CN112522955A - Preparation method of environmentally-friendly and durable fabric antistatic agent - Google Patents
Preparation method of environmentally-friendly and durable fabric antistatic agent Download PDFInfo
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- CN112522955A CN112522955A CN202011393141.6A CN202011393141A CN112522955A CN 112522955 A CN112522955 A CN 112522955A CN 202011393141 A CN202011393141 A CN 202011393141A CN 112522955 A CN112522955 A CN 112522955A
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
- D06M15/65—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain containing epoxy groups
- D06M15/651—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain containing epoxy groups comprising carboxylic groups
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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
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/42—Block-or graft-polymers containing polysiloxane sequences
- C08G77/46—Block-or graft-polymers containing polysiloxane sequences containing polyether sequences
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/227—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of hydrocarbons, or reaction products thereof, e.g. afterhalogenated or sulfochlorinated
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/32—Polyesters
Abstract
The invention relates to the field of textile auxiliaries, in particular to a preparation method of an environment-friendly and durable fabric antistatic agent; according to the invention, high-hygroscopicity imidazole is introduced into the tail end of an acrylic polyoxyethylene ether molecule and then grafted on hydrogen-containing siloxane to prepare hydrophilic polyether silicone oil, and meanwhile, the hydrophilic polyether silicone oil and polyolefin wax grafted with polar group sodium acrylate are crosslinked under the action of a coupling agent, so that a high-molecular durable antistatic agent with polar groups and hydrophilic groups forms chemical bonds on the surface of a fabric under the actions of baking and ultraviolet light to form firm combination, and a long-acting antistatic effect is formed; the long-acting and durable antistatic agent has the characteristics of excellent performances, such as good antistatic performance, durable antistatic effect, washing resistance, good toughness, no influence of environmental humidity, small influence on the performance of a base material and the like, and is a polymer type ring long-time antistatic agent with good commercial prospect.
Description
Technical Field
The invention relates to the field of textile auxiliaries, in particular to a preparation method of an environment-friendly and durable fabric antistatic agent.
Background
Many textiles now contain a large amount of synthetic fibers, which have many superior properties to natural fibers, and thus have been rapidly developed and widely used in recent years. For example, the invention of polyester fiber in 1941 is a synthetic fiber spun by a fiber-forming polymer in which each chain unit in a macromolecular chain is connected through an ester group. However, many synthetic fibers are hydrophobic fibers, have poor conductivity and are poor conductors, and synthetic fibers have amorphous portions as cotton fibers, but lack moisture absorption centers, and have moisture absorption rates of only 0.6% to 0.8% even at 100% relative humidity. Therefore, static electricity is easily generated and dust is easily adsorbed, and static electricity is more easily accumulated. The obvious disadvantages of the material as the clothing material are strong static electricity and poor moisture absorption. In the spinning, weaving, printing and dyeing processes and even in the actual taking process, static electricity is generated, so that much inconvenience is brought to the spinning process, the wearing application and the like.
CN109371674A discloses a preparation method of a textile antistatic agent. The existing antistatic agent can be compounded with an eight-carbon fluorine-containing waterproof agent, but when the antistatic agent is compounded with a six-carbon fluorine-containing waterproof agent and a fluorine-free waterproof agent, the waterproof effect is greatly influenced. The main structure of the antistatic agent is short-chain fatty alcohol or phosphate monoester of fatty alcohol containing 2-3 hydroxyl groups, and the adopted preparation method comprises the following steps: firstly, short-chain fatty alcohol or fatty alcohol containing 2-3 hydroxyl groups reacts with a phosphorylation reagent, deionized water with the weight of 2-6% of that of a phosphorylation product is added for hydrolysis, then alkali is used for neutralization to obtain a phosphate product, and finally a chelating dispersant with the weight of 2-5% of that of the phosphate product is added for compounding to obtain a finished product; the chelating dispersant is prepared by reacting tristyrylphenol polyoxyethylene ether with gluconic acid, and the reaction temperature is 170-180 ℃. The antistatic agent can be compounded with six-carbon fluorine-containing waterproof agent, fluorine-free waterproof agent and silicone oil, has little influence on the waterproof effect and the hand feeling of the silicone oil, and has excellent antistatic performance.
