CN112726211A - Preparation method of polyurethane modified organic silicon softening agent - Google Patents
Preparation method of polyurethane modified organic silicon softening agent Download PDFInfo
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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
- D06M15/653—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain modified by isocyanate compounds
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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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Abstract
The invention relates to the technical field of finishing processing after textile printing and dyeing, in particular to a preparation method of a polyurethane modified organic silicon softening agent, which is suitable for finishing processing after cellulose fibers, synthetic fibers and blending thereof. The method comprises the following steps: the tertiary amine compound reacts with epoxy silicone oil firstly, then reacts with isocyanate, then uses a sealing agent to seal excessive isocyanate groups, and finally removes the solvent through emulsification dispersion and distillation to obtain the polyurethane modified organic silicon softening agent. The polyurethane modified organic silicon softener prepared by the invention is applied to the softening processing of textile fabrics, has excellent hand feeling, has certain water absorption for cotton fabrics, does not influence the whiteness of the fabrics, basically does not reduce the hand feeling during washing, has excellent washing resistance and has wide market prospect.
Description
Technical Field
The invention relates to the technical field of finishing processing after textile printing and dyeing, in particular to a preparation method of a polyurethane modified organic silicon softening agent, which is suitable for finishing processing after cellulose fibers, synthetic fibers and blending thereof.
Background
Along with the improvement of living standard of people, the requirement of people on wearing comfort is higher and higher, the requirement on handfeel is richer and more strict, and meanwhile, the requirement on the quality of fabrics is also higher and more strict, such as slippage, fastness, water absorption, fluffing and pilling and the like.
The main chain of the organosilicon softener is-Si-O-chain length which is longer than-C-O-chain length, so that molecular chains are softer, the organosilicon softener has excellent lubricating and softening properties, and the organosilicon softener is widely applied to finishing after spinning. The development process goes through the following four stages.
The first generation of silicone softeners, which began in the fifth and sixty years of the last century, represented products such as dimethyl siloxane (PDMS) and hydroxy silicone oil emulsions. The first generation of products has the advantages of low cost, small color change of treated fabrics, very lubrication and the like. However, the lack of reactive functional groups results in poor wash fastness, poor softness of hand and rebound, and the emulsion is unstable and delaminates, resulting in the formation of silicone oil spots. The first generation products are now rarely used as fabric softeners, typically as yarn lubricants, filling fiber treatments or chemical fiber spinning oils.
Because the first generation of organosilicon softener has the problems of single function and easy demulsification, bleaching and the like in use, a second generation of organosilicon softener, namely a modified organosilicon softener, is developed by competitive development of organosilicon workers from the eighties of the last century. The products are prepared by introducing amino groups and epoxy groups on siloxane side chains or performing emulsion polymerization. The second generation products greatly improve the washability of the fabric and rely on different groups to impart different styles to the fabric. The amino modified silicone oil has smooth hand feeling and rebound effect, good washability, and can improve the tearing strength of the fabric, and can be used together with resin in one bath. But the defects that the emulsion is unstable and delaminated to cause silicone oil spots, the water-absorbent fabric is not hydrophilic after being finished, and the water-absorbent fabric has larger yellowing and color change and the like exist. The amino modified silicone oil is the modified silicone fabric softener with the highest utilization rate in the market at present. Compared with the dry and comfortable touch, the epoxy modified silicone oil has the rebound effect, the treated fabric has little yellowing, the tearing strength of the fabric can be improved, and the epoxy modified silicone oil can be used together with resin. However, the finished fabric is lack of plump and soft feeling, emulsion can be unstable and delaminated to cause the generation of silicone oil spots, and the water-absorbing fabric is not hydrophilic after finishing, and is generally applied to water-repellent soft finishing. The emulsion polymerized silicone oil has the advantages of simultaneous polymerization and emulsification in the production process, low production cost, larger emulsion particles, very good smooth feeling, and the main defects of poor hand feeling and a small amount of precipitate in the product storage process. The method is mainly applied to smooth finishing of various fiber fabrics.
