CN111087653A - Preservative for waterborne polyurethane emulsion and preparation method thereof - Google Patents
Preservative for waterborne polyurethane emulsion and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/02—Organic and inorganic ingredients
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/0008—Organic ingredients according to more than one of the "one dot" groups of C08K5/01 - C08K5/59
- C08K5/0058—Biocides
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08K5/00—Use of organic ingredients
- C08K5/36—Sulfur-, selenium-, or tellurium-containing compounds
- C08K5/45—Heterocyclic compounds having sulfur in the ring
- C08K5/46—Heterocyclic compounds having sulfur in the ring with oxygen or nitrogen in the ring
- C08K5/47—Thiazoles
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/53—Phosphorus bound to oxygen bound to oxygen and to carbon only
- C08K5/5317—Phosphonic compounds, e.g. R—P(:O)(OR')2
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Abstract
The invention provides a preservative for aqueous polyurethane emulsion and a preparation method thereof, wherein the preservative comprises the following components in percentage by mass: 2-15 parts of 1, 2-benzisothiazolin-3-one, 2-15 parts of 2-methyl-4-isothiazolin-3-one, 0.5-6 parts of an alkali substance, 0.1-2 parts of a stabilizer A, 0.1-2 parts of a stabilizer B and 60-96 parts of water. The preservative is prepared by mixing isothiazolinone substances, a stabilizer, an alkaline substance and water in a certain order and compounding. The product does not contain the forbidden substances specified by the current domestic and foreign laws and standards, does not contain organic solvents, does not crosslink emulsion, has broad antibacterial spectrum and good compatibility with waterborne polyurethane emulsion. The water-based polyurethane emulsion is used in the emulsification process of the polyurethane prepolymer, and can prevent the water-based polyurethane emulsion from being corroded by microorganisms in the storage process.
Description
[ technical field ] A method for producing a semiconductor device
The invention relates to the technical field of sterilization and mildew prevention, in particular to a preservative for aqueous polyurethane emulsion and a preparation method thereof.
[ background of the invention ]
The waterborne polyurethane refers to a polyurethane product which takes water as a dispersion medium instead of an organic solvent, and the appearance of the polyurethane product is usually in a semitransparent or opaque emulsion state. Waterborne polyurethane is an important direction for the development of polyurethane industry, is widely used as a coating, an adhesive, a fabric coating and finishing agent, a leather finishing agent, a paper surface treating agent and a fiber surface treating agent at present, and has a wide application prospect in multiple industrial fields.
However, since aqueous polyurethane emulsions are generally ionic, the emulsions are generally weakly basic (pH 7.0 to 9.0). The pH range provides favorable conditions for breeding of bacteria and yeasts, so that the waterborne polyurethane emulsion can be decomposed by microorganisms in the storage and transportation process, and the quality problems of layering, deterioration, smelliness and the like of the emulsion are caused. Therefore, the emulsion needs to be preserved by using a specific measure to ensure the stability of the product quality.
The added preservative is the simplest and most effective mode for inhibiting the breeding of microorganisms in the emulsion (Schogwen et al, waterborne polyurethane materials, chemical industry Press, 2010, 122-124). among the preservatives used at present, isothiazolinone substances are the most widely (Wang Lei et al, application research of isothiazolinone bactericides, industrial microorganisms, 2015,5: 60-64). however, the preservative for the waterborne polyurethane emulsion meets the following requirements that ① does not contain divalent or high-valent cations so as to avoid emulsion crosslinking, ② does not contain organic solvents so as not to increase the content of volatile organic matters in the emulsion and not to influence the film forming performance of the emulsion, ③ has good stability and no decomposition of effective components under weak alkaline conditions, ④ has good high-temperature resistance, does not decompose during high-temperature curing after the emulsion is formed and is embedded in the emulsion to form durable antibacterial performance, ⑤ has good antibacterial performance and low cost, and raw materials are easy to obtain.
[ summary of the invention ]
The invention aims to solve the problems in the prior art, provides a preservative for aqueous polyurethane emulsion and a preparation method thereof, and can solve the problems of deterioration, layering, peculiar smell and the like of the aqueous polyurethane emulsion possibly caused by microbial corrosion in the storage and transportation process.
In order to achieve the purpose, the invention provides a preservative for aqueous polyurethane emulsion, which comprises the following components in percentage by mass: 2-15 parts of 1, 2-benzisothiazolin-3-one, 2-15 parts of 2-methyl-4-isothiazolin-3-one, 0.5-6 parts of an alkali substance, 0.1-2 parts of a stabilizer A, 0.1-2 parts of a stabilizer B and 60-96 parts of water.
