CN119798590B - Wet rubbing fastness improver with soft hand feeling and preparation method thereof - Google Patents
Wet rubbing fastness improver with soft hand feeling and preparation method thereofInfo
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Abstract
本发明公开了一种柔软手感的湿摩擦牢度提升剂及其制备方法，属于纺织化学品技术领域，用于解决现有技术中织物所用的湿摩擦牢度提升剂牢固程度低和提升织物的柔软手感作用低的问题，其中柔软手感的湿摩擦牢度提升剂的制备方法包括：改性硅烷、丙烯酸二甲胺基乙酯加入到丙酮中，反应，得到季铵盐型改性硅烷；在氮气氛围下，季铵盐型改性硅烷和3‑氯过氧苯甲酸加入到二氯甲烷中，低温条件下反应，得到端环氧基的季铵盐型改性硅烷；由本发明制备得到的湿摩擦牢度提升剂具有良好的性能，用其处理后的织物不仅更具柔软性，还提高了织物的湿摩擦牢度和耐水洗性。
This invention discloses a wet rubbing fastness improver for a soft hand feel and its preparation method, belonging to the field of textile chemical technology. It addresses the problems of low fastness and limited effectiveness in improving the softness of fabrics using existing wet rubbing fastness improvers. The preparation method of the wet rubbing fastness improver for a soft hand feel includes: adding modified silane and dimethylaminoethyl acrylate to acetone and reacting to obtain a quaternary ammonium salt modified silane; then, under a nitrogen atmosphere, adding the quaternary ammonium salt modified silane and 3-chloroperoxybenzoic acid to dichloromethane and reacting at low temperature to obtain an epoxy-terminated quaternary ammonium salt modified silane. The wet rubbing fastness improver prepared by this invention has excellent performance; fabrics treated with it are not only softer but also have improved wet rubbing fastness and washability.
Description
Technical Field
The invention relates to the technical field of textile chemicals, in particular to a wet rubbing fastness improver with soft hand feeling and a preparation method thereof.
Background
At present, with the improvement of consumption level, the quality requirements of people on clothing wearability are higher and higher, wherein the wet rubbing fastness of water-soluble dyes such as direct dyes, reactive dyes, acid dyes and the like can not meet the requirements of customers. The wet rubbing color fastness is an important index of clothing wear performance, and refers to the degree of transferring color from the surface of a dyed fabric to the surface of other objects contacted with the dyed fabric when the dyed fabric is rubbed in a wet state. It is an important index in the color fastness test of textiles, and is used for evaluating the fastness degree of the color of dyed fabrics in the actual use process (such as washing, contacting with water when wearing, etc.). At present, dyeing and finishing workers can select dyes with relatively high fastness or use a smoothing agent to carry out smooth and soft treatment on the fabric, so that the resistance and friction coefficient during friction are reduced, and the wet friction fastness of the dyed fabric is improved. However, these processes only improve the wet crockfastness of the fabric to a certain extent.
The invention discloses a wet friction fastness improver for dyed fabrics, which is a nonionic polymer, and is prepared by mixing low-hydrogen silicone oil, polyurethane prepolymer and polyacrylic acid-maleic acid copolymer (30-60) according to the mass ratio of (10-30) to (20-40) and copolymerizing under the condition of catalytic heating, wherein the wet friction fastness improver for dyed fabrics, which is prepared by the invention, is required to improve the soft hand feeling of the fabrics, the invention, which is disclosed by the invention, is a preparation method of an aqueous polyurethane wet friction fastness improver, a proper amount of polycaprolactone triol is added into a reactor for high-temperature vacuumizing dehydration treatment, the temperature of the reactor is reduced to 60 ℃, a proper amount of diisocyanate is added, the temperature is raised to 75 ℃, the temperature is kept for 3 hours, the polyurethane prepolymer is obtained, a proper amount of hydrophilic chain extender is added into the reactor for chain extension, the reaction is carried out, a proper amount of small molecular polyol is added into the reactor for chain extension and reaction, the triethylamine is added into the reactor for pH value of the reactor to be 6-7, the aqueous polyurethane is prepared into the reactor for uniform friction fastness, the aqueous friction fastness is further improved, and the aqueous polyurethane is prepared, which is required to be 3, and the wet friction fastness is further improved.
