CN108252104B - Preparation method of textile smoothing agent - Google Patents
Preparation method of textile smoothing agent Download PDFInfo
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- CN108252104B CN108252104B CN201711410071.9A CN201711410071A CN108252104B CN 108252104 B CN108252104 B CN 108252104B CN 201711410071 A CN201711410071 A CN 201711410071A CN 108252104 B CN108252104 B CN 108252104B
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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
- D06M15/647—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain containing polyether sequences
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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
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/77—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof
- D06M11/79—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof with silicon dioxide, silicic acids or their salts
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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
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/244—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus
- D06M13/248—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus with compounds containing sulfur
- D06M13/256—Sulfonated compounds esters thereof, e.g. sultones
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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
- D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
- D06M15/03—Polysaccharides or derivatives thereof
- D06M15/05—Cellulose or derivatives thereof
- D06M15/09—Cellulose ethers
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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
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/50—Modified hand or grip properties; Softening compositions
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- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention discloses a preparation method of a textile smoothing agent, and belongs to the field of textile additives. The invention also adds polydimethylsiloxane to carry out graft modification on the surface of the nano silicon dioxide and add the nano silicon dioxide into the emulsion, and the polydimethylsiloxane is coated on the surface of the nano carbon dioxide in a silicon-oxygen bond mode, so that the organic components on the surface of particles are increased, the content of hydroxyl on the surface of the particles is reduced, the electronegativity is reduced, the hydrophobic property of the particles is improved, and the defoaming and foam inhibiting properties are better, so that the problems of difficult emulsification and easy layering of the organic silicon are better solved. The invention solves the problems that the smoothing agent on the market at present belongs to an organic silicon soft smoothing agent, has common application effect, is easy to delaminate and has poor emulsion stability.
Description
Technical Field
The invention belongs to the field of textile additives, and particularly relates to a preparation method of a textile smoothing agent.
Background
The smoothing agent is a textile additive used in the textile industry, and can endow plush fabrics, leather fabrics and cotton fabrics with smooth hand feeling in the textile printing and dyeing industry, so that the textiles can become soft, smooth and bright. The water-based polyurethane resin is suitable for finished products of various fibers, has excellent glossiness, dry and wet rubbing resistance, flexibility, strong adhesive force, water resistance, stain resistance, fast drying, high and low temperature resistance, smooth and fine hand feeling, high solid content of some smoothing agents and good dispersibility, and can be diluted by water in any proportion, thereby effectively prolonging the shelf life. The smoothing agent can improve the glossiness of the fabric and endow the fabric with good smoothness and glossiness, so the smoothing agent is widely applied to the after finishing process of various fabrics and is the best choice of a new generation of high-grade textile softening finishing agent.
The textile smoothing agent in the market is mainly prepared by compounding dimethyl silicone oil, hydroxyl silicone oil, amino silicone oil and the like and then emulsifying, although the textile smoothing agent has a certain effect on fabrics, the textile smoothing agent has a common application effect, has the problems of easy delamination, poor emulsion stability and the like, and has high requirements on the environment. Therefore, it is necessary to produce a textile smoothing agent which is effective in use and is not easy to delaminate.
Disclosure of Invention
The technical problems to be solved by the invention are as follows: aiming at the problems that most smoothing agents on the market at present belong to organosilicon softening smoothing agents, the application effect is common, the layering is easy, and the emulsion stability is poor, the preparation method of the textile smoothing agent is provided.