CN103668971A relates to a special antistatic finishing agent for textiles, which is mainly used for the antistatic after-finishing process of artificial and natural fiber textiles, so that the textiles have the characteristics of antistatic property, static elimination, antibiosis and dust prevention. Has the advantages of simple preparation, convenient use, permanent antistatic property, water washing resistance, no irritation and no toxic or side effect.
CN103668941A provides an antistatic nano finishing agent for rabbit hair textiles and a finishing process. The finishing agent takes nano ZnO as a main component and takes a green and safe surfactant as an auxiliary component, ensures the specific appearance quality and performance of the rabbit hair fiber on the basis of excellent biocompatibility and environmental friendliness, and particularly shows incomparable advantages on the performances of antistatic effect, ultraviolet protection, antibiosis, bacteriostasis and the like. The optimized finishing process not only ensures that the nano finishing agent is well attached to the surface of the fiber when acting with rabbit hair textiles, is filled to the included angle of the scales and even the medullary cavity, and interacts with the fiber to generate valence bond combination to form a continuous and stable functional nano film, so that the finished rabbit hair textiles have antistatic, ultraviolet-proof, antibacterial and bacteriostatic properties and good mechanical properties, but also are convenient to operate and suitable for industrial use and popularization.
The principle of antistatic finishing is to form a highly conductive layer on the surface of the fibers. The antistatic agent can endow the surfaces of the fibers and the resin with certain hygroscopicity and ionicity, so that the conductivity is improved, and the antistatic purpose is achieved; however, the antistatic finishing agent prepared by the technology is easy to migrate on the surface of the fabric, and the antistatic effect is easy to lose after a long time.
Disclosure of Invention
In order to solve the problems, the invention provides a preparation method of an environment-friendly and durable fabric antistatic agent.
A preparation method of an environment-friendly and durable fabric antistatic agent comprises the following specific scheme:
adding 24-36 parts of acrylic acid polyoxyethylene ether, 5.2-8.6 parts of epoxy chloropropane, 0.6-1.8 parts of potassium hydroxide and 0.1-0.5 part of tetrabutylammonium bromide into 50-80 parts of organic solvent according to the mass parts, controlling the temperature to be 40-100 ℃, reacting for 5-10h, filtering after the reaction is finished, removing small molecules through reduced pressure distillation, adding into 60-100 parts of acetone, uniformly mixing, adding 2.4-6.2 parts of imidazole, heating to 40-60 ℃, reacting for 120-180min, and evaporating the solvent to obtain the epoxy acrylic acid polyoxyethylene ether;
uniformly mixing the obtained epoxy acrylic acid polyoxyethylene and 14-22 parts of hydrogen-containing siloxane, controlling the temperature to be 60-100 ℃, stirring for reaction for 30-120min, then adding 0.01-0.05 part of chloroplatinic acid, continuing to stir for reaction for 1-5h, then adding 2.8-6.7 parts of modified polyolefin wax, 0.2-0.8 part of epoxy siloxane and 0.01-0.04 part of catalyst, and reacting for 30-60min under the protection of nitrogen, thus obtaining the environment-friendly and durable fabric antistatic agent.
The preparation method of the modified polyolefin wax comprises the following steps:
according to the mass portion of the components,
1) adding 20-35 parts of polyolefin wax into 80-120 parts of toluene, uniformly mixing and stirring, heating to 85-100 ℃ under the protection of nitrogen, uniformly mixing 5.6-12.8 parts of acrylic acid, 1.2-3.6 parts of 4-vinylbenzoic acid, 0.1-0.5 part of vinyl phenyl sulfone, 0.01-0.05 part of 4-vinylpyridine-nickel and 0.2-0.7 part of benzoyl peroxide with 15-25 parts of toluene, adding 30-50% of the mixture into a reaction kettle, slowly adding the rest into the reaction kettle within 60-120min, continuously reacting for 60-180min, cooling, and distilling under reduced pressure for 40-60min to obtain the carboxylated polyolefin wax.
