A soft-feel wet rubbing fastness improver and its preparation method

Abstract

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

[0001] The present application relates to the technical field of textile chemicals, in particular to a soft-hand wet rubbing fastness improver and a preparation method thereof. BACKGROUND

[0002] At present, with the improvement of consumption level, people have higher and higher requirements on the quality of clothing performance. The wet rubbing fastness of water-soluble dyes such as direct dyes, reactive dyes and acid dyes cannot meet the requirements of customers. The wet rubbing fastness of color is an important indicator of clothing performance, which refers to the degree of color transfer from the surface of dyed fabric to the surface of other objects in contact with it under the action of friction in a wet state. It is an important indicator in textile color fastness testing, which is used to evaluate the fastness of color of dyed fabric in actual use process (such as washing, wearing and contacting with water in wet environment). At present, dyers can choose dyes with relatively high fastness or use smooth agents to smooth and soften the fabric to reduce the friction resistance and friction coefficient, and improve the wet rubbing fastness of dyed fabric. However, these methods can only improve the wet rubbing fastness of fabric to a certain extent.

[0003] Chinese patent CN101503860B discloses a dyed fabric wet rubbing fastness improver, which is a non-ionic polymer prepared by mixing low hydrogen-containing silicone oil, polyurethane prepolymer and polyacrylic acid-maleic acid copolymer in a mass ratio of (10-30):(30-60):(20-40) under catalytic heating conditions, but the dyed fabric wet rubbing fastness improver prepared by the present application needs to improve the soft hand feeling of the fabric; Chinese patent CN112341597B discloses a preparation method of water-based polyurethane wet rubbing fastness improver, a proper amount of polycaprolactone triol is added to the reactor for high-temperature vacuum dehydration treatment; the temperature of the reactor is reduced to 60℃, a proper amount of diisocyanate is added, and the reaction is carried out for 2h, then the temperature is increased to 75℃, and the reaction is carried out for 3h to obtain polyurethane prepolymer; a proper amount of hydrophilic chain extender is added to the reactor for chain extension and heat preservation reaction; a proper amount of small molecule polyol is added to the reactor for chain extension and heat preservation reaction; a proper amount of triethylamine is added to the reactor to adjust the pH to 6-7; the temperature of the reactor is reduced to room temperature, and water is added to emulsify uniformly to obtain a water-based polyurethane wet rubbing fastness improver, but the wet rubbing fastness of the water-based polyurethane wet rubbing fastness improver prepared by the present application is 3, and the wet rubbing fastness performance needs to be further improved. SUMMARY

[0004] In order to solve the above technical problems, the present application provides a soft-hand wet rubbing fastness improver and a preparation method thereof, which solves the problems of low fastness and low soft-hand effect of the wet rubbing fastness improver used in the prior art.

[0005] To achieve the above object, the application provides a preparation method of a soft-hand wet rubbing fastness improver, comprising the following steps:

[0006] Step (1) adding epoxy organosilane and 2-chloro-1,3-propanediol into N,N-dimethylformamide, heating, reacting, stopping the reaction, rotary evaporation, and obtaining modified silane;

[0007] Step (2) adding the modified silane and dimethylaminoethyl acrylate into acetone, reacting, stopping the reaction, filtering, washing, drying, and obtaining quaternary ammonium salt type modified silane;

[0008] Step (3) adding the quaternary ammonium salt type modified silane and 3-chlorine peroxyl benzoic acid into dichloromethane under nitrogen atmosphere, reacting under low temperature, stopping the reaction, filtering, washing, drying, and obtaining epoxy group terminated quaternary ammonium salt type modified silane;

[0009] Step (4) heating and stirring dimethyl biphenyl diisocyanate, polyether diol and tetrahydrofuran to obtain polyurethane prepolymer; adding the epoxy group terminated quaternary ammonium salt type modified silane, chain extender and catalyst into the polyurethane prepolymer, mixing uniformly, heating, and defoaming to obtain the soft-hand wet rubbing fastness improver.

[0010] Preferably, in step (1), the mass ratio of the epoxy silane, 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.

