CN111101232B - Preparation method of antibacterial spandex - Google Patents
Preparation method of antibacterial spandex Download PDFInfo
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- CN111101232B CN111101232B CN201911374857.9A CN201911374857A CN111101232B CN 111101232 B CN111101232 B CN 111101232B CN 201911374857 A CN201911374857 A CN 201911374857A CN 111101232 B CN111101232 B CN 111101232B
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/94—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of other polycondensation products
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/08—Processes
- C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4854—Polyethers containing oxyalkylene groups having four carbon atoms in the alkylene group
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6666—Compounds of group C08G18/48 or C08G18/52
- C08G18/667—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38
- C08G18/6681—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/32 or C08G18/3271 and/or polyamines of C08G18/38
- C08G18/6685—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/32 or C08G18/3271 and/or polyamines of C08G18/38 with compounds of group C08G18/3225 or polyamines of C08G18/38
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
- D01F1/103—Agents inhibiting growth of microorganisms
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Artificial Filaments (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention relates to a preparation method of antibacterial spandex, which comprises the following specific steps: reacting polytetramethylene ether glycol with 4, 4-diphenylmethane diisocyanate, adding N, N-dimethylacetamide for dilution, adding an N, N-dimethylacetamide solution in which 1, 2-propylene diamine, 1, 5-pentamethylene diamine and ethanolamine are dissolved for chain extension reaction and termination reaction, and adding a flatting agent, an antioxidant and an ultraviolet absorber to obtain a polyurethane stock solution; mixing and stirring the compound essential oil, sorbitol, menthol and cationic surfactant to obtain a green antibacterial agent; adding a green antibacterial agent into the polyurethane stock solution, and uniformly mixing to obtain an antibacterial spandex spinning solution; and (4) carrying out dry spinning after the antibacterial spandex spinning solution is cured to obtain the antibacterial spandex. By adding the green antibacterial agent, the spandex has excellent antibacterial effect on staphylococcus aureus, escherichia coli and candida albicans, and the cinnamon oil, the coleus oil and the blumea oil in the green antibacterial agent are matched with each other and act synergistically, so that the antibacterial effect is further improved.
Description
Technical Field
The invention relates to the field of preparation of spandex, in particular to a preparation method of antibacterial spandex.
Background
Spandex (spandex), which is one of the most elastic fibers in synthetic fibers, is called polyurethane elastic fiber and has the characteristics of high elasticity and high elongation. Spandex has gradually replaced traditional rubber filament products since the 21 st century, and is widely applied to the clothing and textile industry; the application fields include swimming clothes, silk stockings, diapers and the like.
With the development of science and technology, people can pursue more value characteristics of spandex besides characteristics of comfort, resilience and the like. Of these, spandex, which is functional against bacteria, is currently an important concern.
Disclosure of Invention
The invention aims to: provides a preparation method of antibacterial spandex.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of antibacterial spandex comprises the following specific steps:
s1: reacting polytetramethylene ether glycol and 4, 4-diphenylmethane diisocyanate at 65-70 ℃ for 55-65min, adding N, N-dimethylacetamide for dilution, adding an N, N-dimethylacetamide solution in which 1, 2-propylene diamine, 1, 5-pentamethylene diamine and ethanolamine are dissolved while stirring, carrying out chain extension reaction and termination reaction, and adding a flatting agent, an antioxidant and an ultraviolet absorber to obtain a polyurethane stock solution;
s2: mixing and stirring the compound essential oil, sorbitol, menthol and cationic surfactant to obtain a green antibacterial agent;
s3: adding a green antibacterial agent into the polyurethane stock solution, and uniformly mixing to obtain an antibacterial spandex spinning solution;
s4: and curing the antibacterial spandex spinning solution, and then carrying out dry spinning to obtain the antibacterial spandex.
Preferably, the molar ratio of polytetramethylene ether glycol to 4, 4-diphenylmethane diisocyanate in step S1 is from 1.6 to 1.9: 1.