2) Adding 30-50 parts of carboxylated polyolefin wax into 30-50 parts of ethanol, dispersing at high speed for 30-50min, adding 2-10 parts of sodium hydroxide into a reaction kettle, controlling the temperature at 60-75 ℃, stirring for reaction for 10-30min, evaporating the solvent, precipitating the residual product in acetone, filtering, washing and drying to obtain the modified polyolefin wax.
The polyolefin wax is polyethylene wax or polypropylene wax.
The main reaction of the modified polyolefin wax is that the polyolefin wax and alkenyl acid containing unsaturated bonds and the like are subjected to free radical addition to obtain grafted carboxylated polyolefin wax, and then the grafted carboxylated polyolefin wax and alcohol base are subjected to salinization reaction with carboxyl to generate sodium carboxylate, namely the modified polyolefin wax is prepared. The main reaction formula can be shown as follows:
the average molecular weight of the acrylic polyoxyethylene ether is 2000-8000.
The epoxy siloxane is 1,1,3, 3-tetramethyl-1, 3 bis [3- (epoxy ethyl methoxy) propyl ] disiloxane, glycidyl propyl (dimethoxy) methylsilane or 3-glycidyl ether oxypropyltriethoxysilane.
The catalyst is sodium ethoxide or potassium hydroxide.
The organic solvent is dichloromethane or chloroform or toluene.
The application method of the environment-friendly and durable fabric antistatic agent comprises the following steps: preparing the antistatic agent into 0.5-2.5% aqueous solution finishing agent according to the mass parts, then dipping and binding the fabric in the finishing agent, drying for 5-10min at 60-100 ℃, and irradiating for 5-10s under ultraviolet light after drying to complete the antistatic treatment.
According to the preparation method of the environment-friendly durable fabric antistatic agent, high-hygroscopicity imidazole is introduced into the tail end of an acrylic polyoxyethylene ether molecule and then grafted on hydrogen-containing siloxane to prepare hydrophilic polyether silicone oil, and meanwhile, the hydrophilic polyether silicone oil and polyolefin wax grafted with polar group sodium acrylate are crosslinked under the action of a coupling agent, so that the high-molecular durable antistatic agent with polar groups and hydrophilic groups forms a chemical bond on the surface of a fabric under the actions of baking and ultraviolet light to form firm combination and a long-acting antistatic effect; the long-acting and durable antistatic agent has the characteristics of excellent performances, such as good antistatic performance, durable antistatic effect, washing resistance, good toughness, no influence of environmental humidity, small influence on the performance of a base material and the like, and is a polymer type ring long-time antistatic agent with good commercial prospect.
Drawings
FIG. 1 is a Fourier infrared spectrum of the polymeric ring type permanent antistatic agent prepared in example 3;
at 1728cm-1The absorption peak of ester carbonyl group is at 1052cm-1A symmetric telescopic absorption peak of ester carbon-oxygen single bond is present nearby and is 1133cm-1An antisymmetric telescopic absorption peak of ether bond existing nearby and is 2966cm-1The presence of a flexible absorption peak of carbon hydrogen nearby indicates that the epoxy acrylic acid polyoxyethylene and the modified polyThe olefin wax takes part in the reaction; at 1177/802cm-1The anti-symmetric stretching/symmetric stretching absorption peak of the silicon oxygen exists nearby, and is 670cm-1The existence of a stretching absorption peak of silicon carbon nearby indicates that the hydrogen-containing siloxane and the epoxy siloxane participate in the reaction.