[0011] Preferably, in step (1), the epoxy organosilane is any one of 2-(3,4-epoxycyclohexane) ethyl trimethoxysilane, epoxy propoxy octyl trimethoxysilane, epoxy propoxy butyl trimethoxysilane and epoxy propoxy propyl methyl dimethoxysilane.

[0012] Preferably, in step (2), the mass ratio of the epoxy organosilane, dimethylaminoethyl acrylate and acetone is (80-100):(30-50):(1500-3500).

[0013] Preferably, in step (3), the mass ratio of the quaternary ammonium salt type modified silane, 3-chlorine peroxyl benzoic acid and dichloromethane is (40-60):(200-400):(1000-1800); the reaction temperature is 1-5℃, and the reaction time is 2-4h.

[0014] Preferably, the polyether diol is any one of polytetrahydrofuran diol and polyethylene oxide diol.

[0015] Preferably, in step (4), the mass ratio of dimethyl diphenyl diisocyanate, polyether diol and tetrahydrofuran is (30-70):(10-20):(10-30); the reaction condition is 70-80 DEG C for 2-5h.

[0016] Preferably, in step (4), the chain extender comprises glycerol; and the catalyst comprises triisopropanolamine.

[0017] Preferably, in step (4), the mass ratio of polyurethane prepolymer, end epoxy group modified silane of quaternary ammonium salt type, chain extender and catalyst is (80-90):(4-10):(2-3):(0.8-1.2).

[0018] Preferably, in step (4), the second heating temperature is 100-110 DEG C, and the heating time is 1-2h.

[0019] Preferably, the soft hand feeling wet rubbing fastness improver is prepared by the preparation method of the soft hand feeling wet rubbing fastness improver.

[0020] Preferably, the soft hand feeling wet rubbing fastness improver is applied to a fabric.

[0021] Preferably, the fabric comprises cotton fabric, polyester cotton fabric and nylon fabric.

[0022] Compared with the prior art, the present application has the following beneficial effects:

[0023] 1. In the present application, the epoxy organosilane has certain heat resistance, contains long chain structure, and endows it with certain softness, the epoxy group in the epoxy organosilane and the hydroxyl group in 2-chloro-1,3-propanediol react to form an ether group with stronger chemical stability and better water resistance; the chlorine group in the modified silane can react with the tertiary amine group in dimethylaminoethyl acrylate to form a quaternary ammonium salt type modified silane, at this time there are quaternary ammonium salt cation groups and silicon hydroxyl groups in the epoxy organosilane, the quaternary ammonium salt cation groups have strong polarity and can react with the anion of the dye to form insoluble dye salt precipitate to fix the dye on the fabric, and the silicon hydroxyl groups have strong reactivity and can react with the active groups such as hydroxyl groups and amino groups of the dye on the fabric during the drying process to form stable chemical bonds to further fix the dye on the fabric; at the same time, the long chain structure in dimethylaminoethyl acrylate can enhance the flexibility of the polymer, and the lack of it will lead to a more compact polymer structure, thereby affecting the softness of the fabric. The unsaturated double bond contained in the quaternary ammonium salt type modified silane can form an epoxy group with better stability under the action of 3-chloroperoxybenzoic acid, and the epoxy group can react with the hydroxyl group, amino group, etc. on the fabric to form stable covalent bonds, promote wet rubbing fastness, increase water resistance, and at the same time, this close and uniform combination is conducive to maintaining the original structure and flexibility of the fabric fibers, thereby better maintaining or even improving the softness; the quaternary ammonium salt type modified silane with terminal epoxy group contains ether group, hydroxyl group and epoxy group, which can further react with polyurethane prepolymer to form a cross-linked structure, endowing the fabric with good elasticity, and forming a film layer with certain fastness on the textile material, thereby improving the washing fastness and wet rubbing fastness of the fixing agent.