Disclosure of Invention
In order to solve the technical problems, the invention provides the wet rubbing fastness improver with soft hand feeling and the preparation method thereof, and solves the problems of low firmness degree of the wet rubbing fastness improver used for fabrics and low effect of improving the soft hand feeling of the fabrics in the prior art.
In order to achieve the above object, the present invention provides a method for preparing a wet rubbing fastness improver with soft hand feeling, comprising the following steps:
Step (1) adding epoxy organosilane and 2-chloro-1, 3-propanediol into N, N-dimethylformamide, mixing, heating, reacting, and performing rotary evaporation to obtain modified silane;
adding modified silane and dimethylaminoethyl acrylate into acetone, reacting, filtering, washing and drying to obtain quaternary ammonium salt modified silane;
under the nitrogen atmosphere, adding quaternary ammonium salt type modified silane and 3-chloroperoxybenzoic acid into methylene dichloride, reacting at a low temperature, filtering, washing and drying to obtain epoxy-terminated quaternary ammonium salt type modified silane;
And (4) heating and stirring dimethyl diphenyl diisocyanate, polyether glycol and tetrahydrofuran to obtain a polyurethane prepolymer, and adding epoxy-terminated quaternary ammonium salt modified silane, a chain extender and a catalyst into the polyurethane prepolymer, uniformly mixing, heating and defoaming to obtain the wet friction fastness improver with soft hand feeling.
Preferably, in the step (1), the mass ratio of the epoxy silane to the 2-chloro-1, 3-propanediol to the N, N-dimethylformamide is (10-20): 100-180): 1000-1800, the reaction temperature is 60-70 ℃ and the reaction time is 38-48h.
Preferably, in step (1), the epoxyorganosilane is any one of 2- (3, 4-epoxycyclohexane) ethyl trimethoxysilane, glycidoxy octyl trimethoxysilane, glycidoxy butyl trimethoxysilane and glycidoxy propyl methyl dimethoxy silane.
Preferably, in the step (2), the mass ratio of the epoxy organosilane, the dimethylaminoethyl acrylate and the acetone is (80-100): 30-50): 1500-3500.
Preferably, in the step (3), the mass ratio of the quaternary ammonium salt type modified silane to the 3-chloroperoxybenzoic acid to the dichloromethane is (40-60): 200-400): 1000-1800, the reaction temperature is 1-5 ℃, and the reaction time is 2-4h.
Preferably, the polyether glycol is any one of polytetrahydrofuran glycol and polyoxyethylene glycol.
Preferably, in the step (4), the mass ratio of the dimethylbiphenyl diisocyanate to the polyether glycol to the tetrahydrofuran is (30-70): 10-20): 10-30, and the reaction condition is 70-80 ℃ for 2-5 hours.
Preferably, in step (4), the chain extender comprises glycerol and the catalyst comprises triisopropanolamine.
Preferably, in the step (4), the mass ratio of the polyurethane prepolymer to the epoxy group-terminated quaternary ammonium salt modified silane to the chain extender to the catalyst is (80-90): 4-10): 2-3): 0.8-1.2.
Preferably, in the step (4), the temperature of the second heating is 100-110 ℃ and the heating time is 1-2h.
Preferably, the soft-feel wet rubbing fastness improver prepared by the preparation method of the soft-feel wet rubbing fastness improver is adopted.
Preferably, the use of said soft feel wet crockfastness enhancing agent in a fabric.
Preferably, the fabric includes cotton fabric, polyester cotton fabric and nylon fabric.