In the nineties of the last century, developers introduced polyether active groups on siloxane side chains to improve the hydrophilic performance of fabrics finished by the third-generation silicone softener, and representative products comprise polyether modified silicone oil and amino (epoxy group)/polyether modified silicone oil. The pure polyether modified silicone oil can provide instant water absorption performance, has the characteristics of water dispersion/water solubility, does not cause yellowing and color change of the treated fabric, does not need emulsification, does not cause the problems of layering and oil stain, and can be dyed and printed again after the fabric is treated. However, the finished fabric has poor smoothness, no plump soft feeling, low hydrophilicity and soft feeling, and no improvement on tearing strength of the fabric. The product is only suitable for the products which need to absorb water instantly, and the hand feeling requires general soft finishing. Compared with the polyether modified silicone oil, the amino (epoxy group)/polyether modified silicone oil mainly has better hand feeling than the polyether modified silicone oil, has slightly higher yellowing, and is mainly used as a general hydrophilic soft finishing agent for general fabrics.
Around 2000 years, foreign organosilicon workers developed a fourth generation organosilicon softener, namely a linear block multi-component copolymerization modified organosilicon softener. The fourth generation product integrates the advantages of the first three generation products, well avoids the problems of the first three generation products, and is a novel organic silicon softener product with excellent comprehensive performance. The product has wide application range, can be used for various fibers and fabrics, is convenient and simple to use, is easy to disperse in water, and basically does not use an emulsifier or uses a small amount of an emulsifier. The high-concentration product can be directly used; the compatibility is very good, and the product has excellent stability to strong acid, strong alkali, high electrolyte and the like; the high-temperature and high-shear stability is good, and the adaptability and flexibility to processes and equipment are extremely high; the product is used without layering, demulsification, oil stain, roller and cylinder sticking; very low yellowing and color change; better washing fastness; the fabric has the advantages of full and fluffy hand feeling, elasticity, smoothness, strong silk feeling and approximate natural comfortable feeling, overcomes the defect that the traditional amino silicone oil is excessively greasy, has very good hand feeling improvement, can achieve super softness and hydrophilicity higher than medium level, and can be used with organic fluorine easy-to-clean finishing; the polyester finishing agent can be used for color repair, stripping, re-dyeing and over-dyeing, does not cause secondary pollution, basically does not influence the heat migration fastness of disperse dyes on polyester, and keeps the color fastness of washing and rubbing before soft finishing. In view of the numerous advantages of the fourth generation linear block multi-component copolymerization modified organosilicon softening agent, some domestic chemical auxiliary agents are also intensively researched and developed at present, and similar products are sold in the market.
Despite the many excellent properties of silicone, the inherent disadvantages of single structure polymers, low mechanical strength, poor solvent resistance and poor surface adhesion, which are inherent to the structure of silicone, still cannot be overcome, and these disadvantages limit the range of applications of silicone. In order to make up for the deficiency of the organic silicon polymer, it is an effective solution to combine the organic silicon polymer with other organic polymers.
Polyurethane and silicone products each have many excellent characteristics, but they also have respective drawbacks due to structural deficiencies, such as poor water resistance, poor weather resistance, low mechanical strength of silicone, poor adhesion, and the like. The copolymerization modification of the two is an effective way for overcoming the defects of a single polymer, and the polyurethane organosilicon copolymerization product has the advantages of the two, such as good flexibility, excellent water resistance, excellent surface adhesion and good biocompatibility, i.e., the problems of low mechanical strength and poor adhesion of organosilicon and poor weather resistance of polyurethane are solved, and products with different properties can be prepared by adopting different synthesis processes and raw material ratios, thereby meeting various market requirements. Polyurethane silicone can be roughly divided into three structures of block type, graft type and interpenetrating network type according to different synthesis modes and raw materials.