[0024] 2. The soft-hand wet rubbing fastness improver prepared by the present application is a polyether type polyurethane containing quaternary ammonium salt and epoxy group, which has good performance, and the fabric treated with it not only has better softness, but also has improved wet rubbing fastness and washing resistance, and can also endow the fabric with the properties of fullness, air permeability, comfort, softness, brightness and antistatic property. BRIEF DESCRIPTION OF DRAWINGS

[0025] Figure 1 The preparation process flow chart of the soft-hand wet rubbing fastness improver in the present application. DETAILED DESCRIPTION

[0026] The technical solutions of the present application will be described below in conjunction with the embodiments, obviously, the described embodiments are only part of the embodiments of the present application, not all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor are within the scope of protection of the present application.

[0027] Example 1

[0028] The embodiment provides a preparation method of a soft-hand wet rubbing fastness improver, and the method comprises the following steps:

[0029] Step (1), epoxypropoxybutyltrimethoxysilane, 2-chloro-1,3-propanediol and N,N-dimethylformamide are mixed according to a mass ratio of 10:100:1000, and reaction is carried out at 60 DEG C for 48h; after the reaction is completed, rotary evaporation is carried out, and modified silane is obtained;

[0030] Step (2), the modified silane, dimethylaminoethyl acrylate and acetone are mixed according to a mass ratio of 80:30:1500, and reaction is carried out at 25 DEG C for 6h; after the reaction is completed, filtration is carried out, the filter is washed with anhydrous ethanol, and drying is carried out at 60 DEG C for 8h, so that the quaternary ammonium salt type modified silane is obtained;

[0031] Step (3), the quaternary ammonium salt type modified silane, 3-chlorine peroxyl benzoic acid and dichloromethane are mixed according to a mass ratio of 40:200:1000 under a nitrogen atmosphere, and reaction is carried out at 1 DEG C for 4h; after the reaction is completed, filtration is carried out, washing with acetone is carried out for 3 times, and drying is carried out at 60 DEG C for 16h, so that the quaternary ammonium salt type modified silane with an epoxy group at the end is obtained;

[0032] Step (4), dimethyl diphenyl diisocyanate, polytetrahydrofuran diol and tetrahydrofuran are uniformly mixed according to a mass ratio of 30:10:10, and reaction is carried out at 70 DEG C and a rotation speed of 100r / min for 5h, so that a polyurethane prepolymer is obtained; the quaternary ammonium salt type modified silane with an epoxy group at the end, glycerol and triisopropanolamine are uniformly mixed in the polyurethane prepolymer, and heating is carried out at 100 DEG C for 2h, so that the soft-hand wet rubbing fastness improver is obtained after defoaming;

[0033] The mass ratio of the polyurethane prepolymer, the quaternary ammonium salt type modified silane with an epoxy group at the end, the glycerol and the triisopropanolamine is 80:4:2:0.8.

[0034] Embodiment 2

[0035] The embodiment provides a preparation method of a soft-hand wet rubbing fastness improver, and the method comprises the following steps:

[0036] Step (1), epoxypropoxybutyltrimethoxysilane, 2-chloro-1,3-propanediol and N,N-dimethylformamide are mixed according to a mass ratio of 12:120:1200, and reaction is carried out at 62 DEG C for 45.5h; after the reaction is completed, rotary evaporation is carried out, and modified silane is obtained;

[0037] Step (2) mixing the modified silane, dimethylaminoethyl acrylate and acetone according to the mass ratio of 85:35:2000, reacting for 5.3 h at 27℃, filtering after the reaction is completed, washing with anhydrous ethanol, and drying at 65℃ for 7.5 h to obtain the quaternary ammonium salt type modified silane;

[0038] Step (3) mixing the quaternary ammonium salt type modified silane, 3-chloroperbenzoic acid and dichloromethane according to the mass ratio of 45:250:1200 under a nitrogen atmosphere, reacting for 3.5 h at 2℃, filtering after the reaction is completed, washing with acetone for 3 times, and drying at 65℃ for 15 h to obtain the epoxy-terminated quaternary ammonium salt type modified silane;