Compared with the prior art, the invention has the beneficial effects that:
1. The epoxy organosilane has certain heat resistance and contains a long-chain structure, a certain flexibility is provided for the epoxy organosilane, epoxy groups in the epoxy organosilane and hydroxyl groups in 2-chloro-1, 3-propanediol react to generate ether groups with stronger chemical stability and are more waterproof, chlorine groups in the modified silane can react with tertiary amine groups in dimethylaminoethyl acrylate to generate salt to obtain quaternary ammonium salt type modified silane, quaternary ammonium salt cationic groups and silicon hydroxyl groups in the epoxy organosilane are generated at the moment, the quaternary ammonium salt cationic groups have stronger polarity and can react with anions of dyes to form insoluble dye salt precipitation, the effect of fixing the dyes on fabrics is achieved, the silicon hydroxyl groups have stronger reactivity, the reactive groups of the silicon hydroxyl groups and the reactive groups of the dyes on fabrics can be dehydrated in the drying process to form stable chemical bonds, the dyes on the fabrics can be further fixed, and meanwhile, the long-chain structure in the dimethylaminoethyl acrylate can enhance the flexibility of the polymer, and the lack of the quaternary ammonium salt type modified silane can cause the compactness of the polymer structure, so that the softness of the fabrics is influenced. The unsaturated double bond contained in the quaternary ammonium salt type modified silane is reacted with 3-chloroperoxybenzoic acid to obtain epoxy groups with better stability, the epoxy groups can react with hydroxyl groups, amino groups and the like on the fabric to form stable covalent bonds, the wet friction fastness is promoted, the water resistance is improved, meanwhile, the tight and uniform combination mode is favorable for keeping the original structure and flexibility of the fabric fiber, so that the softness is better kept or even improved, the epoxy group-terminated quaternary ammonium salt type modified silane contains ether groups, hydroxyl groups and epoxy groups, the epoxy groups can further react with polyurethane prepolymer to form a crosslinked structure, the fabric is endowed with good elasticity, a film layer with certain fastness is formed on the textile material, and the washing fastness and the wet friction fastness of the color fixing agent are improved.
2. The wet rubbing fastness improver with soft hand feeling, which is prepared by the invention, is polyether polyurethane containing quaternary ammonium salt and epoxy groups, has good performance, and the fabric treated by the agent not only has more softness, but also improves the wet rubbing fastness and the washing fastness of the fabric, and can also endow the fabric with the properties of fullness, thickness, ventilation, comfort, softness, brightness and static resistance.
Drawings
FIG. 1 is a flow chart of a process for preparing a wet crockfastness enhancing agent of soft feel according to the present invention.
Detailed Description
The technical solutions of the present invention will be clearly and completely described in connection with the embodiments, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The embodiment provides a preparation method of a wet rubbing fastness improver with soft hand feeling, which comprises the following steps:
Step (1) mixing glycidoxy butyl trimethoxy silane, 2-chloro-1, 3-propanediol and N, N-dimethylformamide according to the mass ratio of 10:100:1000, reacting for 48 hours at 60 ℃, and performing rotary evaporation to obtain modified silane;
step (2) mixing modified silane, dimethylaminoethyl acrylate and acetone according to the mass ratio of 80:30:1500, reacting for 6 hours at the temperature of 25 ℃, filtering after the reaction is finished, washing with absolute ethyl alcohol, and drying for 8 hours at the temperature of 60 ℃ to obtain quaternary ammonium salt modified silane;
Step (3) under the nitrogen atmosphere, mixing quaternary ammonium salt type modified silane, 3-chloroperoxybenzoic acid and methylene dichloride according to the mass ratio of 40:200:1000, reacting for 4 hours at the temperature of 1 ℃, filtering after the reaction is finished, washing for 3 times by adopting acetone, and drying for 16 hours at the temperature of 60 ℃ to obtain epoxy-terminated quaternary ammonium salt type modified silane;
Uniformly mixing dimethylbiphenyl diisocyanate, polytetrahydrofuran glycol and tetrahydrofuran according to the mass ratio of 30:10:10, and reacting for 5 hours at 70 ℃ and a rotating speed of 100r/min to obtain a polyurethane prepolymer; adding epoxy-terminated quaternary ammonium salt modified silane, glycerol and triisopropanolamine into the polyurethane prepolymer, uniformly mixing, heating for 2 hours at 100 ℃, and defoaming to obtain a soft-feel wet rubbing fastness improver;
wherein the mass ratio of the polyurethane prepolymer to the epoxy group-terminated quaternary ammonium salt modified silane to the glycerol to the triisopropanolamine is 80:4:2:0.8.