In recent years, polyurethane-modified silicone softeners have appeared on the market, but most of them have no reactive isocyanate group left in spite of their polyurethane structure, and cannot further react with a hydroxyl group, an amino group, a carboxylic acid group, or the like on the fiber when the fabric is processed, thereby achieving a hand feeling effect of water washing resistance. Although the literature reports that the isocyanate-terminated polyether modified siloxane is applied to crease-resistant finishing of real silk, isocyanate can be released at high temperature and combined with hydroxyl, amino and the like on the fabric to realize a certain washing-resistant effect. However, because the structure is lack of cationic quaternary ammonium salt groups, multipoint anion and cation adsorption is not easy to form on the surface of the fiber, so that the directional arrangement effect of the molecular structure on the surface of the fabric is poor, and the hand feeling is insufficient. According to the method, a molecular chain segment contains a silicone oil chain segment and a polyurethane chain segment, meanwhile, a proper quaternary ammonium salt group is introduced, the isocyanate group is blocked and protected, the isocyanate group is released under the high-temperature shaping condition, and the isocyanate group is combined with hydroxyl, amino and the like on the fabric, so that the problem of insufficient hand feeling is solved, and the effect of water washing resistance is realized.
Disclosure of Invention
The invention mainly solves the defects in the prior art, and provides a preparation method of a polyurethane modified organosilicon softener which not only endows a fabric with an excellent hand feeling effect, does not influence the whiteness of the fabric, has certain hydrophilicity, but also keeps the hand feeling after washing.
The technical problem of the invention is mainly solved by the following technical scheme:
a preparation method of a polyurethane modified organosilicon softener comprises the following steps:
1) adding 3-10 parts of tertiary amine compound into 30-100 parts of epoxy silicone oil to neutralize 1-2 parts of organic acid, starting stirring, and reacting for 3 hours at 60-80 ℃;
2) adding 10-50 parts of isocyanate into the reaction system in the step 1), and reacting for 1-3 hours at 60-70 ℃;
3) adding a mixture of 3-20 parts of a sealing agent and 12-20 parts of a ketone solvent into the reaction system in the step 2), reacting for 2-5 hours at 60-80 ℃, and sealing excessive isocyanate groups by using the sealing agent to form a polyurethane modified organic silicon polymer;
4) dispersing the polyurethane modified organic silicon polymer synthesized in the step 3) in aqueous solution of 3-7 parts of neutralizing agent and 10-100 parts of emulsifier, emulsifying for 10-20min under stirring, and then distilling under reduced pressure to remove ketone solvent to obtain polyurethane modified organic silicon softener with solid content of 30-35%;
the raw materials are in parts by weight.
Preferably, the tertiary amine compound in the step 1) is fatty chain tertiary amine, and the end group is tertiary amine, and the structure of the tertiary amine is as follows:
wherein, P is 0 to 20;
the tertiary amine compound in the step 1) is one or more of tetramethylpropanediamine, tetramethylhexanediamine, tetramethylpentanediamine, tetramethyloctanediamine and tetramethylnonanediamine.
Preferably, the epoxy silicone oil in step 1) contains polysiloxane with epoxy groups at two ends, and the structural formula is as follows:
wherein R is epoxy group, n is 0-260;
the epoxy silicone oil in the step 1) is subjected to ring-opening reaction by adding alkali into octamethylcyclotetrasiloxane, an epoxy group organosilicon end-capping agent is added, the molecular weight can be controlled by adjusting the using amount of the end-capping agent, and the numerical value of the polymerization degree is controlled.
Preferably, the epoxy silicone capping agent in step 1) is 3- (2, 3-glycidoxy) propyltrimethoxysilane, 1, 3-bis (3-glycidoxypropyl) -1,1,3, 3-tetramethyldisiloxane.
Preferably, the organic acid in step 1) is one or more of acetic acid, citric acid and malic acid.
Preferably, the isocyanate in step 2) is one or more of toluene diisocyanate, isophorone diisocyanate, diphenylmethane diisocyanate, hexamethylene diisocyanate, toluene diisocyanate trimer, and hexamethylene diisocyanate trimer.