Preferably, the mass ratio of each component is as follows: 4-6 parts of 1, 2-benzisothiazolin-3-one, 4-6 parts of 2-methyl-4-isothiazolin-3-one, 1-2 parts of alkali substances, 0.1-0.5 part of stabilizer A, 0.1-0.5 part of stabilizer B and 85-91 parts of water.
Preferably, the 1, 2-benzisothiazolin-3-one is selected from a powdery substance or a liquid after dissolving.
Preferably, the 2-methyl-4-isothiazolin-3-one is selected from a powdery substance or a liquid in which the powdery substance is dissolved.
Preferably, the alkali substance can be sodium hydroxide or potassium hydroxide.
Preferably, the stabilizer A can be one of ethylenediamine tetraacetic acid or a sodium salt thereof, hydroxyethylidene diphosphonic acid or a sodium salt thereof.
Preferably, the 1, 2-benzisothiazolin-3-one is a powdery substance with the mass percentage of not less than 85%; the 2-methyl-4-isothiazoline-3-ketone is a liquid substance with the mass percentage of not less than 50 percent; the alkali substance is potassium hydroxide with the mass percentage content not lower than 95%; the stabilizer A is hydroxyethylidene diphosphonic acid with the mass percentage of not less than 98 percent.
Preferably, the stabilizer B is sodium nitrite with the mass percentage content of not less than 99%.
Preferably, the water is deionized water.
The invention also provides a preparation method of the preservative for the waterborne polyurethane emulsion, which sequentially comprises the following steps:
step a, accurately weighing the metered stabilizer A, adding the stabilizer A into the metered water, and stirring for 10-20 min at 40-50 rpm to fully dissolve the stabilizer A in the water.
And b, accurately weighing the metered 1, 2-benzisothiazolin-3-one, slowly adding the weighed 1, 2-benzisothiazolin-3-one into the solution obtained in the step a under the stirring condition of 40-50 rpm, and then stirring for 10-30 min under the stirring condition of 70-80 rpm.
And c, accurately weighing the metered alkali substances, adding the alkali substances into the solution obtained in the step b for 10-20 times under the condition of stirring at 40-50 rpm, wherein each time interval is 2-4 min, and stirring for 20-60 min under the condition of 70-80 rpm after the addition is finished.
And d, accurately weighing the metered 2-methyl-4-isothiazolin-3-one, slowly adding the weighed 2-methyl-4-isothiazolin-3-one into the solution obtained in the step c under the stirring condition of 40-50 rpm, and then stirring for 10-30 min under the stirring condition of 70-80 rpm.
And e, accurately weighing the metered stabilizer B, slowly adding the stabilizer B into the solution obtained in the step d under the stirring condition of 40-50 rpm, stirring at 40-50 rpm for 10-30 min after the addition is finished, standing for 1h, sampling, performing qualification detection on the product, filtering and packaging after the product is qualified, and thus obtaining a finished preservative.
Preferably, the temperature range of the preparation process in the steps a, b, c, d and e is 15-30 ℃.
In the invention, two substances, namely 1, 2-benzisothiazolin-3-one (BIT for short, chemical abstract number: 2634-33-5) and 2-methyl-4-isothiazolin-3-one (MIT for short, chemical abstract number: 2682-20-4), are used as effective components of the preservative, then proper auxiliary agents (cosolvent and stabilizer) are selected, and a water-based preparation with stable quality and excellent antibacterial performance is prepared by reasonable collocation of the components and optimization of processing conditions, so that the water-based polyurethane emulsion can be prevented from being corroded by microorganisms in the storage process.
The invention has the beneficial effects that:
(1) the preservative does not contain forbidden substances specified by current domestic and foreign laws and standards, has no Volatile Organic Compounds (VOC), no odor, no divalent salt and no crosslinking emulsion, is harmless under the use concentration and does not cause cumulative pollution to the environment.
(2) The preservative contains two preservative components of BIT and MIT, has broader-spectrum anti-mildew performance, is simple and convenient to use and has low cost.
The features and advantages of the present invention will be described in detail by way of examples.
[ detailed description ] embodiments
The present invention is described in detail below by way of examples, it should be noted that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention, and those skilled in the art can make many insubstantial modifications and adaptations of the present invention based on the above disclosure.