Example 2
The embodiment provides a preparation method of a wet rubbing fastness improver with soft hand feeling, which comprises the following steps:
step (1) mixing glycidoxy butyl trimethoxy silane, 2-chloro-1, 3-propanediol and N, N-dimethylformamide according to the mass ratio of 12:120:1200, reacting for 45.5 hours at the temperature of 62 ℃, and performing rotary evaporation to obtain modified silane;
Step (2) mixing modified silane, dimethylaminoethyl acrylate and acetone according to a mass ratio of 85:35:2000, reacting for 5.3 hours at a temperature of 27 ℃, filtering after the reaction is finished, washing with absolute ethyl alcohol, and drying for 7.5 hours at a temperature of 65 ℃ to obtain quaternary ammonium salt type modified silane;
Mixing quaternary ammonium salt type modified silane, 3-chloroperoxybenzoic acid and methylene dichloride according to the mass ratio of 45:250:1200 in a nitrogen atmosphere, reacting for 3.5 hours at the temperature of 2 ℃, filtering after the reaction is finished, washing for 3 times by adopting acetone, and drying for 15 hours at the temperature of 65 ℃ to obtain epoxy-terminated quaternary ammonium salt type modified silane;
Uniformly mixing dimethylbiphenyl diisocyanate, polytetrahydrofuran glycol and tetrahydrofuran according to the mass ratio of 40:12:15, and reacting for 4.3 hours at the temperature of 72 ℃ and the rotating speed of 125r/min to obtain a polyurethane prepolymer; adding epoxy-terminated quaternary ammonium salt modified silane, glycerol and triisopropanolamine into the polyurethane prepolymer, uniformly mixing, heating for 1.8h at 102 ℃, and defoaming to obtain a soft-feel wet rubbing fastness improver;
wherein the mass ratio of the polyurethane prepolymer to the epoxy group-terminated quaternary ammonium salt modified silane to the glycerol to the triisopropanolamine is 82:5.5:2.2:0.9.
Example 3
The embodiment provides a preparation method of a wet rubbing fastness improver with soft hand feeling, which comprises the following steps:
step (1) mixing glycidoxy butyl trimethoxy silane, 2-chloro-1, 3-propanediol and N, N-dimethylformamide according to the mass ratio of 15:140:1400, reacting for 43h at 65 ℃, and performing rotary evaporation to obtain modified silane;
Step (2) mixing modified silane, dimethylaminoethyl acrylate and acetone according to the mass ratio of 90:40:2500, reacting for 4.5 hours at the temperature of 30 ℃, filtering after the reaction is finished, washing with absolute ethyl alcohol, and drying for 7 hours at the temperature of 70 ℃ to obtain quaternary ammonium salt modified silane;
mixing quaternary ammonium salt type modified silane, 3-chloroperoxybenzoic acid and methylene dichloride according to the mass ratio of 50:300:1400 in a nitrogen atmosphere, reacting for 3 hours at the temperature of 3 ℃, filtering after the reaction is finished, washing for 3 times by adopting acetone, and drying for 14 hours at the temperature of 70 ℃ to obtain epoxy-terminated quaternary ammonium salt type modified silane;
uniformly mixing dimethylbiphenyl diisocyanate, polytetrahydrofuran glycol and tetrahydrofuran according to the mass ratio of 50:15:20, and reacting for 3.5 hours at the temperature of 75 ℃ and the rotating speed of 150r/min to obtain a polyurethane prepolymer; adding epoxy-terminated quaternary ammonium salt modified silane, glycerol and triisopropanolamine into the polyurethane prepolymer, uniformly mixing, heating for 1.5h at 105 ℃, and defoaming to obtain a soft-feel wet rubbing fastness improver;
wherein the mass ratio of the polyurethane prepolymer to the epoxy group-terminated quaternary ammonium salt modified silane to the glycerol to the triisopropanolamine is 85:7:2.5:1.
Example 4
The embodiment provides a preparation method of a wet rubbing fastness improver with soft hand feeling, which comprises the following steps:
step (1) mixing glycidoxy butyl trimethoxy silane, 2-chloro-1, 3-propanediol and N, N-dimethylformamide according to the mass ratio of 17:160:1600, reacting for 40.5 hours at 67 ℃, and performing rotary evaporation to obtain modified silane;
step (2) mixing modified silane, dimethylaminoethyl acrylate and acetone according to the mass ratio of 95:45:3000, reacting for 3.8 hours at the temperature of 32 ℃, filtering after the reaction is finished, washing with absolute ethyl alcohol, and drying for 6.5 hours at the temperature of 75 ℃ to obtain quaternary ammonium salt type modified silane;
Mixing quaternary ammonium salt type modified silane, 3-chloroperoxybenzoic acid and methylene dichloride according to the mass ratio of 55:350:1600 in a nitrogen atmosphere, reacting for 2.5 hours at the temperature of 4 ℃, filtering after the reaction is finished, washing for 3 times by adopting acetone, and drying for 13 hours at the temperature of 75 ℃ to obtain epoxy-terminated quaternary ammonium salt type modified silane;
Uniformly mixing dimethylbiphenyl diisocyanate, polytetrahydrofuran glycol and tetrahydrofuran according to the mass ratio of 60:17:25, and reacting for 2.8 hours at 77 ℃ and 175r/min to obtain a polyurethane prepolymer; adding epoxy-terminated quaternary ammonium salt modified silane, glycerol and triisopropanolamine into the polyurethane prepolymer, uniformly mixing, heating for 1.2h at the temperature of 107 ℃, and defoaming to obtain a wet rubbing fastness improver with soft hand feeling;
Wherein the mass ratio of the polyurethane prepolymer to the epoxy group-terminated quaternary ammonium salt modified silane to the glycerol to the triisopropanolamine is 87:8.5:2.7:1.1.