In order to solve the technical problems, the invention adopts the following technical scheme:
a preparation method of a textile smoothing agent comprises the following steps:
(1) according to the weight parts, 10-15 parts of octamethylcyclotetrasiloxane, 5-6 parts of epoxy chloropropane, 2-3 parts of anhydrous stannic chloride and 1-2 parts of sodium hydroxide are taken, the octamethylcyclotetrasiloxane, the epoxy chloropropane and the anhydrous stannic chloride are mixed, the temperature is raised to 70-80 ℃, the temperature is kept for 5-6 hours, the sodium hydroxide is added for mixing when the temperature is reduced to 50-60 ℃, the mixture is stood, and reduced pressure distillation is carried out to obtain a distillate, wherein the mass ratio of the octamethylcyclotetrasiloxane to the epoxy chloropropane is 3-4: 5-6: 7-8, mixing the distillate, toluene and a sodium hydroxide solution, standing, and then carrying out reduced pressure distillation to obtain a distillate;
(2) taking 10-15 parts by weight of organic amine, 7-8 parts by weight of polyglycol ether, 5-6 parts by weight of distillate and 3-4 parts by weight of isopropanol, mixing the organic amine, the polyglycol ether and the isopropanol, stirring at the temperature of 45-50 ℃, heating to 80-90 ℃, dropwise adding the distillate, preserving heat at the temperature of 80-85 ℃ for 5-6 hours, and adjusting the pH value to 4-5 to obtain a heat preservation substance for later use;
(3) according to the mass ratio of 1: 2: 8-10, mixing ethyl orthosilicate, ammonia water and absolute ethyl alcohol, stirring at the temperature of 25-30 ℃, filtering to obtain filter residues, centrifugally washing the filter residues for 2-3 times by using ethanol, drying at the temperature of 35-40 ℃ to obtain a dried substance, putting 10-15 parts by weight of methanol, 5-6 parts by weight of deionized water, 3-4 parts by weight of polydimethylsiloxane, 3-4 parts by weight of ammonia water and 1-2 parts by weight of the dried substance into a container, stirring at the temperature of 50-65 ℃, adding ammonia water, refluxing, cooling to room temperature, centrifuging to obtain a precipitate, washing the precipitate for 3-4 times by using an ethanol solution, and drying at the temperature of 40-50 ℃ to obtain the dried substance;
(4) according to the weight parts, 20-30 parts of deionized water, 10-15 parts of the heat-insulating material for standby in the step (2), 7-8 parts of emulsifier, 1-2 parts of dry material, 0.5-0.8 part of hydroxymethyl cellulose, 0.1-0.2 part of catalyst and 0.1-0.2 part of formaldehyde are taken, the heat-insulating material for standby in the step (2), the emulsifier, the catalyst and the deionized water are mixed, the temperature is raised to 150-180 ℃, the mixture is stirred, the mixture is cooled to 50-60 ℃, the dry material, the hydroxymethyl cellulose and the formaldehyde are added, the mixture is stirred again and mixed uniformly, and the textile smoothing agent is obtained.
In the step (2), the organic amine is any one of hexamethylene diamine, N-diethyl propane diamine and ethanolamine.
In the step (4), the emulsifier is prepared by mixing the following raw materials in a mass ratio of 1: 1, uniformly mixing the dodecylbenzene sulfonic acid and the sorbitan monolaurate to obtain the emulsifier.
The catalyst in the step (4) is hydrochloric acid.
Compared with other methods, the method has the beneficial technical effects that:
(1) the invention utilizes the directional arrangement of amino groups in the whole molecule formed by combining polyether and siloxane, the polyether chain segment also increases the smoothness to a certain extent, the number of amino groups is large, the more the molecular positive charge is, the large binding capacity with fiber is realized, thus the smoothing agent not only has good film forming property on the surface of fiber and enables the fabric to have good hand feeling and smoothness, but also can permeate into the fabric to enable the fabric to have certain fluffiness and better hydrophilicity and air permeability, simultaneously, the solution of the smoothing agent contains free hydrogen ions under the catalysis of hydrochloric acid, the hydrogen ions are then attracted to the surface of emulsion particles to enable the surface of the emulsion particles to have positive charge, thereby effectively eliminating the floating oil phenomenon without layering, and then the polymerization is carried out under the combined action of anion and nonionic emulsifiers, the emulsion particles of the smoothing agent are basically anionic under the action of the emulsifiers, and the intramolecular and intermolecular of the emulsion particles are quite strong, in the chain initiation stage, hydrogen ions ionized from the dodecylbenzene sulfonic acid can be combined with the oxygen of siloxane, so that the bond energy of silicon-oxygen bonds is reduced, the silicon-oxygen bonds are weakened, the stability among latex particles is further improved, a uniform and stable emulsion system is obtained, and the problem that a smoothing agent is easy to break emulsion is solved.