Preferably, the molar ratio of the 1, 2-propanediamine, the 1, 5-pentanediamine and the ethanolamine in the step S1 is 4: 3: 2.
preferably, in step S1, the matting agent is titanium dioxide, the antioxidant is AT245, and the ultraviolet absorber is UV-320.
Preferably, the cationic surfactant described in step S2 is a polyquaternium.
Preferably, the complex essential oils in step S2 are cinnamon oil, coleus oil and argyi oil.
Preferably, the molar ratio of the cinnamon oil, the coleus oil and the wormwood oil in the compound essential oil in the step S2 is 1:1: 2.
Preferably, in the step S2, the molar ratio of the complex essential oil, sorbitol, menthol and cationic surfactant in the green antibacterial agent is 2-3: 0.1-0.3: 0.5-1:3-4.
Preferably, the addition amount of the green antibacterial agent in step S2 is 1.2-2.2% by mass of the polyurethane stock solution.
The invention has the beneficial effects that:
according to the invention, the green antibacterial agent is added into the polyurethane stock solution, so that the prepared spandex has excellent antibacterial effect on staphylococcus aureus, escherichia coli and candida albicans, and the cinnamon oil, the coleus oil and the blumea oil in the green antibacterial agent are mutually matched and act synergistically, so that the antibacterial effect is further improved.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
Example 1
A preparation method of antibacterial spandex comprises the following specific steps:
s1: polytetramethylene ether glycol (170g) and 4, 4-diphenylmethane diisocyanate (40g) were reacted at 68 ℃ for 60min, then N, N-dimethylacetamide (340g) was added to dilute the mixture, a solution of 1, 2-propanediamine (4.1g), 1, 5-pentanediamine (1.9g) and ethanolamine (0.4g) (100g) in N, N-dimethylacetamide (100g) was rapidly added with stirring to conduct chain extension and termination reactions, and then a delustering agent TiO was added 2 (1.5g), an antioxidant AT245(1.2g) and an anti-ultraviolet auxiliary agent UV-320(1g) to obtain a polyurethane stock solution;
s2: mixing and stirring the compound essential oil, sorbitol, menthol and polyquaternium to obtain a green antibacterial agent;
wherein the compound essential oil is cinnamon oil, coleus oil and blumea oil, and the molar ratio of the cinnamon oil to the coleus oil to the blumea oil is 1:1: 2; the molar ratio of the compound essential oil, the sorbitol, the menthol and the cationic surfactant in the green antibacterial agent is 2.5: 0.2: 0.8:3.2.
S3: adding a green antibacterial agent into the polyurethane stock solution, and uniformly mixing to obtain an antibacterial spandex spinning solution;
wherein the addition amount of the green antibacterial agent is 1.2 percent of the mass of the polyurethane stock solution;
s4: and curing the antibacterial spandex spinning solution, and then carrying out dry spinning to obtain the antibacterial spandex.
Example 2
A preparation method of antibacterial spandex comprises the following specific steps:
s1: polytetramethylene ether glycol (170g) and 4, 4-diphenylmethane diisocyanate (40g) were reacted at 68 ℃ for 60min, then N, N-dimethylacetamide (340g) was added to dilute the mixture, a solution of 1, 2-propanediamine (4.1g), 1, 5-pentanediamine (1.9g) and ethanolamine (0.4g) (100g) in N, N-dimethylacetamide (100g) was rapidly added with stirring to conduct chain extension and termination reactions, and then a delustering agent TiO was added 2 (1.5g), an antioxidant AT245(1.2g) and an anti-ultraviolet auxiliary agent UV-320(1g) to obtain a polyurethane stock solution;
s2: mixing and stirring the compound essential oil, sorbitol, menthol and polyquaternium to obtain a green antibacterial agent;
wherein the compound essential oil is cinnamon oil, coleus oil and blumea oil, and the molar ratio of the cinnamon oil to the coleus oil to the blumea oil is 1:1: 2; the molar ratio of the compound essential oil, the sorbitol, the menthol and the cationic surfactant in the green antibacterial agent is 2.5: 0.2: 0.8:3.2.