Example 5
The embodiment provides a preparation method of a wet rubbing fastness improver with soft hand feeling, which comprises the following steps:
Step (1) mixing glycidoxy butyl trimethoxy silane, 2-chloro-1, 3-propanediol and N, N-dimethylformamide according to the mass ratio of 20:180:1800, reacting for 38 hours at 70 ℃, and performing rotary evaporation to obtain modified silane;
Step (2) mixing modified silane, dimethylaminoethyl acrylate and acetone according to the mass ratio of 100:50:3500, reacting for 3 hours at the temperature of 35 ℃, filtering after the reaction, washing with absolute ethyl alcohol, and drying for 6 hours at the temperature of 80 ℃ to obtain quaternary ammonium salt modified silane;
mixing quaternary ammonium salt type modified silane, 3-chloroperoxybenzoic acid and methylene dichloride according to the mass ratio of 60:400:1800 in a nitrogen atmosphere, reacting for 2 hours at the temperature of 5 ℃, filtering after the reaction is finished, washing for 3 times by adopting acetone, and drying for 12 hours at the temperature of 80 ℃ to obtain epoxy-terminated quaternary ammonium salt type modified silane;
Uniformly mixing dimethylbiphenyl diisocyanate, polytetrahydrofuran glycol and tetrahydrofuran according to the mass ratio of 70:20:30, and reacting for 2 hours at 80 ℃ and a rotating speed of 200r/min to obtain a polyurethane prepolymer; adding epoxy-terminated quaternary ammonium salt modified silane, glycerol and triisopropanolamine into the polyurethane prepolymer, uniformly mixing, heating for 1h at 110 ℃, and defoaming to obtain a soft-feel wet rubbing fastness improver;
wherein the mass ratio of the polyurethane prepolymer to the epoxy group-terminated quaternary ammonium salt modified silane to the glycerol to the triisopropanolamine is 90:10:3:1.2.
Comparative example 1
The comparative example provides a method for preparing a wet rubbing fastness improver with soft hand feeling, which comprises the following steps:
Step (1) mixing glycidoxy butyl trimethoxy silane, 2-chloro-1, 3-propanediol and N, N-dimethylformamide according to the mass ratio of 10:100:1000, reacting for 48 hours at 60 ℃, and performing rotary evaporation to obtain modified silane;
step (2) mixing modified silane, dimethylaminoethyl acrylate and acetone according to the mass ratio of 80:30:1500, reacting for 6 hours at the temperature of 25 ℃, filtering after the reaction is finished, washing with absolute ethyl alcohol, and drying for 8 hours at the temperature of 60 ℃ to obtain quaternary ammonium salt modified silane;
Uniformly mixing dimethylbiphenyl diisocyanate, polytetrahydrofuran glycol and tetrahydrofuran according to the mass ratio of 30:10:10, and reacting for 5 hours at 70 ℃ and a rotating speed of 100r/min to obtain a polyurethane prepolymer; adding quaternary ammonium salt modified silane, glycerol and triisopropanolamine into the polyurethane prepolymer, uniformly mixing, heating for 2 hours at 100 ℃, and defoaming to obtain a wet rubbing fastness improver with soft hand feeling;
Wherein the mass ratio of the polyurethane prepolymer to the quaternary ammonium salt modified silane to the triisopropanolamine is 80:4:2:0.8.