(2) The invention also adds polydimethylsiloxane to carry out graft modification on the surface of the nano silicon dioxide and add the nano silicon dioxide into the emulsion, and the polydimethylsiloxane is coated on the surface of the nano carbon dioxide in a silicon-oxygen bond mode, so that the organic components on the surface of particles are increased, the content of hydroxyl on the surface of the particles is reduced, the electronegativity is reduced, the hydrophobic property of the particles is improved, and the defoaming and foam inhibiting properties are better, so that the problems of difficult emulsification and easy layering of the organic silicon are better solved.
Detailed Description
The organic amine is any one of hexamethylene diamine, N-diethyl propane diamine and ethanolamine.
The emulsifier is prepared from the following components in percentage by mass 1: 1, uniformly mixing the dodecylbenzene sulfonic acid and the sorbitan monolaurate to obtain the emulsifier.
The catalyst is hydrochloric acid.
A preparation method of a textile smoothing agent comprises the following steps:
(1) according to the weight parts, 10-15 parts of octamethylcyclotetrasiloxane, 5-6 parts of epoxy chloropropane, 2-3 parts of anhydrous stannic chloride and 1-2 parts of sodium hydroxide are taken, the octamethylcyclotetrasiloxane, the epoxy chloropropane and the anhydrous stannic chloride are mixed, the temperature is raised to 70-80 ℃, the temperature is kept for 5-6 hours, the sodium hydroxide is added for mixing when the temperature is reduced to 50-60 ℃, the mixture is kept still for 4-5 hours, and then reduced pressure distillation is carried out under the conditions that the vacuum degree is 13.3Pa and the temperature is 55-65 ℃ to obtain distillate, wherein the mass ratio of the octamethylcyclotetrasiloxane to the epoxy chloropropane is 3-4: 5-6: 7-8, mixing the distillate, toluene and a sodium hydroxide solution, standing for 1-2 hours, and then carrying out reduced pressure distillation under the conditions of vacuum degree of 13.3Pa and temperature of 55-65 ℃ to obtain a distillate;
(2) taking 10-15 parts by weight of organic amine, 7-8 parts by weight of polyglycol ether, 5-6 parts by weight of distillate and 3-4 parts by weight of isopropanol, mixing the organic amine, the polyglycol ether and the isopropanol, stirring for 1-2 hours at the temperature of 45-50 ℃ and 200-300 r/min, heating to 80-90 ℃, dropwise adding the distillate, preserving heat for 5-6 hours at the temperature of 80-85 ℃, and adjusting the pH value to 4-5 to obtain a heat preservation substance for later use;
(3) according to the mass ratio of 1: 2: 8-10, mixing tetraethoxysilane, ammonia water and absolute ethyl alcohol, stirring for 20-24 hours at the temperature of 25-30 ℃ and the speed of 600-800 r/min, filtering to obtain filter residues, centrifugally washing the filter residues with ethanol for 2-3 times, drying for 2-3 hours at the temperature of 35-40 ℃ to obtain dried substances, taking 10-15 parts by weight of methanol, 5-6 parts by weight of deionized water, 3-4 parts by weight of polydimethylsiloxane, 3-4 parts by weight of ammonia water and 1-2 parts by weight of dried substances, putting the methanol, the deionized water, the polydimethylsiloxane and the dried substances into a container, stirring for 30-40 minutes at the temperature of 50-65 ℃ and the speed of 200-300 r/min, adding the ammonia water, refluxing for 0.8-1 hour at the temperature of 70-80 ℃, cooling to room temperature, centrifuging for 3-5 minutes at the speed of 3000-4000 r/min to obtain precipitates, washing the precipitates with an ethanol solution for 3-4 times, drying at the temperature of 40-50 ℃ to obtain a dried substance;
(4) according to the weight parts, 20-30 parts of deionized water, 10-15 parts of the heat-insulating material for standby in the step (2), 7-8 parts of emulsifier, 1-2 parts of dry material, 0.5-0.8 part of hydroxymethyl cellulose, 0.1-0.2 part of catalyst and 0.1-0.2 part of formaldehyde are taken, the heat-insulating material for standby in the step (2), the emulsifier, the catalyst and the deionized water are mixed, the temperature is raised to 150-180 ℃, the mixture is stirred for 100-120 min at 700-800 r/min, the mixture is cooled to 50-60 ℃, the mixture is stirred for 8-10 min at the rotating speed of 4000-5000 r/min, the dry material, the hydroxymethyl cellulose and the formaldehyde are added, and then the mixture is stirred for 3-5 min at the rotating speed of 400-500 r/min, and the mixture is uniformly mixed, so that the textile smoothing agent is obtained.