Detailed Description
The invention is further illustrated by the following specific examples:
the antistatic agents prepared in the following examples and comparative examples are prepared into 0.5% aqueous solution finishing agent according to the mass parts, then polyester fabrics are soaked and pricked in the finishing agent, dried at 80 ℃ for 8min and irradiated under ultraviolet light for 5-10s after being dried; the YG321 type material specific resistance instrument is adopted for testing, and the test conditions are as follows: specific resistance values were tested at 25 ℃ and 40% humidity. The fabric was washed 10 times with a detergent under normal conditions and the specific resistance value was again measured, the less the specific resistance value increased, the better the durability of the antistatic effect.
Example 1
A preparation method of an environment-friendly and durable fabric antistatic agent comprises the following specific scheme:
adding 24g of acrylic acid polyoxyethylene ether, 5.2g of epoxy chloropropane, 0.6g of potassium hydroxide and 0.1g of tetrabutylammonium bromide into 50g of organic solvent according to the mass parts, controlling the temperature to be 40 ℃, reacting for 5 hours, filtering after the reaction is finished, removing small molecules through reduced pressure distillation, adding into 60g of acetone, uniformly mixing, adding 2.4g of imidazole, heating to 40 ℃, reacting for 120 minutes, and evaporating the solvent to obtain epoxy acrylic acid polyoxyethylene; and uniformly mixing the obtained epoxy acrylic acid polyoxyethylene and 14g of hydrogen-containing siloxane, controlling the temperature at 60 ℃, stirring for reaction for 30min, then adding 0.01g of chloroplatinic acid, continuing to stir for reaction for 1h, then adding 2.8g of modified polyolefin wax, 0.2g of epoxy siloxane and 0.01g of catalyst, and reacting for 30min under the protection of nitrogen, thus obtaining the environment-friendly and durable fabric antistatic agent.
The preparation method of the modified polyolefin wax comprises the following steps:
1) adding 20g of polyolefin wax into 120g of toluene, uniformly mixing and stirring, heating to 100 ℃ under the protection of nitrogen, uniformly mixing 12.8g of acrylic acid, 3.6g of 4-vinylbenzoic acid, 0.5g of vinyl phenyl sulfone, 0.01g of 4-vinylpyridine-nickel and 0.7g of benzoyl peroxide with 25g of toluene, adding 50% of the mixture into a reaction kettle, slowly adding the rest into the reaction kettle within 120min, continuously reacting for 60min, cooling, and distilling under reduced pressure for 60min to obtain the carboxylated polyolefin wax.
2) Adding 50g of 1) obtained carboxylated polyolefin wax into 50g of ethanol, dispersing at high speed for 30min, then adding 10g of sodium hydroxide into a reaction kettle, controlling the temperature at 60 ℃, stirring for reaction for 30min, evaporating the solvent, precipitating the residual product in acetone, filtering, washing and drying to obtain the modified polyolefin wax.
The polyolefin wax is polyethylene wax.
The average molecular weight of the acrylic polyoxyethylene ether is 2000.
The epoxy siloxane is 1,1,3, 3-tetramethyl-1, 3-bis [3- (epoxy ethyl methoxy) propyl ] disiloxane.
The catalyst is sodium ethoxide.
The organic solvent is dichloromethane.
Example 2
A preparation method of an environment-friendly and durable fabric antistatic agent comprises the following specific scheme:
adding 32g of acrylic acid polyoxyethylene ether, 7.2g of epoxy chloropropane, 1.2g of potassium hydroxide and 0.3g of tetrabutylammonium bromide into 60g of organic solvent according to the mass parts, controlling the temperature to be 60 ℃, reacting for 8 hours, filtering after the reaction is finished, removing small molecules through reduced pressure distillation, adding into 80g of acetone, uniformly mixing, adding 4.8g of imidazole, heating to 50 ℃, reacting for 150 minutes, and evaporating the solvent to obtain epoxy acrylic acid polyoxyethylene; and uniformly mixing the obtained epoxy acrylic acid polyoxyethylene and 18g of hydrogen-containing siloxane, controlling the temperature at 80 ℃, stirring for reaction for 80min, then adding 0.03g of chloroplatinic acid, continuing to stir for reaction for 3h, then adding 4.2g of modified polyolefin wax, 0.6g of epoxy siloxane and 0.04g of catalyst, and reacting for 40min under the protection of nitrogen, thus obtaining the environment-friendly and durable fabric antistatic agent.