[0039] Step (4) uniformly mixing dimethyl diphenyl diisocyanate, polytetrahydrofuran diol and tetrahydrofuran according to the mass ratio of 40:12:15, reacting for 4.3 h at 72℃ and a rotating speed of 125 r / min to obtain a polyurethane prepolymer; uniformly mixing the epoxy-terminated quaternary ammonium salt type modified silane, glycerol and triisopropanolamine into the polyurethane prepolymer, heating at 102℃ for 1.8 h, and defoaming to obtain the soft-hand wet rubbing fastness enhancer;

[0040] The mass ratio of the polyurethane prepolymer, the epoxy-terminated quaternary ammonium salt type modified silane, the glycerol and the triisopropanolamine is 82:5.5:2.2:0.9.

[0041] Example 3

[0042] The embodiment provides a preparation method of a soft-hand wet rubbing fastness enhancer, including the following steps:

[0043] Step (1) mixing epoxypolybutyltrimethoxysilane, 2-chloro-1,3-propanediol and N,N-dimethylformamide according to the mass ratio of 15:140:1400, reacting for 43 h at 65℃, and obtaining the modified silane by rotary evaporation after the reaction is completed;

[0044] Step (2) mixing the modified silane, dimethylaminoethyl acrylate and acetone according to the mass ratio of 90:40:2500, reacting for 4.5 h at 30℃, filtering after the reaction is completed, washing with anhydrous ethanol, and drying at 70℃ for 7 h to obtain the quaternary ammonium salt type modified silane;

[0045] Step (3) mixing the quaternary ammonium salt type modified silane, 3-chloroperbenzoic acid and dichloromethane according to the mass ratio of 50:300:1400 under a nitrogen atmosphere, reacting for 3 h at 3℃, filtering after the reaction is completed, washing with acetone for 3 times, and drying at 70℃ for 14 h to obtain the epoxy-terminated quaternary ammonium salt type modified silane;

[0046] Step (4) mixing dimethyl diphenyl diisocyanate, polytetrahydrofuran diol and tetrahydrofuran uniformly according to the mass ratio of 50:15:20, reacting at 75℃, 150r / min rotating speed for 3.5h, obtaining polyurethane prepolymer; adding the epoxy group terminated quaternary ammonium salt type modified silane, glycerol, triisopropanol amine into the polyurethane prepolymer, mixing uniformly, heating at 105℃ for 1.5h, defoaming, obtaining the soft hand feeling wet rubbing fastness improver;

[0047] The mass ratio of the polyurethane prepolymer, the epoxy group terminated quaternary ammonium salt type modified silane, the glycerol and the triisopropanol amine is 85:7:2.5:1.

[0048] Example 4

[0049] The embodiment provides a preparation method of a soft hand feeling wet rubbing fastness improver, comprising the following steps:

[0050] Step (1) mixing epoxy propoxy butyl trimethoxysilane, 2-chloro-1,3-propanediol and N,N-dimethylformamide according to the mass ratio of 17:160:1600, reacting at 67℃ for 40.5h, after the reaction, rotary evaporation, obtaining the modified silane;

[0051] Step (2) mixing the modified silane, dimethylaminoethyl acrylate and acetone according to the mass ratio of 95:45:3000, reacting at 32℃ for 3.8h, after the reaction, filtering, washing with anhydrous ethanol, drying at 75℃ for 6.5h, obtaining the quaternary ammonium salt type modified silane;

[0052] Step (3) mixing the quaternary ammonium salt type modified silane, 3-chloro peroxi benzoic acid and dichloromethane according to the mass ratio of 55:350:1600 under the nitrogen atmosphere, reacting at 4℃ for 2.5h, after the reaction, filtering, washing with acetone for 3 times, drying at 75℃ for 13h, obtaining the epoxy group terminated quaternary ammonium salt type modified silane;

[0053] Step (4) mixing dimethyl diphenyl diisocyanate, polytetrahydrofuran diol and tetrahydrofuran uniformly according to the mass ratio of 60:17:25, reacting at 77℃, 175r / min rotating speed for 2.8h, obtaining polyurethane prepolymer; adding the epoxy group terminated quaternary ammonium salt type modified silane, glycerol, triisopropanol amine into the polyurethane prepolymer, mixing uniformly, heating at 107℃ for 1.2h, defoaming, obtaining the soft hand feeling wet rubbing fastness improver;

[0054] The mass ratio of the polyurethane prepolymer, the epoxy group terminated quaternary ammonium salt type modified silane, the glycerol and the triisopropanol amine is 87:8.5:2.7:1.1.