Example 1
The organic amine is hexamethylenediamine.
The emulsifier is prepared from the following components in percentage by mass 1: 1, uniformly mixing the dodecylbenzene sulfonic acid and the sorbitan monolaurate to obtain the emulsifier.
The catalyst is hydrochloric acid.
A preparation method of a textile smoothing agent comprises the following steps:
(1) according to the weight parts, 10 parts of octamethylcyclotetrasiloxane, 5 parts of epichlorohydrin, 2 parts of anhydrous stannic chloride and 1 part of sodium hydroxide are taken, the octamethylcyclotetrasiloxane, the epichlorohydrin and the anhydrous stannic chloride are mixed, the temperature is raised to 70 ℃, the temperature is kept for 5 hours, the sodium hydroxide is added for mixing when the temperature is reduced to 50 ℃, the mixture is kept stand for 4 hours, and then the reduced pressure distillation is carried out under the conditions that the vacuum degree is 13.3Pa and the temperature is 55 ℃, so that a distillate is obtained, wherein the mass ratio of the octamethylcyclotetrasiloxane to the epichlorohydrin is 3: 5: 7, mixing the distillate, toluene and sodium hydroxide solution, standing for 1h, and then carrying out reduced pressure distillation under the conditions of vacuum degree of 13.3Pa and temperature of 55 ℃ to obtain distillate;
(2) taking 10 parts of organic amine, 7 parts of polyglycol ether, 5 parts of distillate and 3 parts of isopropanol according to parts by weight, mixing the organic amine, the polyglycol ether and the isopropanol, stirring at 45 ℃ and 200r/min for 1h, heating to 80 ℃, dropwise adding the distillate, preserving heat at 80 ℃ for 5h, and adjusting the pH value to 4 to obtain a heat preservation substance for later use;
(3) according to the mass ratio of 1: 2: 8, mixing tetraethoxysilane, ammonia water and absolute ethyl alcohol, stirring for 20 hours at the temperature of 25 ℃ and the temperature of 600r/min, filtering to obtain filter residue, centrifugally washing the filter residue for 2 times by using the ethanol, drying for 2 hours at the temperature of 35 ℃ to obtain a dried substance, taking 10 parts of methanol, 5 parts of deionized water, 3 parts of polydimethylsiloxane, 3 parts of ammonia water and 1 part of the dried substance according to parts by weight, putting the methanol, the deionized water, the polydimethylsiloxane and the dried substance into a container, stirring for 30 minutes at the temperature of 50 ℃ and the temperature of 200r/min, adding the ammonia water, refluxing for 0.8 hour at the temperature of 70 ℃, cooling to room temperature, centrifuging for 3 minutes at the temperature of 3000r/min to obtain a precipitate, washing the precipitate for 3 times by using an ethanol solution, and drying at the temperature of 40 ℃ to obtain the dried substance;
(4) according to the weight parts, 20 parts of deionized water, 10 parts of the heat-insulating material for standby in the step (2), 7 parts of emulsifier, 1 part of dry material, 0.5 part of hydroxymethyl cellulose, 0.1 part of catalyst and 0.1 part of formaldehyde are taken, the heat-insulating material for standby in the step (2), the emulsifier, the catalyst and the deionized water are mixed, the temperature is increased to 150 ℃, the mixture is stirred for 100min at 700r/min, the mixture is cooled to 50 ℃, the mixture is stirred for 8min at the rotating speed of 4000r/min, the dry material, the hydroxymethyl cellulose and the formaldehyde are added, the mixture is stirred for 3min at the rotating speed of 400r/min, and the textile smoothing agent is obtained after uniform mixing.
Example 2
The organic amine is N, N-diethylpropanediamine.