The preparation method of the modified polyolefin wax comprises the following steps:
1) adding 35g of polyolefin wax into 80g of toluene, uniformly mixing and stirring, heating to 85 ℃ under the protection of nitrogen, uniformly mixing 5.6g of acrylic acid, 1.2g of 4-vinylbenzoic acid, 0.1g of vinyl phenyl sulfone, 0.05g of 4-vinylpyridine-nickel, 0.2g of benzoyl peroxide and 15g of toluene, adding 30% of the mixture into a reaction kettle, slowly adding the rest into the reaction kettle within 60min, continuously reacting for 180min, cooling, and distilling under reduced pressure for 40min to obtain the carboxylated polyolefin wax.
2) Adding 30g of 1) obtained carboxylated polyolefin wax into 30g of ethanol, dispersing at high speed for 50min, adding 2g of sodium hydroxide into a reaction kettle, controlling the temperature at 75 ℃, stirring for reaction for 10min, evaporating the solvent, precipitating the residual product in acetone, filtering, washing and drying to obtain the modified polyolefin wax.
The polyolefin wax is polypropylene wax.
The average molecular weight of the acrylic polyoxyethylene ether is 5000.
The epoxy siloxane is glycidol propyl (dimethoxy) methylsilane.
The catalyst is potassium hydroxide.
The organic solvent is chloroform.
Example 3
A preparation method of an environment-friendly and durable fabric antistatic agent comprises the following specific scheme:
according to the mass parts, 36g of acrylic acid polyoxyethylene ether, 8.6g of epoxy chloropropane, 1.8g of potassium hydroxide and 0.5g of tetrabutylammonium bromide are added into 80g of organic solvent, the temperature is controlled at 100 ℃, the reaction lasts for 10 hours, the mixture is filtered after the reaction is finished, the mixture is added into 100g of acetone after the micromolecules are removed by reduced pressure distillation, 6.2g of imidazole is added after the mixture is uniformly mixed, the mixture is heated to 60 ℃, the reaction lasts for 180 minutes, and the epoxy acrylic acid polyoxyethylene is obtained after the solvent is evaporated; and uniformly mixing the obtained epoxy acrylic acid polyoxyethylene and 22g of hydrogen-containing siloxane, controlling the temperature to be 100 ℃, stirring for reaction for 120min, then adding 0.05g of chloroplatinic acid, continuing to stir for reaction for 5h, then adding 6.7g of modified polyolefin wax, 0.8g of epoxy siloxane and 0.04g of catalyst, and reacting for 60min under the protection of nitrogen, thus obtaining the environment-friendly and durable fabric antistatic agent.
The preparation method of the modified polyolefin wax comprises the following steps:
1) adding 25g of polyolefin wax into 100g of toluene, uniformly mixing and stirring, heating to 90 ℃ under the protection of nitrogen, uniformly mixing 7.5g of acrylic acid, 2.4g of 4-vinylbenzoic acid, 0.3g of vinyl phenyl sulfone, 0.03g of 4-vinylpyridine-nickel and 0.4g of benzoyl peroxide with 20g of toluene, adding 40% of the mixture into a reaction kettle, slowly adding the rest into the reaction kettle within 90min, continuously reacting for 120min, cooling, and distilling under reduced pressure for 55min to obtain the carboxylated polyolefin wax.
2) 40g of carboxylated polyolefin wax obtained in the step 1) is added into 40g of ethanol for high-speed dispersion for 45min, then 7g of sodium hydroxide is added into a reaction kettle, the temperature is controlled at 66 ℃, the mixture is stirred for reaction for 25min, the solvent is evaporated, the residual product is precipitated in acetone, and the modified polyolefin wax is obtained after filtration, washing and drying.
The polyolefin wax is polyethylene wax.
The average molecular weight of the acrylic polyoxyethylene ether is 8000.