Preferably, the blocking agent of step 3) is one or more of acetone oxime, epsilon-caprolactam, butanol, 5-dimethylpyrazole and 3, 5-dimethylpyrazole;
preferably, the ketone solvent in step 3) is one or more of acetone, methyl ethyl ketone and butanone.
Preferably, the neutralizing agent of step 4) is one or more of glacial acetic acid, sulfuric acid, hydrochloric acid, formic acid, citric acid, succinic acid and glycolic acid.
Preferably, the emulsifier in the step 4) is a mixed emulsifier which is compounded by two to four fatty alcohol-polyoxyethylene ethers with different HLB values, and the HLB value of the mixed emulsifier is 5-19; fatty alcohol polyoxyethylene ethers, also known as polyethoxylated fatty alcohols; the surfactant is prepared by the addition reaction of fatty alcohol and ethylene oxide and is represented by the following general formula: R-O- (CH2CH2O) n-H, wherein R is a saturated or unsaturated C12-18 alkyl group, which is a straight chain alkyl group or a branched chain alkyl group, and n is the addition number of ethylene oxide and refers to the number of oxyethylene groups in a surfactant molecule.
The polyurethane modified organosilicon softener can be used for softening and finishing various textile fabrics, and the textile fabrics comprise all cotton, all polyester, polyester cotton, hemp, polyester viscose, acrylic fibers, chinlon and the like.
The polyurethane modified organic silicon softener prepared by the invention is applied to the softening processing of textile fabrics, not only has excellent hand feeling, but also has certain water absorption for cotton fabrics, does not influence the whiteness of the fabrics, does not basically reduce the hand feeling of washing, has excellent washing resistance and has wide market prospect.
Detailed Description
The technical scheme of the invention is further specifically described by the following embodiments.
The following examples describe a polyurethane modified silicone softener, its preparation and its use in textile fabrics, the parts in the examples being parts by weight unless otherwise specified.
Example 1: adding 3 parts of tetramethylhexamethylenediamine, 50 parts of epoxy silicone oil (molecular weight 8000) in a formula (1) and 1 part of acetic acid into a stainless steel reaction kettle with heating, cooling, nitrogen protection, stirring, temperature and pressure indication (recording) and vacuum feeding conditions, slowly heating to 70 ℃, and keeping the temperature for 5 hours. 15 parts of hexamethylene diisocyanate were added at this temperature and the reaction was carried out at 60 ℃ until the NCO content had reached the theoretical value (which was determined by di-n-butylamine titration);
cooling to 40 ℃, adding a mixed solution of 4 parts of butanone oxime and 13 parts of acetone into a four-mouth bottle, and reacting at 70 ℃ until the NCO content reaches a theoretical value (detected by a di-n-butylamine titration method), thereby obtaining a polyurethane modified organic silicon polymer;
adding 400 parts of polyurethane modified organic silicon polymer and lauryl polyoxyethylene ether AEO into an enamel reaction kettle with the conditions of heating, cooling, stirring, temperature and vacuum feeding345 parts of lauryl polyoxyethylene ether AEO520 parts of lauryl polyoxyethylene ether AEO915 parts of deionized water and 5 parts of acetic acid, and slowly adding 1300 parts of deionized water to obtain a final product.