The emulsifier is prepared from the following components in percentage by mass 1: 1, uniformly mixing the dodecylbenzene sulfonic acid and the sorbitan monolaurate to obtain the emulsifier.
The catalyst is hydrochloric acid.
A preparation method of a textile smoothing agent comprises the following steps:
(1) taking 15 parts of octamethylcyclotetrasiloxane, 6 parts of epoxy chloropropane, 3 parts of anhydrous stannic chloride and 2 parts of sodium hydroxide, mixing the octamethylcyclotetrasiloxane, the epoxy chloropropane and the anhydrous stannic chloride, heating to 80 ℃, keeping the temperature for 6 hours, adding the sodium hydroxide for mixing when the temperature is reduced to 60 ℃, standing for 5 hours, and carrying out reduced pressure distillation under the conditions of vacuum degree of 13.3Pa and temperature of 65 ℃ to obtain a distillate, wherein the mass ratio of the octamethylcyclotetrasiloxane to the epoxy chloropropane to the anhydrous stannic chloride is 4: 6: 8, mixing the distillate, toluene and sodium hydroxide solution, standing for 2 hours, and then carrying out reduced pressure distillation under the conditions of vacuum degree of 13.3Pa and temperature of 65 ℃ to obtain distillate;
(2) taking 15 parts of organic amine, 8 parts of polyglycol ether, 6 parts of distillate and 4 parts of isopropanol according to parts by weight, mixing the organic amine, the polyglycol ether and the isopropanol, stirring at the temperature of 50 ℃ and 300r/min for 2 hours, heating to 90 ℃, dropwise adding the distillate, preserving heat at the temperature of 85 ℃ for 6 hours, and adjusting the pH value to 5 to obtain a heat preservation substance for later use;
(3) according to the mass ratio of 1: 2: 10, mixing tetraethoxysilane, ammonia water and absolute ethyl alcohol, stirring for 24 hours at the temperature of 30 ℃ and the temperature of 800r/min, filtering to obtain filter residue, centrifugally washing the filter residue for 3 times by using the ethanol, drying for 3 hours at the temperature of 40 ℃ to obtain a dried substance, taking 15 parts of methanol, 6 parts of deionized water, 4 parts of polydimethylsiloxane, 4 parts of ammonia water and 2 parts of the dried substance according to parts by weight, putting the methanol, the deionized water, the polydimethylsiloxane and the dried substance into a container, stirring for 40 minutes at the temperature of 65 ℃ and the temperature of 300r/min, adding the ammonia water, refluxing for 1 hour at the temperature of 80 ℃, cooling to the room temperature, centrifuging for 5 minutes at the temperature of 4000r/min to obtain a precipitate, washing the precipitate for 4 times by using an ethanol solution, and drying at the temperature of 50 ℃ to obtain the dried substance;
(4) according to the weight parts, 30 parts of deionized water, 15 parts of the heat-insulating material for standby in the step (2), 8 parts of emulsifier, 2 parts of dry material, 0.8 part of hydroxymethyl cellulose, 0.2 part of catalyst and 0.2 part of formaldehyde are taken, the heat-insulating material for standby in the step (2), the emulsifier, the catalyst and the deionized water are mixed, the temperature is increased to 180 ℃, the mixture is stirred for 120 min at the speed of 800r/min, the mixture is cooled to 60 ℃, the mixture is stirred for 10min at the speed of 5000r/min, the dry material, the hydroxymethyl cellulose and the formaldehyde are added, the mixture is stirred for 5min at the speed of 500r/min, and the textile smoothing agent is obtained after uniform mixing.
Example 3
The organic amine is ethanolamine.
The emulsifier is prepared from the following components in percentage by mass 1: 1, uniformly mixing the dodecylbenzene sulfonic acid and the sorbitan monolaurate to obtain the emulsifier.
The catalyst is hydrochloric acid.