The epoxy siloxane is 3-glycidyl ether oxypropyl triethoxysilane.
The catalyst is potassium hydroxide.
The organic solvent is toluene.
The performance results of the polyester fabrics corresponding to the antistatic agents prepared in the above examples are shown in the following table:
| specific resistance value (omega/cm) | Increase in specific resistance value (%) | |
| Untreated nylon fabric | 4.21×1016 | -- |
| Example 1 | 8.27×109 | 0.24 |
| Example 2 | 7.48×109 | 0.18 |
| Example 3 | 7.19×109 | 0.16 |
Comparative example 1
A preparation method of an environment-friendly and durable fabric antistatic agent comprises the following specific scheme:
according to the weight portion, 24g of acrylic polyoxyethylene ether and 14g of hydrogen-containing siloxane are uniformly mixed, the temperature is controlled at 60 ℃, the mixture is stirred and reacts for 30min, then 0.01g of chloroplatinic acid is added, the mixture is continuously stirred and reacts for 1h, then 2.8g of modified polyolefin wax, 0.2g of epoxy siloxane and 0.01g of catalyst are added, and the mixture reacts for 30min under the protection of nitrogen, so that the environment-friendly and durable fabric antistatic agent can be obtained.
The preparation method of the modified polyolefin wax comprises the following steps:
1) adding 20g of polyolefin wax into 120g of toluene, uniformly mixing and stirring, heating to 100 ℃ under the protection of nitrogen, uniformly mixing 12.8g of acrylic acid, 3.6g of 4-vinylbenzoic acid, 0.5g of vinyl phenyl sulfone, 0.01g of 4-vinylpyridine-nickel and 0.7g of benzoyl peroxide with 25g of toluene, adding 50% of the mixture into a reaction kettle, slowly adding the rest into the reaction kettle within 120min, continuously reacting for 60min, cooling, and distilling under reduced pressure for 60min to obtain the carboxylated polyolefin wax.
2) Adding 50g of 1) obtained carboxylated polyolefin wax into 50g of ethanol, dispersing at high speed for 30min, then adding 10g of sodium hydroxide into a reaction kettle, controlling the temperature at 60 ℃, stirring for reaction for 30min, evaporating the solvent, precipitating the residual product in acetone, filtering, washing and drying to obtain the modified polyolefin wax.
The polyolefin wax is polyethylene wax.
The average molecular weight of the acrylic polyoxyethylene ether is 2000.
The epoxy siloxane is 1,1,3, 3-tetramethyl-1, 3-bis [3- (epoxy ethyl methoxy) propyl ] disiloxane.
The catalyst is sodium ethoxide.
The organic solvent is dichloromethane.
Comparative example 2
A preparation method of an environment-friendly and durable fabric antistatic agent comprises the following specific scheme:
adding 24g of acrylic acid polyoxyethylene ether, 5.2g of epoxy chloropropane, 0.6g of potassium hydroxide and 0.1g of tetrabutylammonium bromide into 50g of organic solvent according to the mass parts, controlling the temperature to be 40 ℃, reacting for 5 hours, filtering after the reaction is finished, removing small molecules through reduced pressure distillation, adding into 60g of acetone, uniformly mixing, adding 2.4g of imidazole, heating to 40 ℃, reacting for 120 minutes, and evaporating the solvent to obtain epoxy acrylic acid polyoxyethylene; and uniformly mixing the obtained epoxy acrylic acid polyoxyethylene and 14g of hydrogen-containing siloxane, controlling the temperature at 60 ℃, stirring for reaction for 30min, then adding 0.01g of chloroplatinic acid, continuing to stir for reaction for 1h, then adding 2.8g of polyolefin wax, 0.2g of epoxy siloxane and 0.01g of catalyst, and reacting for 30min under the protection of nitrogen, thus obtaining the environment-friendly and durable fabric antistatic agent.
The polyolefin wax is polyethylene wax.
The average molecular weight of the acrylic polyoxyethylene ether is 2000.