[0055] Example 5

[0056] The embodiment provides a preparation method of a soft-hand wet rubbing fastness improver, and comprises the following steps:

[0057] Step (1), epoxypropoxybutyltrimethoxysilane, 2-chloro-1, 3-propanediol and N, N-dimethylformamide are mixed according to a mass ratio of 20:180:1800, reaction is carried out at 70 DEG C for 38h, after the reaction is completed, rotary evaporation is carried out, and modified silane is obtained;

[0058] Step (2), the modified silane, dimethylaminoethyl acrylate and acetone are mixed according to a mass ratio of 100:50:3500, reaction is carried out at 35 DEG C for 3h, after the reaction is completed, filtration is carried out, the filter is washed with anhydrous ethanol, and drying is carried out at 80 DEG C for 6h, so that the quaternary ammonium salt type modified silane is obtained;

[0059] Step (3), the quaternary ammonium salt type modified silane, 3-chlorine peroxyl benzoic acid and dichloromethane are mixed according to a mass ratio of 60:400:1800 under a nitrogen atmosphere, reaction is carried out at 5 DEG C for 2h, after the reaction is completed, filtration is carried out, washing is carried out with acetone for 3 times, and drying is carried out at 80 DEG C for 12h, so that the quaternary ammonium salt type modified silane with an epoxy group at the end is obtained;

[0060] Step (4), dimethyl diphenyl diisocyanate, polytetrahydrofuran diol and tetrahydrofuran are uniformly mixed according to a mass ratio of 70:20:30, reaction is carried out at 80 DEG C and a rotation speed of 200r / min for 2h, so that a polyurethane prepolymer is obtained; the quaternary ammonium salt type modified silane with an epoxy group at the end, glycerol and triisopropanolamine are uniformly mixed in the polyurethane prepolymer, heating is carried out at 110 DEG C for 1h, and defoaming is carried out, so that the soft-hand wet rubbing fastness improver is obtained;

[0061] In the embodiment, the mass ratio of the polyurethane prepolymer, the quaternary ammonium salt type modified silane with an epoxy group at the end, the glycerol and the triisopropanolamine is 90:10:3:1.2.

[0062] Comparative Example 1

[0063] The comparative example provides a preparation method of a soft-hand wet rubbing fastness improver, and comprises the following steps:

[0064] Step (1), epoxypropoxybutyltrimethoxysilane, 2-chloro-1, 3-propanediol and N, N-dimethylformamide are mixed according to a mass ratio of 10:100:1000, reaction is carried out at 60 DEG C for 48h, after the reaction is completed, rotary evaporation is carried out, and modified silane is obtained;

[0065] Step (2), the modified silane, dimethylaminoethyl acrylate and acetone are mixed according to a mass ratio of 80:30:1500, reaction is carried out at 25 DEG C for 6h, after the reaction is completed, filtration is carried out, the filter is washed with anhydrous ethanol, and drying is carried out at 60 DEG C for 8h, so that the quaternary ammonium salt type modified silane is obtained;

[0066] Step (3) uniformly mix dimethyl diphenyl diisocyanate, polytetrahydrofuran diol and tetrahydrofuran in a mass ratio of 30:10:10, and react at 70 DEG C and a rotation speed of 100 r / min for 5 h to obtain a polyurethane prepolymer; add quaternary ammonium salt type modified silane, glycerol and triisopropanolamine into the polyurethane prepolymer, uniformly mix, heat at 100 DEG C for 2 h, and defoam to obtain a soft-hand wet rubbing fastness enhancer;

[0067] The mass ratio of the polyurethane prepolymer, the quaternary ammonium salt type modified silane, the glycerol and the triisopropanolamine is 80:4:2:0.8.