A preparation method of a textile smoothing agent comprises the following steps:
(1) according to the weight parts, 12.5 parts of octamethylcyclotetrasiloxane, 5.5 parts of epichlorohydrin, 2.5 parts of anhydrous stannic chloride and 1.5 parts of sodium hydroxide are taken, the octamethylcyclotetrasiloxane, the epichlorohydrin and the anhydrous stannic chloride are mixed, the temperature is raised to 75 ℃, the temperature is kept for 5.5 hours, when the temperature is lowered to 55 ℃, sodium hydroxide is added for mixing, the mixture is kept stand for 4.5 hours, and then reduced pressure distillation is carried out under the conditions that the vacuum degree is 13.3Pa and the temperature is 60 ℃ to obtain a distillate, wherein the mass ratio of the octamethylcyclotetrasiloxane to the epichlorohydrin is 3.5: 5.5: 7.5, mixing the distillate, toluene and sodium hydroxide solution, standing for 1.5h, and then carrying out reduced pressure distillation under the conditions of vacuum degree of 13.3Pa and temperature of 60 ℃ to obtain distillate;
(2) taking 12.5 parts of organic amine, 7.5 parts of polyglycol ether, 5.5 parts of distillate and 3.5 parts of isopropanol, mixing the organic amine, the polyglycol ether and the isopropanol, stirring at 47 ℃ and 250r/min for 1.5 hours, heating to 85 ℃, dropwise adding the distillate, preserving heat at 83 ℃ for 5.5 hours, and adjusting the pH value to 4.5 to obtain a heat preservation substance for later use;
(3) according to the mass ratio of 1: 2: 9, mixing tetraethoxysilane, ammonia water and absolute ethyl alcohol, stirring for 22 hours at the temperature of 27 ℃ and 700r/min, filtering to obtain filter residue, centrifugally washing the filter residue for 2 times by using the ethanol, drying for 2.5 hours at the temperature of 37 ℃ to obtain a dried substance, taking 12.5 parts of methanol, 5.5 parts of deionized water, 3.5 parts of polydimethylsiloxane, 3.5 parts of ammonia water and 1.5 parts of the dried substance by weight, putting the methanol, the deionized water, the polydimethylsiloxane and the dried substance into a container, stirring for 35 minutes at the temperature of 57 ℃ and 250r/min, adding the ammonia water, refluxing for 0.9 hour at the temperature of 75 ℃, cooling to room temperature, centrifuging for 4 minutes at 35000r/min to obtain a precipitate, washing the precipitate for 3 times by using an ethanol solution, and drying at the temperature of 45 ℃ to obtain the dried substance;
(4) according to the weight parts, 25 parts of deionized water, 12.5 parts of the heat-insulating material for standby in the step (2), 7.5 parts of emulsifier, 1.5 parts of dry material, 0.65 part of hydroxymethyl cellulose, 0.15 part of catalyst and 0.15 part of formaldehyde are taken, the heat-insulating material for standby in the step (2), the emulsifier, the catalyst and the deionized water are mixed, the temperature is increased to 165 ℃, the mixture is stirred for 110min at 750r/min, the mixture is cooled to 55 ℃, the mixture is stirred for 9min at the rotating speed of 4500r/min, the dry material, the hydroxymethyl cellulose and the formaldehyde are added, the mixture is stirred for 4min at the rotating speed of 450r/min, and the spinning smoothing agent is obtained after uniform mixing.
Comparative example: a textile smoothing agent manufactured by a company of Suzhou city.
The smoothing agent of the invention and the smoothing agent of the comparative example are respectively used and nursed for the same batch of clothes produced by the same manufacturer, 50 persons are selected after one month to comprehensively evaluate the aspects of fading, pilling and the like of the used clothes, the layering condition of the smoothing agent is evaluated after half a year, and the test results are shown in table 1.
Table 1:
| test items | Example 1 | Example 2 | Example 3 | Comparative example |
| Fading of clothes | The clothes do not fade | The clothes do not fade | The clothes do not fade | The color fading is severe |
| Pilling of clothes | No pilling phenomenon | No pilling phenomenon | No pilling phenomenon | Surface part pilling |
| Case of fabric | Soft and smooth | Soft and smooth | Soft and smooth | Become hard in texture |
| Smoothing agent stratification condition | No delamination phenomenon | No delamination phenomenon | No delamination phenomenon | Severe delamination |
In conclusion, the textile smoothing agent disclosed by the invention is harmless to clothes after being used, and can effectively prevent the phenomena of clothes fading, pilling and the like.