The epoxy siloxane is 1,1,3, 3-tetramethyl-1, 3-bis [3- (epoxy ethyl methoxy) propyl ] disiloxane.
The catalyst is sodium ethoxide.
The organic solvent is dichloromethane.
Comparative example 3
A preparation method of an environment-friendly and durable fabric antistatic agent comprises the following specific scheme:
adding 24g of acrylic acid polyoxyethylene ether, 5.2g of epoxy chloropropane, 0.6g of potassium hydroxide and 0.1g of tetrabutylammonium bromide into 50g of organic solvent according to the mass parts, controlling the temperature to be 40 ℃, reacting for 5 hours, filtering after the reaction is finished, removing small molecules through reduced pressure distillation, adding into 60g of acetone, uniformly mixing, adding 2.4g of imidazole, heating to 40 ℃, reacting for 120 minutes, and evaporating the solvent to obtain epoxy acrylic acid polyoxyethylene; uniformly mixing the obtained epoxy acrylic acid polyoxyethylene and 14g of hydrogen-containing siloxane, controlling the temperature at 60 ℃, stirring for reaction for 30min, then adding 0.01g of chloroplatinic acid, continuing to stir for reaction for 1h, then adding 2.8g of modified polyolefin wax and 0.01g of catalyst, and reacting for 30min under the protection of nitrogen, thus obtaining the environment-friendly and durable fabric antistatic agent.
The polyolefin wax is polyethylene wax.
The average molecular weight of the acrylic polyoxyethylene ether is 2000.
The catalyst is sodium ethoxide.
The organic solvent is dichloromethane.
The performance results of the polyester fabrics corresponding to the antistatic agents prepared in the above examples are shown in the following table:
| specific resistance value(Ω/cm) | Increase in specific resistance value (%) | |
| Comparative example 1 | 2.4×1011 | 2.64 |
| Comparative example 2 | 8.3×1010 | 1.87 |
| Comparative example 3 | 4.8×1010 | 8.47 |
Claims (8)
1. A preparation method of an environment-friendly and durable fabric antistatic agent comprises the following specific scheme:
adding 24-36 parts of acrylic acid polyoxyethylene ether, 5.2-8.6 parts of epoxy chloropropane, 0.6-1.8 parts of potassium hydroxide and 0.1-0.5 part of tetrabutylammonium bromide into 50-80 parts of organic solvent according to the mass parts, controlling the temperature to be 40-100 ℃, reacting for 5-10h, filtering after the reaction is finished, removing small molecules through reduced pressure distillation, adding into 60-100 parts of acetone, uniformly mixing, adding 2.4-6.2 parts of imidazole, heating to 40-60 ℃, reacting for 120-180min, and evaporating the solvent to obtain epoxy acrylic acid polyoxyethylene; uniformly mixing the obtained epoxy acrylic acid polyoxyethylene and 14-22 parts of hydrogen-containing siloxane, controlling the temperature to be 60-100 ℃, stirring for reaction for 30-120min, then adding 0.01-0.05 part of chloroplatinic acid, continuing to stir for reaction for 1-5h, then adding 2.8-6.7 parts of modified polyolefin wax, 0.2-0.8 part of epoxy siloxane and 0.01-0.04 part of catalyst, and reacting for 30-60min under the protection of nitrogen, thus obtaining the environment-friendly and durable fabric antistatic agent.