Comparative example 2
The comparative example provides a method for preparing a wet rubbing fastness improver with soft hand feeling, which comprises the following steps:
Step (1) mixing glycidoxy butyl trimethoxy silane, 2-chloro-1, 3-propanediol and N, N-dimethylformamide according to the mass ratio of 10:100:1000, reacting for 48 hours at 60 ℃, and performing rotary evaporation to obtain modified silane;
uniformly mixing dimethylbiphenyl diisocyanate, polytetrahydrofuran glycol and tetrahydrofuran according to the mass ratio of 30:10:10, and reacting for 5 hours at 70 ℃ and a rotating speed of 100r/min to obtain a polyurethane prepolymer; adding modified silane, glycerol and triisopropanolamine into the polyurethane prepolymer, uniformly mixing, heating for 2 hours at 100 ℃, and defoaming to obtain a wet rubbing fastness improver with soft hand feeling;
wherein the mass ratio of the polyurethane prepolymer to the modified silane to the triisopropanolamine is 80:4:2:0.8.
In the examples and comparative examples, 2-chloro-1, 3-propanediol was obtained from Guangdong Weng Jiang chemical reagent Co., ltd., CAS number 497-04-1, dimethylaminoethyl acrylate was obtained from Shanghai China Fluotai chemical Co., ltd., CAS number 2439-35-2, polytetrahydrofuran diol was obtained from Jinliduo chemical Co., ltd., content not less than 99 (%), product P1000, glycerol was obtained from Wuhan Jixin Yibang Biotechnology Co., ltd., 56-81-5, dimethylbiphenyl diisocyanate was obtained from Shanghai Taitan technology Co., ltd., CAS number 91-97-4, tetrahydrofuran was obtained from Shanxi Ruijia optima Co., ltd., CAS number 109-99-9.
The soft hand wet crock fastness improving agent prepared in examples 1-5 and comparative examples 1-2 was tested, using a cotton fabric, using a soft hand wet crock fastness improving agent of 15g/L, according to the process flow of one padding (mill residue: 70%) → setting (180 ° Cx60 s) → moisture regain→ performance evaluation, wherein the test items were as follows:
(1) Wet rubbing fastness test, namely testing according to GB/T3920-2008 "rubbing fastness to textile color fastness test", the specific results are shown in Table 1;
(2) Washing resistance test, namely after fixing color of cotton fabric by using a soft-hand wet rubbing fastness improver according to the standard of 5g/L, recording wet rubbing fastness of cotton fabric subjected to washing for 50 times, wherein the specific results are shown in table 1;
(3) The softness performance test comprises the steps of evaluating by a hand touch method, namely, feeling the softness, smoothness, fluffiness and the like of the fabric through hand touch, wherein the softness performance of a person with optimal hand feeling is specified as 5 grades, the softness performance grade of an unfinished fabric is specified as 1 grade, and the softness performance of other finished fabrics is rated relative to the standard, wherein the specific test results are shown in table 1;
TABLE 1
As shown in the test results of Table 1, the wet rubbing fastness improver with soft hand feeling prepared by the invention has good wet rubbing fastness and water washing resistance, and can increase the soft hand feeling when being applied to fabrics. In the embodiment 1, double bonds contained in the quaternary ammonium salt modified silane have instability, carbon-carbon double bonds can be subjected to epoxidation under the action of 3-chloroperoxybenzoic acid, on one hand, the formation of epoxy groups increases stability, on the other hand, the epoxy groups can react with hydroxyl groups, amino groups and the like on the fabric to form stable covalent bonds so as to promote wet rubbing fastness and increase water resistance, meanwhile, the tight and uniform combination mode is favorable for keeping the original structure and flexibility of the fabric fiber, so that the softness is better kept or even improved, once the wet rubbing fastness and the water resistance of the embodiment 1 are reduced, the softness level of the embodiment 1 is higher than that of the embodiment 1, in the embodiment 2, the formation of quaternary ammonium salt is reduced, so that the wet rubbing fastness and the water resistance of the embodiment 1 are better than those of the embodiment 2, and the addition of dimethylaminoethyl acrylate is not needed, the long-chain structure is reduced, and the softness level of the embodiment 1 is higher than that of the embodiment 2.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made hereto without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. A method for preparing a soft-feel wet rubbing fastness improver, which is characterized by comprising the following steps:
Step (1) adding epoxy organosilane and 2-chloro-1, 3-propanediol into N, N-dimethylformamide, mixing, heating, reacting, and performing rotary evaporation to obtain modified silane;
adding modified silane and dimethylaminoethyl acrylate into acetone, reacting, filtering, washing and drying to obtain quaternary ammonium salt modified silane;
under the nitrogen atmosphere, adding quaternary ammonium salt type modified silane and 3-chloroperoxybenzoic acid into methylene dichloride, reacting at a low temperature, filtering, washing and drying to obtain epoxy-terminated quaternary ammonium salt type modified silane;
And (4) heating and stirring dimethyl diphenyl diisocyanate, polyether glycol and tetrahydrofuran to obtain a polyurethane prepolymer, and adding epoxy-terminated quaternary ammonium salt modified silane, a chain extender and a catalyst into the polyurethane prepolymer, uniformly mixing, heating and defoaming to obtain the wet friction fastness improver with soft hand feeling.