Example 2: 4 parts of tetramethylpropanediamine, 80 parts of epoxy silicone oil (molecular weight 10000) shown in the formula (1) and 1.5 parts of acetic acid are added into a stainless steel reaction kettle with the conditions of heating, cooling, nitrogen protection, stirring, temperature and pressure indication (recording) and vacuum feeding, slowly heated to 60 ℃, and kept warm for 4 hours. At this temperature, 25 parts of hexamethylene diisocyanate were added and reacted at 60 ℃ until the NCO content reached the theoretical value (which was determined by di-n-butylamine titration);
cooling to 40 ℃, adding a mixed solution of 5 parts of epsilon-caprolactam and 15 parts of butanone into a four-mouth bottle, and reacting at 75 ℃ until the NCO content reaches a theoretical value (detected by a di-n-butylamine titration method), thereby obtaining a polyurethane modified organic silicon polymer;
adding 450 parts of polyurethane modified organic silicon polymer and lauryl polyoxyethylene ether AEO into an enamel reaction kettle with the conditions of heating, cooling, stirring, temperature and vacuum feeding355 parts of,Dodecyl alcohol polyoxyethylene ether AEO535 parts of glycolic acid and 4 parts of deionized water are slowly added into the mixture to obtain the final product.
Example 3: adding 3 parts of tetramethylnonanediamine, 100 parts of epoxy silicone oil (with the molecular weight of 12000) shown in the formula (1) and 1 part of acetic acid into a stainless steel reaction kettle with the conditions of heating, cooling, nitrogen protection, stirring, temperature and pressure indication (recording) and vacuum feeding, slowly heating to 65 ℃, and keeping the temperature for 9 hours. Hexamethylene diisocyanate trimer was added at this temperature and reacted at 65 ℃ until the NCO content reached the theoretical value (which was determined by di-n-butylamine titration);
cooling to 40 ℃, adding a mixed solution of 5 parts of epsilon-caprolactam and 18 parts of butanone into a four-mouth bottle, and reacting at 70 ℃ until the NCO content reaches a theoretical value (detected by a di-n-butylamine titration method), thereby obtaining a polyurethane modified organic silicon polymer;
adding 500 parts of polyurethane modified organic silicon polymer and lauryl polyoxyethylene ether AEO into an enamel reaction kettle with the conditions of heating, cooling, stirring, temperature and vacuum feeding330 parts of lauryl polyoxyethylene ether AEO540 parts of glycolic acid and 4 parts of deionized water are slowly added into the mixture, and the final product is obtained.
Example 4: adding 3 parts of tetramethylnonanediamine, 100 parts of epoxy silicone oil (with the molecular weight of 12000) shown in the formula (1) and 1.5 parts of citric acid into a stainless steel reaction kettle with the conditions of heating, cooling, nitrogen protection, stirring, temperature and pressure indication (recording) and vacuum feeding, slowly heating to 65 ℃, and keeping the temperature for 9 hours. Hexamethylene diisocyanate trimer was added at this temperature and reacted at 65 ℃ until the NCO content reached the theoretical value (which was determined by di-n-butylamine titration);
cooling to 40 ℃, adding a mixed solution of 5 parts of epsilon-caprolactam and 15 parts of butanone into a four-mouth bottle, and reacting at 70 ℃ until the NCO content reaches a theoretical value (detected by a di-n-butylamine titration method), thereby obtaining a polyurethane modified organic silicon polymer;
adding 500 parts of polyurethane modified organic silicon polymer and lauryl polyoxyethylene ether AEO into an enamel reaction kettle with the conditions of heating, cooling, stirring, temperature and vacuum feeding320 parts of lauryl polyoxyethylene ether AEO560 parts of lauryl polyoxyethylene ether AEO940 parts of glycolic acid and 1100 parts of deionized water are slowly added to obtain the final product.
Example 5: adding 5 parts of tetramethyl pentanediamine, 90 parts of epoxy silicone oil (molecular weight of 14000) shown in formula (1) and 1.5 parts of malic acid into a stainless steel reaction kettle with the conditions of heating, cooling, nitrogen protection, stirring, temperature indication (recording) and vacuum feeding, slowly heating to 75 ℃, and keeping the temperature for 12 hours. 40 parts of hexamethylene diisocyanate trimer are added at the temperature, and the reaction is carried out at 65 ℃ until the NCO content reaches the theoretical value (the NCO content is detected by a di-n-butylamine titration method);
cooling to 40 ℃, adding a mixed solution of 4 parts of 5-dimethylpyrazole and 13 parts of acetone into a four-mouth bottle, and reacting at 70 ℃ until the NCO content reaches a theoretical value (detected by a di-n-butylamine titration method), thereby obtaining a polyurethane modified organic silicon polymer;
adding 500 parts of polyurethane modified organic silicon polymer and lauryl polyoxyethylene ether AEO into an enamel reaction kettle with the conditions of heating, cooling, stirring, temperature and vacuum feeding320 parts of lauryl polyoxyethylene ether AEO530 parts of lauryl polyoxyethylene ether AEO910 parts and 4 parts of glycolic acid, and 1100 parts of deionized water is slowly added to obtain the final product.