[0068] Comparative Example 2

[0069] The present comparative example provides a preparation method of a soft-hand wet rubbing fastness enhancer, comprising the following steps:

[0070] Step (1) mix epoxpropoxybutyltrimethoxysilane, 2-chloro-1,3-propanediol and N,N-dimethylformamide in a mass ratio of 10:100:1000, and react at 60 DEG C for 48 h; after the reaction is completed, spin evaporation is performed to obtain a modified silane;

[0071] Step (2) uniformly mix dimethyl diphenyl diisocyanate, polytetrahydrofuran diol and tetrahydrofuran in a mass ratio of 30:10:10, and react at 70 DEG C and a rotation speed of 100 r / min for 5 h to obtain a polyurethane prepolymer; add the modified silane, glycerol and triisopropanolamine into the polyurethane prepolymer, uniformly mix, heat at 100 DEG C for 2 h, and defoam to obtain a soft-hand wet rubbing fastness enhancer;

[0072] The mass ratio of the polyurethane prepolymer, the modified silane, the glycerol and the triisopropanolamine is 80:4:2:0.8.

[0073] In the present example and the comparative example, the 2-chloro-1,3-propanediol is from Guangdong Wengjiang Chemical Reagent Co., Ltd., and the CAS number is 497-04-1; the dimethylaminoethyl acrylate is from Shanghai Huafu Tai Chemical Co., Ltd., and the CAS number is 2439-35-2; the polytetrahydrofuran diol is from Jining Lido Chemical Co., Ltd., and the content is greater than or equal to 99(%), and the product is P1000; the glycerol is from Wuhan Jixin Yibang Biological Technology Co., Ltd., and the CAS number is 56-81-5; the dimethyl diphenyl diisocyanate is from Shanghai Titan Science and Technology Co., Ltd., and the CAS number is 91-97-4; and the tetrahydrofuran is from Shaanxi Ruigia Optimization Chemical Co., Ltd., and the CAS number is 109-99-9.

[0074] The soft hand wet rubbing fastness enhancer prepared in Examples 1-5 and Comparative Examples 1-2 is tested, the fabric is cotton fabric, the soft hand wet rubbing fastness enhancer is used in an amount of 15 g / L, and the process flow is: one dip and one roll (pick-up rate: 70%) → setting (180 ℃ x 60 s) → moisture regain → performance evaluation; wherein the test items are as follows:

[0075] (1) Wet rubbing fastness test: tested according to GB / T 3920-2008 “Textiles - Colour fastness to rubbing”, and the specific results are shown in Table 1;

[0076] (2) Wash resistance test: after the soft hand wet rubbing fastness enhancer is fixed on the cotton fabric according to the standard of 5 g / L, the wet rubbing fastness of the cotton fabric after 50 times of washing is recorded, and the specific results are shown in Table 1;

[0077] (3) Softness test: the hand touch method is used for evaluation, that is, the softness, smoothness and bulkiness of the fabric are felt by hand touch, and the comparison standard is that the softness of the best one is rated as 5; the softness of the unfinishing fabric is rated as 1; and the softness of other finishing fabrics is rated according to the standard, and the specific test results are shown in Table 1;

[0078] Table 1

[0079]

[0080] From the test results in Table 1, it can be seen that the soft hand wet rubbing fastness enhancer prepared by the application has good wet rubbing fastness and wash resistance, and it can increase the soft hand feeling when applied to the fabric. In Example 1, the double bond contained in the quaternary ammonium salt modified silane is unstable, and under the action of 3-chloro peroxobenzoic acid, the carbon-carbon double bond can be epoxidized, and the formation of the epoxy group increases the stability on the one hand, and on the other hand, it can react with the hydroxyl group, amino group and the like on the fabric to form a stable covalent bond, thereby improving the wet rubbing fastness and increasing the water resistance. At the same time, this close and uniform combination mode is beneficial to maintaining the original structure and flexibility of the fabric fibers, so that the softness is well maintained or even improved. Once it is lacking, the performance is reduced, so the wet rubbing fastness and wash resistance of Example 1 are better than those of Comparative Example 1, and the softness grade of Example 1 is higher than that of Comparative Example 1. In Comparative Example 2, the quaternary ammonium salt is not formed compared with Comparative Example 1, so the wet rubbing fastness and wash resistance of Comparative Example 1 are better than those of Comparative Example 2, and without the addition of dimethylaminoethyl acrylate, the long chain structure is reduced, and the flexibility is reduced, so the softness grade of Comparative Example 1 is higher than that of Comparative Example 2.