Claims (3)
1. The preparation method of the textile smoothing agent is characterized by comprising the following steps:
(1) according to the weight parts, 10-15 parts of octamethylcyclotetrasiloxane, 5-6 parts of epoxy chloropropane, 2-3 parts of anhydrous stannic chloride and 1-2 parts of sodium hydroxide are taken, the octamethylcyclotetrasiloxane, the epoxy chloropropane and the anhydrous stannic chloride are mixed, the temperature is raised to 70-80 ℃, the temperature is kept for 5-6 hours, the sodium hydroxide is added for mixing when the temperature is reduced to 50-60 ℃, the mixture is stood, and reduced pressure distillation is carried out to obtain a distillate, wherein the mass ratio of the octamethylcyclotetrasiloxane to the epoxy chloropropane is 3-4: 5-6: 7-8, mixing the distillate, toluene and a sodium hydroxide solution, standing, and then carrying out reduced pressure distillation to obtain a distillate;
(2) taking 10-15 parts by weight of organic amine, 7-8 parts by weight of polyglycol ether, 5-6 parts by weight of distillate and 3-4 parts by weight of isopropanol, mixing the organic amine, the polyglycol ether and the isopropanol, stirring at the temperature of 45-50 ℃, heating to 80-90 ℃, dropwise adding the distillate, preserving heat at the temperature of 80-85 ℃ for 5-6 hours, and adjusting the pH value to 4-5 to obtain a heat preservation substance for later use;
(3) according to the mass ratio of 1: 2: 8-10, mixing ethyl orthosilicate, ammonia water and absolute ethyl alcohol, stirring at the temperature of 25-30 ℃, filtering to obtain filter residues, centrifugally washing the filter residues for 2-3 times by using ethanol, drying at the temperature of 35-40 ℃ to obtain a dried substance, putting 10-15 parts by weight of methanol, 5-6 parts by weight of deionized water, 3-4 parts by weight of polydimethylsiloxane, 3-4 parts by weight of ammonia water and 1-2 parts by weight of the dried substance into a container, stirring at the temperature of 50-65 ℃, adding ammonia water, refluxing, cooling to room temperature, centrifuging to obtain a precipitate, washing the precipitate for 3-4 times by using an ethanol solution, and drying at the temperature of 40-50 ℃ to obtain the dried substance;
(4) according to the weight parts, 20-30 parts of deionized water, 10-15 parts of the heat insulation material for standby in the step (2), 7-8 parts of an emulsifier, 1-2 parts of a dry material, 0.5-0.8 part of hydroxymethyl cellulose, 0.1-0.2 part of a catalyst and 0.1-0.2 part of formaldehyde are taken, wherein the emulsifier is prepared from the following raw materials in parts by mass: 1, uniformly mixing dodecyl benzene sulfonic acid and sorbitan monolaurate to obtain an emulsifier; and (3) mixing the heat-insulating material, the emulsifier, the catalyst and the deionized water which are reserved in the step (2), heating to 150-180 ℃, stirring, cooling to 50-60 ℃, stirring, adding the dried material, the hydroxymethyl cellulose and the formaldehyde, stirring again, and uniformly mixing to obtain the textile smoothing agent.
2. The method for preparing the textile smoothing agent of claim 1, wherein the organic amine in the step (2) is any one of hexamethylenediamine, N-diethylpropanediamine and ethanolamine.
3. The method for preparing the textile smoothing agent of claim 1, wherein the catalyst in the step (4) is hydrochloric acid.
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| CN112663332A (en) * | 2020-12-23 | 2021-04-16 | 南通恒润新材料科技有限公司 | Preparation method of high-stability high-temperature-resistant smoothing agent |
| CN113445318A (en) * | 2021-07-28 | 2021-09-28 | 沂水祥腾化工有限公司 | Yarn smoothing agent for spinning and preparation method thereof |
| CN117645728B (en) * | 2024-01-29 | 2024-06-18 | 江苏恒力化纤股份有限公司 | Preparation method of flexibility-enhanced flame retardant and high-strength flexibility flame-retardant polyester industrial yarn |
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