
Note: the strains used in the test were standard strains.
According to the experimental data of table 9: example 3 the concentration of the compound preservative is 15.5% in total, and the MIC of each strain in Table 9 is more balanced with that of SPT or BIT with the specific concentration of 20% in example 3, which proves that the broad spectrum antibacterial property of example 3 is more excellent. Meanwhile, compared with the MIC of each strain in Table 9 in example 4, example 5 and example 6 and the SPT or BIT with the concentration of 20%, the advantages are more obvious; the SPT compound preservative is proved to have more excellent antibacterial broad spectrum.
The embodiments are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same or similar parts among the embodiments are referred to each other. The device disclosed by the embodiment corresponds to the method disclosed by the embodiment, so that the description is simple, and the relevant points can be referred to the method part for description.
The sodium pyrithione compound preservative, the preparation method and the application thereof provided by the invention are described in detail above. The principles and embodiments of the present invention are explained herein using specific examples, which are presented only to assist in understanding the method and its core concepts. It should be noted that, for those skilled in the art, it is possible to make various improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the scope of the claims of the present invention.

Claims (10)

1. The sodium pyrithione compound preservative is characterized in that the formula of the sodium pyrithione compound preservative in percentage by weight is as follows:
Figure FDA0003321681770000011
2. the sodium pyrithione formulated preservative according to claim 1, characterized in that: the chelating agent is one or more selected from sodium tripolyphosphate, diethylenetriamine pentaacetic acid, disodium ethylene diamine tetraacetate, tetrasodium ethylene diamine tetraacetate, hydroxyethylidene diphosphonic acid, tetrasodium hydroxyethylidene diphosphonate and ethylene diamine tetramethylene phosphoric acid.
3. The sodium pyrithione formulated preservative according to claim 1, characterized in that: the antifreezing agent is one or more selected from ethylene glycol, propylene glycol, glycerol and isopropanol.
4. The sodium pyrithione formulated preservative according to claim 1, characterized in that: the pH regulator is selected from one of sodium hydroxide, potassium hydroxide, lithium hydroxide, 2-amino-2-methyl-1-propanol (AMP-95) or ammonia water.
5. The sodium pyrithione formulated preservative according to claim 1, characterized in that: the pH value of the sodium pyrithione compound preservative is 9.0-9.5.
6. The sodium pyrithione formulated preservative according to claim 1, characterized in that: the sodium pyrithione compound preservative comprises the following components in percentage by weight:
Figure FDA0003321681770000012
7. the sodium pyrithione formulated preservative according to claim 1, characterized in that: the sodium pyrithione compound preservative contains:
10.0 to 20.0 percent of Sodium Pyrithione (SPT),
2.5 to 8.0 percent of Benzisothiazolinone (BIT),
2.5 to 5.0 percent of Methylisothiazolinone (MIT).
8. A method for preparing the sodium pyrithione complex preservative according to claim 1, comprising the steps of:
s1, adding the water with the formula amount into a container, adding the SPT with the formula amount into the container under the condition of stirring at a low speed of not more than 100r/min, and uniformly dispersing;
s2, adding the chelating agent with the formula amount under the low-speed stirring of not more than 100r/min, and dispersing uniformly;
s3, slowly adding BIT with the formula amount under the condition of low-speed stirring of not more than 100r/min, and adding a pH regulator in the process of dissolution after the BIT is completely added to keep the pH value of the system between 9.0 and 9.5;
and S4, after the BIT is completely dissolved, adding MIT in the formula amount, fully dispersing, and uniformly stirring to obtain the product.
9. The application of the sodium pyrithione compound preservative of claim 1 in mildew prevention, antibiosis and preservation in industrial production.
10. Use according to claim 9, characterized in that: the application is mildew-proof, antibacterial and antiseptic treatment on products with the concentration of iron ions less than or equal to 40ppm, the products comprise daily chemical industry, building coatings, adhesives, sealants, pesticides, textiles, leather products, metal processing liquids, medical medicines and crops, and the daily chemical industry comprises shampoos and hair care products.
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002128609A (en) * 2000-10-27 2002-05-09 Nagase Kasei Kogyo Kk Antimicrobial agent composition
CN101044853A (en) * 2005-03-30 2007-10-03 栗田工业株式会社 Industrial antibiotic composition and antibacterial method
CN103931627A (en) * 2014-05-13 2014-07-23 陕西省石油化工研究设计院 Composite synergistic bactericidal and preservative agent for organic foaming agents
CN105101948A (en) * 2013-04-18 2015-11-25 宝洁公司 Personal care composition comprising zinc pyrithione and metal-phosphonate complex

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002128609A (en) * 2000-10-27 2002-05-09 Nagase Kasei Kogyo Kk Antimicrobial agent composition
CN101044853A (en) * 2005-03-30 2007-10-03 栗田工业株式会社 Industrial antibiotic composition and antibacterial method
CN105101948A (en) * 2013-04-18 2015-11-25 宝洁公司 Personal care composition comprising zinc pyrithione and metal-phosphonate complex
CN103931627A (en) * 2014-05-13 2014-07-23 陕西省石油化工研究设计院 Composite synergistic bactericidal and preservative agent for organic foaming agents

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
陈昭斌等: "化妆品中防腐剂的应用", 《中国消毒学杂志》, no. 10 *

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