2. The method for preparing a wet rubbing fastness improver with soft hand feel according to claim 1, wherein in the step (1), the mass ratio of epoxy organosilane, 2-chloro-1, 3-propanediol and N, N-dimethylformamide is (10-20): (100-180): (1000-1800), the reaction temperature is 60-70 ℃ and the reaction time is 38-48h.
3. The method for preparing a soft-touch wet crockfastness improver according to claim 1, wherein in the step (2), the mass ratio of the modified silane, dimethylaminoethyl acrylate and acetone is (80-100): (30-50): (1500-3500).
4. The method for preparing the wet rubbing fastness improver with soft hand feeling according to claim 1, wherein in the step (3), the mass ratio of the quaternary ammonium salt type modified silane to the 3-chloroperoxybenzoic acid to the dichloromethane is (40-60): 200-400): 1000-1800, the reaction temperature is 1-5 ℃ and the reaction time is 2-4h.
5. The method for preparing a soft touch wet crockfastness improving agent according to claim 1, wherein the polyether glycol is any one of polytetrahydrofuran glycol and polyethylene oxide glycol.
6. The method for preparing the wet rubbing fastness improver with soft hand feeling according to claim 1, wherein in the step (4), the mass ratio of the dimethylbiphenyl diisocyanate to the polyether glycol to the tetrahydrofuran is (30-70): 10-20): 10-30, and the reaction condition is 70-80 ℃ for 2-5 hours.
7. The method of claim 1, wherein in step (4), the chain extender comprises glycerol and the catalyst comprises triisopropanolamine.
8. The method for preparing the wet rubbing fastness improver with soft hand feel according to claim 1, wherein in the step (4), the mass ratio of the polyurethane prepolymer to the epoxy group-terminated quaternary ammonium salt modified silane to the chain extender to the catalyst is (80-90): 4-10): 2-3): 0.8-1.2.
9. The method for preparing a wet crock fastness enhancing agent for soft hand feel according to claim 1, wherein in the step (4), the temperature of the second heating is 100-110 ℃ and the heating time is 1-2h.
10. A soft feel wet crockfastness improving agent prepared by the method for preparing a soft feel wet crockfastness improving agent according to any one of claims 1 to 9.
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Citations (2)
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|---|---|---|---|---|
| CN104761723A (en) * | 2015-04-09 | 2015-07-08 | 南丰县大信科技有限公司 | Polysiloxane softening agent with color fixing property |
| CN111423940A (en) * | 2020-04-15 | 2020-07-17 | 湖南杨家将茶油股份有限公司 | Preparation process of camellia oil detergent |
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| CN101565896B (en) * | 2008-12-22 | 2011-07-27 | 上海氟聚化学产品有限公司 | Quaternary amino cation modified polysiloxane softening agent and preparation method thereof |
| CN113584912B (en) * | 2021-09-09 | 2023-04-07 | 苏州联胜化学有限公司 | Multifunctional color fastness improver for impregnation and preparation method thereof |
| CN116180450B (en) * | 2022-12-17 | 2024-10-18 | 广东湛丰精细化工有限公司 | Wet rubbing fastness improver with high energy efficiency and soft hand feeling and preparation method thereof |
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| CN104761723A (en) * | 2015-04-09 | 2015-07-08 | 南丰县大信科技有限公司 | Polysiloxane softening agent with color fixing property |
| CN111423940A (en) * | 2020-04-15 | 2020-07-17 | 湖南杨家将茶油股份有限公司 | Preparation process of camellia oil detergent |
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