S3: adding a green antibacterial agent into the polyurethane stock solution, and uniformly mixing to obtain an antibacterial spandex spinning solution;
wherein the addition amount of the green antibacterial agent is 1.8 percent of the mass of the polyurethane stock solution;
s4: and curing the antibacterial spandex spinning solution, and then carrying out dry spinning to obtain the antibacterial spandex.
Example 3
A preparation method of antibacterial spandex comprises the following specific steps:
s1: 170g of polytetramethylene ether glycol and 40g of 4, 4-diphenylmethane diisocyanate react for 60min at 68 ℃, 340g N, N-dimethylacetamide is added for dilution, 100g N of N-dimethylacetamide solution in which 4.1g of 1, 2-propanediamine, 1.9g of 1, 5-pentanediamine and 0.4g of ethanolamine are dissolved is rapidly added while stirring, chain extension reaction and termination reaction are carried out, 21.5 g of flatting agent TiO21, 2.2 g of antioxidant AT2451 and 3201 g of ultraviolet resistance auxiliary agent UV-3201 are added, and polyurethane stock solution is obtained;
s2: mixing and stirring the compound essential oil, sorbitol, menthol and polyquaternium to obtain a green antibacterial agent;
wherein the compound essential oil is cinnamon oil, coleus oil and blumea oil, and the molar ratio of the cinnamon oil to the coleus oil to the blumea oil is 1:1: 2; the molar ratio of the compound essential oil, the sorbitol, the menthol and the cationic surfactant in the green antibacterial agent is 2.5: 0.2: 0.8:3.2.
S3: adding a green antibacterial agent into the polyurethane stock solution, and uniformly mixing to obtain an antibacterial spandex spinning solution;
wherein the addition amount of the green antibacterial agent is 2.2 percent of the mass of the polyurethane stock solution;
s4: and curing the antibacterial spandex spinning solution, and then carrying out dry spinning to obtain the antibacterial spandex.
Comparative example 1
A preparation method of antibacterial spandex comprises the following specific steps:
s1: polytetramethylene ether glycol (170g) and 4, 4-diphenylmethane diisocyanate (40g) were reacted at 68 ℃ for 60min, then N, N-dimethylacetamide (340g) was added to dilute the mixture, a solution of 1, 2-propanediamine (4.1g), 1, 5-pentanediamine (1.9g) and ethanolamine (0.4g) (100g) in N, N-dimethylacetamide (100g) was rapidly added with stirring to conduct chain extension and termination reactions, and then a delustering agent TiO was added 2 (1.5g), an antioxidant AT245(1.2g) and an anti-ultraviolet auxiliary agent UV-320(1g) to obtain a polyurethane stock solution;
s2: mixing oleum Cinnamomi, sorbitol, menthol, and polyquaternium, and stirring to obtain green antibacterial agent;
wherein the molar ratio of the cinnamon essential oil to the sorbitol to the menthol to the cationic surfactant is 2.5: 0.2: 0.8:3.2.
S3: adding a green antibacterial agent into the polyurethane stock solution, and uniformly mixing to obtain an antibacterial spandex spinning solution;
wherein, the addition amount of the green antibacterial agent is 1.8 percent of the mass of the polyurethane stock solution;
s4: and curing the antibacterial spandex spinning solution, and then carrying out dry spinning to obtain the antibacterial spandex.
Comparative example 2
Replacing cinnamon oil in the comparative example 1 with coleus oil, and the rest is the same as that in the comparative example 1; comparative example 3
The cinnamon oil of comparative example 1 was replaced with the argyi leaf oil, and the rest was the same as in comparative example 1.