[0081] While the embodiments of the application have been shown and described, it is to be understood that the application is not limited to these embodiments. Since modifications, variations, substitutions and changes can be made to these embodiments without departing from the spirit and the principles of the application, it is intended that the application be understood as not being limited to the particular embodiments described and that the scope of the application is to be interpreted only in accordance with the appended claims.

Claims

1. A process for the preparation of a soft hand wet rub fastness enhancer characterized in that, The method comprises the following steps: Step (1) adding epoxy organosilane and 2-chloro-1,3-propanediol into N,N-dimethylformamide, heating, reacting, ending the reaction, rotary evaporation, and obtaining modified silane; Step (2) adding modified silane and dimethylaminoethyl acrylate into acetone, reacting, ending the reaction, filtering, washing, drying, and obtaining quaternary ammonium salt type modified silane; Step (3) under the atmosphere of nitrogen, adding quaternary ammonium salt type modified silane and 3-chlorine peroxyl benzoic acid into dichloromethane, reacting under low temperature, ending the reaction, filtering, washing, drying, and obtaining end epoxy group quaternary ammonium salt type modified silane; Step (4) heating and stirring dimethyl diphenyl diisocyanate, polyether diol and tetrahydrofuran to obtain polyurethane prepolymer; adding end epoxy group quaternary ammonium salt type modified silane, chain extender and catalyst into the polyurethane prepolymer, mixing uniformly, heating, and defoaming to obtain soft hand feeling wet rubbing fastness improver.

2. The process for preparing a soft hand wet rub fastness booster according to claim 1, characterized in that, In 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 process for preparing a soft hand wet rub fastness enhancer according to claim 1, characterized in that, In step (2), the mass ratio of modified silane, dimethylaminoethyl acrylate and acetone is (80-100):(30-50):(1500-3500).

4. The process for preparing a soft hand wet rub fastness enhancer according to claim 1, characterized in that, In step (3), the mass ratio of quaternary ammonium salt type modified silane, 3-chlorine peroxyl benzoic acid and dichloromethane is (40-60):(200-400):(1000-1800); the reaction temperature is 1-5℃, and the reaction time is 2-4h.

5. The process for preparing a soft hand wet rub fastness enhancer according to claim 1, characterized in that, The polyether diol is any one of polytetrahydrofuran diol and polyoxyethylene diol.

6. The process for preparing a soft hand wet rub fastness enhancer according to claim 1, characterized in that, In step (4), the mass ratio of dimethyl diphenyl diisocyanate, polyether diol and tetrahydrofuran is (30-70):(10-20):(10-30); the reaction condition is 70-80℃ for 2-5h.

7. The process for preparing a soft hand wet rub fastness booster according to claim 1, characterized in that, The chain extender includes glycerol; and the catalyst includes triisopropyl alcohol amine.

8. The process for preparing a soft hand wet rub fastness enhancer according to claim 1, characterized in that, In step (4), the mass ratio of polyurethane prepolymer, end epoxy group quaternary ammonium salt type modified silane, chain extender and catalyst is (80-90):(4-10):(2-3):(0.8-1.2).

9. The process for preparing a soft hand wet rub fastness enhancer according to claim 1, characterized in that, In step (4), the temperature of the second heating is 100-110℃, and the heating time is 1-2h. 10.A soft hand feeling wet rubbing fastness improver prepared by the method in any one of claims 1-9.

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