Example 6: adding 6 parts of tetramethyloctanediamine, 90 parts of epoxy silicone oil (molecular weight of 6000) shown in the formula (1) and 1 part of acetic acid into a stainless steel reaction kettle with heating, cooling, nitrogen protection, stirring, temperature and pressure indication (recording) and vacuum feeding conditions, slowly heating to 75 ℃, and keeping the temperature for 6 hours. Adding 20 parts of hexamethylene diisocyanate trimer at the temperature, and reacting at 65 ℃ until the NCO content reaches the theoretical value (detected by a di-n-butylamine titration method);
cooling to 40 ℃, adding a mixed solution of 10 parts of 5-dimethylpyrazole and 15 parts of acetone into a four-mouth bottle, and reacting at 60 ℃ until the NCO content reaches a theoretical value (detected by a di-n-butylamine titration method), thereby obtaining a polyurethane modified organic silicon polymer;
adding 500 parts of polyurethane modified organic silicon polymer and lauryl polyoxyethylene ether AEO into an enamel reaction kettle with the conditions of heating, cooling, stirring, temperature and vacuum feeding310 parts of lauryl polyoxyethylene ether AEO550 parts of lauryl polyoxyethylene ether AEO930 parts of glycolic acid and 3 parts of deionized water are slowly added into the mixture, and 1100 parts of deionized water are slowly added to obtain a final product.
Performance evaluation:
the product obtained in example 1 was treated on a cotton fabric and prepared into a solution (using amount of 3% Soln) → one-dip-one-roll (retention of 70%) → 160 degrees for 2 minutes. The treated cloth had the following properties:
good feeling → ≈ o-→ Δ → Δ → Δ × → × Δ → × difference
Evaluation of Performance
The product prepared in example 1 is processed on a fluorescent polyester knitted fabric, and the solution preparation (the using amount is 3% Soln) → one-dip-one-roll (the rolling residue is 80%) → 180-degree setting is carried out for 1 minute. The properties of the treated cloth were as follows:
good feeling → ≈ o-→ Δ → Δ → Δ × → × Δ → × difference
Claims (10)
1. A preparation method of a polyurethane modified organosilicon softener is characterized by comprising the following steps:
1) adding 3-10 parts of tertiary amine compound into 30-100 parts of epoxy silicone oil to neutralize 1-2 parts of organic acid, starting stirring, and reacting for 3 hours at 60-80 ℃;
2) adding 10-50 parts of isocyanate into the reaction system in the step 1), and reacting for 1-3 hours at 60-70 ℃;
3) adding a mixture of 3-20 parts of a sealing agent and 12-20 parts of a ketone solvent into the reaction system in the step 2), reacting for 2-5 hours at 60-80 ℃, and sealing excessive isocyanate groups by using the sealing agent to form a polyurethane modified organic silicon polymer;
4) dispersing the polyurethane modified organic silicon polymer synthesized in the step 3) in aqueous solution of 3-7 parts of neutralizing agent and 10-100 parts of emulsifier, emulsifying for 10-20min under stirring, and then distilling under reduced pressure to remove ketone solvent to obtain polyurethane modified organic silicon softener with solid content of 30-35%;
the raw materials are in parts by weight.