Example 1
The invention relates to a preservative for aqueous polyurethane emulsion, which comprises the following components in percentage by mass: 5.0 parts of 1, 2-benzisothiazolin-3-one, 5.0 parts of 2-methyl-4-isothiazolin-3-one, 1.65 parts of potassium hydroxide, 0.5 part of hydroxyethylidene diphosphonic acid, 0.2 part of sodium nitrite and 87.65 parts of water.
The preparation method of the preservative for the waterborne polyurethane emulsion sequentially comprises the following steps (the temperature of the preparation process is 15-30 ℃):
step a, accurately weighing the metered hydroxyethylidene diphosphonic acid, adding the weighed hydroxyethylidene diphosphonic acid into the metered water, and stirring for 15min at 40-50 rpm to fully dissolve the hydroxyethylidene diphosphonic acid in the water;
and b, accurately weighing the metered 1, 2-benzisothiazolin-3-one, slowly adding the weighed 1, 2-benzisothiazolin-3-one into the solution obtained in the step a under the stirring condition of 40-50 rpm, and then stirring for 20min under the stirring condition of 70-80 rpm.
And c, accurately weighing the metered potassium hydroxide, adding the potassium hydroxide into the solution obtained in the step b for 15 times under the stirring condition of 40-50 rpm, wherein the interval is 2min each time, and stirring for 40min under the condition of 70-80 rpm after the addition is finished.
And d, accurately weighing the metered 2-methyl-4-isothiazolin-3-one, slowly adding the weighed 2-methyl-4-isothiazolin-3-one into the solution obtained in the step c under the stirring condition of 40-50 rpm, and then stirring for 30min under the stirring condition of 70-80 rpm.
And e, accurately weighing the metered sodium nitrite, slowly adding the sodium nitrite into the solution obtained in the step d under the stirring condition of 40-50 rpm, continuously stirring for 20min under the condition of 40-50 rpm after the addition is finished, standing for 1h, sampling, carrying out qualification detection on the product, filtering and packaging after the product is qualified, and thus obtaining the finished preservative.
The product qualification detection indexes are as follows: the solution is colorless or light yellow and transparent, and the pH value is 8-9.
Example 2
The invention relates to a preservative for aqueous polyurethane emulsion, which comprises the following components in percentage by mass: 10.0 parts of 1, 2-benzisothiazolin-3-one, 10.0 parts of 2-methyl-4-isothiazolin-3-one, 3.4 parts of potassium hydroxide, 0.5 part of hydroxyethylidene diphosphonic acid, 0.2 part of sodium nitrite and 75.9 parts of water.
The preparation method and the product qualification test method of the preservative for the aqueous polyurethane emulsion are the same as those in example 1.
Example 3
The invention relates to a preservative for aqueous polyurethane emulsion, which comprises the following components in percentage by mass: 2.0 parts of 1, 2-benzisothiazolin-3-one, 2.0 parts of 2-methyl-4-isothiazolin-3-one, 3.5 parts of potassium hydroxide, 0.2 part of hydroxyethylidene diphosphonic acid, 0.9 part of sodium nitrite and 65 parts of deionized water.
The preparation method of the preservative for the waterborne polyurethane emulsion sequentially comprises the following steps (the temperature of the preparation process is 18-30 ℃):
step a, accurately weighing the measured hydroxyethylidene diphosphonic acid, adding the measured hydroxyethylidene diphosphonic acid into the measured water, and stirring for 15min at 40-50 rpm to fully dissolve the hydroxyethylidene diphosphonic acid in the water.
And b, accurately weighing the metered 1, 2-benzisothiazolin-3-one, slowly adding the weighed 1, 2-benzisothiazolin-3-one into the solution obtained in the step a under the stirring condition of 40-50 rpm, and then stirring for 15min at 70-80 rpm.
And c, accurately weighing the metered potassium hydroxide, adding the potassium hydroxide into the solution obtained in the step b for 15 times under the stirring condition of 40-50 rpm, wherein the interval is 2min each time, and stirring for 45min under the condition of 70-80 rpm after the addition is finished.
And d, accurately weighing the metered 2-methyl-4-isothiazolin-3-one, slowly adding the weighed 2-methyl-4-isothiazolin-3-one into the solution obtained in the step c under the condition of stirring at 40-50 rpm, and then stirring for 25min under the condition of 40-50 rpm.
And e, accurately weighing the metered sodium nitrite, slowly adding the sodium nitrite into the solution obtained in the step d under the stirring condition of 40-50 rpm, stirring for 18min at 40-50 rpm after the addition is finished, standing for 1h, sampling, carrying out qualification detection on the product, filtering and packaging after the product is qualified, and obtaining a finished preservative.