2. The method for preparing the environmentally friendly and durable fabric antistatic agent according to claim 1, wherein the method comprises the following steps: the preparation method of the modified polyolefin wax comprises the following steps:
according to the mass portion of the components,
1) adding 20-35 parts of polyolefin wax into 80-120 parts of toluene, uniformly mixing and stirring, heating to 85-100 ℃ under the protection of nitrogen, uniformly mixing 5.6-12.8 parts of acrylic acid, 1.2-3.6 parts of 4-vinylbenzoic acid, 0.1-0.5 part of vinyl phenyl sulfone, 0.01-0.05 part of 4-vinylpyridine-nickel and 0.2-0.7 part of benzoyl peroxide with 15-25 parts of toluene, adding 30-50% of the mixture into a reaction kettle, slowly adding the rest into the reaction kettle within 60-120min, continuously reacting for 60-180min, cooling, and distilling under reduced pressure for 40-60min to obtain carboxylated polyolefin wax;
2) adding 30-50 parts of carboxylated polyolefin wax into 30-50 parts of ethanol, dispersing at high speed for 30-50min, adding 2-10 parts of sodium hydroxide into a reaction kettle, controlling the temperature at 60-75 ℃, stirring for reaction for 10-30min, evaporating the solvent, precipitating the residual product in acetone, filtering, washing and drying to obtain the modified polyolefin wax.
3. The method for preparing the environmentally friendly and durable fabric antistatic agent according to claim 2, wherein the method comprises the following steps: the polyolefin wax is polyethylene wax or polypropylene wax.
4. The method for preparing the environmentally friendly and durable fabric antistatic agent according to claim 1, wherein the method comprises the following steps: the average molecular weight of the acrylic polyoxyethylene ether is 2000-8000.
5. The method for preparing the environmentally friendly and durable fabric antistatic agent according to claim 1, wherein the method comprises the following steps: the epoxy siloxane is 1,1,3, 3-tetramethyl-1, 3 bis [3- (epoxy ethyl methoxy) propyl ] disiloxane, glycidyl propyl (dimethoxy) methylsilane or 3-glycidyl ether oxypropyltriethoxysilane.
6. The method for preparing the environmentally friendly and durable fabric antistatic agent according to claim 1, wherein the method comprises the following steps: the catalyst is sodium ethoxide or potassium hydroxide.
7. The method for preparing the environmentally friendly and durable fabric antistatic agent according to claim 1, wherein the method comprises the following steps: the organic solvent is dichloromethane or chloroform or toluene.
8. The method for preparing the environmentally friendly and durable fabric antistatic agent according to claim 1, wherein the method comprises the following steps: the application method of the environment-friendly and durable fabric antistatic agent comprises the following steps: preparing the antistatic agent into 0.5-2.5% aqueous solution finishing agent according to the mass parts, then dipping and binding the fabric in the finishing agent, drying for 5-10min at 60-100 ℃, and irradiating for 5-10s under ultraviolet light after drying to complete the antistatic treatment.
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| CN114083853A (en) * | 2021-11-12 | 2022-02-25 | 江苏冠之星管道系统有限公司 | Light power cable reinforced protective sleeve and preparation method thereof |
| CN114182433A (en) * | 2021-12-06 | 2022-03-15 | 江苏金太阳纺织科技股份有限公司 | Preparation method of modified cotton wadding |
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| US20050049360A1 (en) * | 2003-08-29 | 2005-03-03 | Tokiko Okamoto | Antistatic resin composition |
| CN103214629A (en) * | 2013-05-09 | 2013-07-24 | 苏州大学 | Antistatic agent for dacron textile and preparation method of antistatic agent |
| CN109371674A (en) * | 2018-09-11 | 2019-02-22 | 杭州传化精细化工有限公司 | A kind of preparation method of textile antistatic agent |
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| US20050049360A1 (en) * | 2003-08-29 | 2005-03-03 | Tokiko Okamoto | Antistatic resin composition |
| CN103214629A (en) * | 2013-05-09 | 2013-07-24 | 苏州大学 | Antistatic agent for dacron textile and preparation method of antistatic agent |
| CN109371674A (en) * | 2018-09-11 | 2019-02-22 | 杭州传化精细化工有限公司 | A kind of preparation method of textile antistatic agent |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114083853A (en) * | 2021-11-12 | 2022-02-25 | 江苏冠之星管道系统有限公司 | Light power cable reinforced protective sleeve and preparation method thereof |
| CN114182433A (en) * | 2021-12-06 | 2022-03-15 | 江苏金太阳纺织科技股份有限公司 | Preparation method of modified cotton wadding |
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