The antibacterial spandex prepared by the method is subjected to an antibacterial test, and the specific process is as follows:
adding a certain amount of the prepared spandex into a triangular flask containing a test bacterium culture solution, sterilizing at high temperature and high pressure, cooling to room temperature, inoculating a test bacterium therein, ensuring that the bacterium solution is uniformly distributed on the spandex, plugging a plug to prevent volatilization, and measuring the bacterium concentration by a dilution plate method (at 37 ℃ for 24 hours). After the fiber and the test bacteria are contacted for a period of time, washing with phosphate buffer solution, after gradient dilution, taking a small amount of bacteria liquid, pouring the bacteria liquid on a nutrient agar plate, and measuring the concentration of the bacteria liquid of the residual viable bacteria in the triangular flask so as to test the antibacterial and bactericidal performance of the spandex.
The results obtained are as follows:
as can be seen from the above examples: the antibacterial spandex prepared by the method has excellent antibacterial performance, the optimal antibacterial rate on staphylococcus aureus, escherichia coli and candida albicans reaches more than 97%, and the following comparative examples show that: the antibacterial effect of the combination of the cinnamon oil, the coleus oil and the argy wormwood leaf oil is obviously better than that of the cinnamon oil, the coleus oil and the argy wormwood leaf oil which are used independently.
Claims (7)
1. A preparation method of antibacterial spandex is characterized by comprising the following specific steps:
s1: reacting polytetramethylene ether glycol and 4, 4-diphenylmethane diisocyanate at 65-70 ℃ for 55-65min, adding N, N-dimethylacetamide for dilution, adding an N, N-dimethylacetamide solution in which 1, 2-propylene diamine, 1, 5-pentamethylene diamine and ethanolamine are dissolved while stirring, carrying out chain extension reaction and termination reaction, and adding a flatting agent, an antioxidant and an ultraviolet absorber to obtain a polyurethane stock solution;
s2: mixing and stirring the compound essential oil, sorbitol, menthol and cationic surfactant to obtain a green antibacterial agent; wherein the compound essential oil is oleum Cinnamomi, Coleus oil and folium Artemisiae Argyi oil; the mol ratio of cinnamon oil, coleus oil and blumea oil in the compound essential oil is 1:1: 2;
s3: adding a green antibacterial agent into the polyurethane stock solution, and uniformly mixing to obtain an antibacterial spandex spinning solution;
s4: and curing the antibacterial spandex spinning solution, and then carrying out dry spinning to obtain the antibacterial spandex.
2. The method of claim 1, wherein the molar ratio of polytetramethylene ether glycol to 4, 4-diphenylmethane diisocyanate in step S1 is 1.6-1.9: 1.
3. The method for preparing antibacterial spandex according to claim 1, wherein the molar ratio of 1, 2-propanediamine, 1, 5-pentanediamine and ethanolamine in step S1 is 25: 4: 3.
4. the method of claim 1, wherein in step S1, the matting agent is titanium dioxide, the antioxidant is AT245, and the UV absorber is UV-320.
5. The method of claim 1, wherein the cationic surfactant in step S2 is a polyquaternium.
6. The method for preparing antibacterial spandex according to claim 1, wherein in step S2, the molar ratio of the complex essential oil, sorbitol, menthol and cationic surfactant in the green antibacterial agent is 2-3: 0.1-0.3: 0.5-1:3-4.
7. The method for preparing antibacterial spandex according to claim 1, wherein the addition amount of the green antibacterial agent in step S3 is 1.2-2.2% of the mass of the polyurethane stock solution.
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Families Citing this family (3)
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| CN112779626A (en) * | 2020-12-29 | 2021-05-11 | 宁夏宁东泰和新材有限公司 | Preparation method of photocatalytic composite antibacterial spandex |
| CN113666886B (en) * | 2021-08-26 | 2022-03-29 | 诸暨华海氨纶有限公司 | Antibacterial spandex fiber for diaper and preparation method thereof |
| CN113979894B (en) * | 2021-11-16 | 2023-06-23 | 北京工商大学 | Safe durable antibacterial natural textile material and preparation method thereof |
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| KR970006566A (en) * | 1995-07-14 | 1997-02-21 | 박홍기 | Manufacturing method of polyurethane elastic fiber with excellent antibacterial and deodorizing property |
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