The product qualification detection indexes are as follows: the solution is colorless or light yellow and transparent, and the pH value is 8-9.
Example 4
The invention relates to a preservative for aqueous polyurethane emulsion, which comprises the following components in percentage by mass: 15.0 parts of 1, 2-benzisothiazolin-3-one, 15.0 parts of 2-methyl-4-isothiazolin-3-one, 5.0 parts of potassium hydroxide, 1.5 parts of hydroxyethylidene diphosphonic acid, 0.8 part of sodium nitrite and 92.5 parts of water.
The preparation method of the preservative for the waterborne polyurethane emulsion sequentially comprises the following steps (the temperature of the preparation process is 18-30 ℃):
step a, accurately weighing the metered hydroxyethylidene diphosphonic acid, adding the metered hydroxyethylidene diphosphonic acid into the metered water, and stirring for 20min at 40-50 rpm to fully dissolve the hydroxyethylidene diphosphonic acid in the water;
and b, accurately weighing the metered 1, 2-benzisothiazolin-3-one, slowly adding the weighed 1, 2-benzisothiazolin-3-one into the solution obtained in the step a under the stirring condition of 40-50 rpm, and then stirring for 25min under the stirring condition of 70-80 rpm.
And c, accurately weighing the metered potassium hydroxide, adding the potassium hydroxide into the solution obtained in the step b for 12 times under the stirring condition of 40-50 rpm, wherein the interval is 3min each time, and stirring for 45min under the condition of 70-80 rpm after the addition is finished.
And d, accurately weighing the metered 2-methyl-4-isothiazolin-3-one, slowly adding the weighed 2-methyl-4-isothiazolin-3-one into the solution obtained in the step c under the stirring condition of 40-50 rpm, and then stirring for 28min under the stirring condition of 40-50 rpm.
And e, accurately weighing the metered sodium nitrite, slowly adding the weighed sodium nitrite into the solution obtained in the step d under the stirring condition of 40-50 rpm, stirring for 25min under the stirring condition of 40-50 rpm after the addition is finished, standing for 1h, sampling, carrying out qualification detection on the product, filtering and packaging after the product is qualified, and thus obtaining the finished preservative.
The product qualification detection indexes are as follows: the solution is colorless or light yellow and transparent, and the pH value is 8-9.
The preservative for the aqueous polyurethane emulsion prepared by the invention has the following physicochemical characteristics: the appearance is colorless or light yellow and transparent, no odor exists, and the pH value is 8-9.
The preservative prepared by the invention is applied to the emulsification process of the aqueous polyurethane emulsion, and the dosage of the preservative is 0.05-0.2% of the total weight of the emulsion.
Description of the application: the preservative product is added when the polyurethane prepolymer is emulsified. Based on 0.05-0.2% of the total amount of the waterborne polyurethane emulsion to be processed, weighing the preservative product, adding the preservative product into water required by emulsification of a polyurethane prepolymer, and then performing subsequent processing according to an emulsification process of waterborne polyurethane to obtain a waterborne polyurethane product containing the preservative.
Determination of the Effect of application
The application effect of the preservative product is measured according to a coating culture method in GB/T30792-2014 test method for antimicrobial infection of in-tank water-based paint.
Weighing 2 parts of 100g of waterborne polyurethane sample containing the preservative (the dosage of the preservative is 0.05-0.2% of the total weight of the emulsion), respectively inoculating 1mL of bacterial suspension and 1mL of yeast suspension, fully and uniformly mixing, then storing at 30 +/-1 ℃, respectively measuring the quantity of bacteria and yeast in the sample on days 3, 5 and 7, and then grading based on the sum of the quantity of the bacteria and the quantity of the yeast. At the same time, comparative tests were carried out on samples of aqueous polyurethane without addition of preservatives. The test results are shown in table 1.
TABLE 1 results of antimicrobial grades
As can be seen from table 1, none of the aqueous polyurethane products to which the preservative was added was impregnated by microorganisms during the test (day 7 results are grade 0), showing good antimicrobial properties; the control was not preserved and the product was contaminated with microorganisms (day 5 results were grade 3). The preservative prepared by the invention is proved to be capable of solving the problems of deterioration, layering, peculiar smell and the like which can occur due to the corrosion of microorganisms in the storage and transportation process of the waterborne polyurethane emulsion.
Claims (10)
1. The preservative for the aqueous polyurethane emulsion is characterized by comprising the following components in parts by weight: comprises the following components in percentage by mass: 2-15 parts of 1, 2-benzisothiazolin-3-one, 2-15 parts of 2-methyl-4-isothiazolin-3-one, 0.5-6 parts of an alkali substance, 0.1-2 parts of a stabilizer A, 0.1-2 parts of a stabilizer B and 60-96 parts of water.