2. The preparation method of the polyurethane modified organosilicon softener according to claim 1, characterized in that: the tertiary amine compound in the step 1) is fatty chain tertiary amine, the end group is tertiary amine, and the structure is as follows:
wherein, P is 0 to 20;
the tertiary amine compound in the step 1) is one or more of tetramethylpropanediamine, tetramethylhexanediamine, tetramethylpentanediamine, tetramethyloctanediamine and tetramethylnonanediamine.
3. The preparation method of the polyurethane modified organosilicon softener according to claim 1, characterized in that: the polysiloxane containing epoxy groups at two ends of the epoxy silicone oil in the step 1) has a structural general formula as follows:
wherein R is epoxy group, n is 0-260;
the epoxy silicone oil in the step 1) is subjected to ring-opening reaction by adding octamethylcyclotetrasiloxane and alkali, an epoxy group organosilicon end-capping agent is added, and the molecular weight and the polymerization degree can be controlled by adjusting the amount of the end-capping agent.
4. The preparation method of the polyurethane modified organosilicon softener according to claim 1, characterized in that: the epoxy organosilicon end-capping reagent in the step 1) is 3- (2, 3-epoxypropoxy) propyl trimethoxy silane and 1, 3-bis (3-glycidoxypropyl) -1,1,3, 3-tetramethyl disiloxane.
5. The preparation method of the polyurethane modified organosilicon softener according to claim 1, characterized in that: the organic acid in the step 1) is one or more of acetic acid, citric acid and malic acid.
6. The preparation method of the polyurethane modified organosilicon softener according to claim 1, characterized in that: and 2) the isocyanate in the step 2) is one or more of toluene diisocyanate, isophorone diisocyanate, diphenylmethane diisocyanate, hexamethylene diisocyanate, toluene diisocyanate tripolymer and hexamethylene diisocyanate tripolymer.
7. The preparation method of the polyurethane modified organosilicon softener according to claim 1, characterized in that: the blocking agent of the step 3) is preferably one or more of acetone oxime, epsilon-caprolactam, butanol, 5-dimethylpyrazole and 3, 5-dimethylpyrazole.
8. The preparation method of the polyurethane modified organosilicon softener according to claim 1, characterized in that: the ketone solvent in the step 3) adopts one or more of acetone, methyl ethyl ketone and butanone.
9. The preparation method of the polyurethane modified organosilicon softener according to claim 1, characterized in that: the neutralizing agent in the step 4) adopts one or more of glacial acetic acid, sulfuric acid, hydrochloric acid, formic acid, citric acid, succinic acid and glycolic acid.
10. The preparation method of the polyurethane modified organosilicon softener according to claim 1, characterized in that: the emulsifier in the step 4) is a mixed emulsifier which is compounded by two to four fatty alcohol-polyoxyethylene ethers with different HLB values, and the HLB value is 5-19; fatty alcohol polyoxyethylene ethers, also known as polyethoxylated fatty alcohols; the surfactant is prepared by the addition reaction of fatty alcohol and ethylene oxide and is represented by the following general formula: R-O- (CH2CH2O) n-H, wherein R is a saturated or unsaturated C12-18 alkyl group, which is a straight chain alkyl group or a branched chain alkyl group, and n is the addition number of ethylene oxide, which refers to the number of oxyethylene groups in a surfactant molecule.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113373696A (en) * | 2021-06-18 | 2021-09-10 | 广东宏昊化工有限公司 | Softening agent for bamboo fiber fabric and preparation method thereof |
| CN115612055A (en) * | 2022-10-11 | 2023-01-17 | 江苏富淼科技股份有限公司 | Solvent-free self-emulsified water-washing-resistant softening agent, and preparation method and application thereof |
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| CN113373696A (en) * | 2021-06-18 | 2021-09-10 | 广东宏昊化工有限公司 | Softening agent for bamboo fiber fabric and preparation method thereof |
| CN115612055A (en) * | 2022-10-11 | 2023-01-17 | 江苏富淼科技股份有限公司 | Solvent-free self-emulsified water-washing-resistant softening agent, and preparation method and application thereof |
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