2. The preservative for aqueous polyurethane emulsions according to claim 1, which comprises: the mass ratio of each component is as follows: 4-6 parts of 1, 2-benzisothiazolin-3-one, 4-6 parts of 2-methyl-4-isothiazolin-3-one, 1-2 parts of alkali substances, 0.1-0.5 part of stabilizer A, 0.1-0.5 part of stabilizer B and 85-91 parts of water.
3. The preservative for aqueous polyurethane emulsions according to claim 1, which comprises: the 1, 2-benzisothiazolin-3-one is a powdery substance or a liquid substance dissolved by the powdery substance, and the mass percentage of the 1, 2-benzisothiazolin-3-one in the powdery substance is not less than 85%.
4. The preservative for aqueous polyurethane emulsions according to claim 1, which comprises: the 2-methyl-4-isothiazoline-3-ketone is a powdery substance or a liquid substance obtained by dissolving the powdery substance, and the mass percentage of the 2-methyl-4-isothiazoline-3-ketone in the liquid substance is not less than 50%.
5. The preservative for aqueous polyurethane emulsions according to claim 1, which comprises: the alkali substance is sodium hydroxide or potassium hydroxide, and the mass percentage of the potassium hydroxide is not less than 95%.
6. The preservative for aqueous polyurethane emulsions according to claim 1, which comprises: the stabilizer A is ethylene diamine tetraacetic acid or sodium salt thereof, hydroxyethylidene diphosphonic acid or sodium salt thereof, and the mass percentage content of the hydroxyethylidene diphosphonic acid is not less than 98%.
7. The preservative for aqueous polyurethane emulsions according to claim 1, which comprises: the stabilizer B is sodium nitrite, and the mass percentage of the sodium nitrite is not less than 99%.
8. The preservative for aqueous polyurethane emulsions according to claim 1, which comprises: the water is deionized water.
9. A method for producing the preservative for aqueous polyurethane emulsions according to any one of claims 1 to 8, characterized in that: the preparation process sequentially comprises the following steps:
step a, accurately weighing the metered stabilizer A, adding the stabilizer A into the metered water, and stirring for 10-20 min at 40-50 rpm to fully dissolve the stabilizer A in the water.
And b, accurately weighing the metered 1, 2-benzisothiazolin-3-one, slowly adding the weighed 1, 2-benzisothiazolin-3-one into the solution obtained in the step a under the stirring condition of 40-50 rpm, and then stirring for 10-30 min under the stirring condition of 70-80 rpm.
And c, accurately weighing the metered alkali substances, adding the alkali substances into the solution obtained in the step b for 10-20 times under the condition of stirring at 40-50 rpm, wherein each time interval is 2-4 min, and stirring for 20-60 min under the condition of 70-80 rpm after the addition is finished.
And d, accurately weighing the metered 2-methyl-4-isothiazolin-3-one, slowly adding the weighed 2-methyl-4-isothiazolin-3-one into the solution obtained in the step c under the condition of stirring at 40-50 rpm, and then stirring for 10-30 min under the condition of 40-50 rpm.
And e, accurately weighing the metered stabilizer B, slowly adding the stabilizer B into the solution obtained in the step d under the stirring condition of 40-50 rpm, continuously stirring for 10-30 min after the addition is finished, standing for 1h, sampling, carrying out qualification detection on the product, filtering and packaging after the product is qualified, and thus obtaining a finished preservative.
10. The method for preparing the preservative for the aqueous polyurethane emulsion according to claim 9, wherein the preservative comprises: the temperature range of the preparation process in the steps a, b, c, d and e is 15-30 ℃.
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| CN112030580A (en) * | 2020-08-28 | 2020-12-04 | 广州市珠之江环保印花材料实业有限公司 | High-fastness elastic suede foaming slurry and preparation method thereof |
| CN112608055A (en) * | 2020-10-23 | 2021-04-06 | 科之杰新材料集团福建有限公司 | Preservative composition and preparation method and application thereof |
| CN115872658A (en) * | 2022-12-23 | 2023-03-31 | 科之杰新材料集团有限公司 | Composite preservative for polycarboxylate superplasticizer and preparation method thereof |
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| CN112030580A (en) * | 2020-08-28 | 2020-12-04 | 广州市珠之江环保印花材料实业有限公司 | High-fastness elastic suede foaming slurry and preparation method thereof |
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