A hydrophilic fluffy dendritic block silicone oil and preparation method thereof

Abstract

The invention relates to the field of textile auxiliaries, and in particular to a hydrophilic fluffy dendritic block silicone oil and a preparation method thereof. First, a Y-shaped structure intermediate is prepared from glycerol triglycidyl ether and monoethanolamine, and then isopropanol is used as a solvent to react the Y-shaped structure intermediate with a double-terminal epoxy polyether silicone oil to prepare the hydrophilic fluffy dendritic block silicone oil. The prepared hydrophilic fluffy dendritic block silicone oil not only has excellent self-emulsification, but also can give cotton, polyester, and polyester-cotton fabrics excellent fluffy hand feel, antistatic properties, and hydrophilic properties.

Description

Technical Field

[0001] The invention relates to the field of textile auxiliaries, in particular to a hydrophilic fluffy dendritic block silicone oil and a preparation method thereof. Background Art

[0002] With the improvement of living standards, people have an increasing demand for diversified fabrics and higher requirements for comfort. The finished fabrics are often not only required to have excellent hydrophilicity, but also excellent antistatic, fluffy, soft and other properties.

[0003] In recent years, the silicone oil industry has developed rapidly, and various functional silicone oils have sprung up, especially in the field of hydrophilic silicone oil with a good feel. Traditional hydrophilic silicone oils are mainly divided into: (1) Side chain hydrogen silicone oil and allyl alcohol polyether to obtain side chain polyether modified silicone oil (CJF); (2) Epoxy silicone oil and hydrophilic polyether amine are alternately arranged in a straight chain copolymer hydrophilic silicone oil; (3) Epoxy silicone oil and tertiary amine are alternately arranged in a straight chain copolymer, and then an alkylating agent is added for modification to obtain a hydrophilic silicone oil; (4) Hydrophilic silicone oil prepared by polyurethane modified silicone. Patent CN201610632480.2 "A ternary copolymer block hydrophilic amino silicone oil and its preparation method and application" and Patent CN201210134514.7 "A super soft hydrophilic block silicone oil compound and preparation method" are prepared through the above-mentioned synthesis process.

[0004] Although the side chain polyether modified silicone oil (CJF) can give the finished fabric excellent hydrophilicity, there are problems such as poor hand feel of the finished fabric and narrow application of the fabric; although the linear copolymer hydrophilic silicone oil with alternating arrangement of epoxy silicone oil and hydrophilic polyether amine or epoxy silicone oil and tertiary amine can give the finished fabric excellent hydrophilicity and hand feel, its structure is a linear polymer, and its hand feel is mainly reflected in softness and smoothness from the structural analysis; although the polyurethane modified silicone hydrophilic silicone oil can also reflect the excellent hydrophilicity of the finished fabric, due to the presence of soft and hard segments in its structure, its main style is slippery and elastic. Comprehensive analysis shows that the above structural products mainly reflect the properties of hydrophilicity, softness, and smoothness, and the fluffy property is second. Therefore, the present invention prepares a hydrophilic and fluffy dendritic block silicone oil by using a homemade Y-shaped structure intermediate to react with a double-ended epoxy polyether silicone oil. The dendritic structure of the silicone oil contains a large amount of siloxane segments, amino segments, hydrophilic polyether segments and hydroxyl segments, thereby giving the silicone oil excellent self-emulsification and giving the finished fabric excellent fluffy, antistatic and hydrophilic properties. Summary of the invention

[0005] The technical problem to be solved by the present invention is to overcome the defects of the above-mentioned prior art and provide a method for preparing a hydrophilic fluffy dendritic block silicone oil.

[0006] In order to achieve the above object, the present invention adopts the following technical solutions:

[0007] A method for preparing a hydrophilic fluffy dendritic block silicone oil, characterized in that it is carried out according to the following synthesis method, calculated by mass fraction:

[0008] 190-200 parts of monoethanolamine are added to a reaction vessel equipped with a condensing reflux device, stirring is started, the temperature is raised to 60-80°C, and then 260 parts of propylene glycol triglycidyl ether are uniformly added dropwise to the reaction vessel through a constant pressure dropping funnel. After the addition is completed, the temperature is kept for 2-4 hours to obtain a Y-type structure intermediate, and the reaction formula is as follows;

[0009]

[0010] 1000 parts of double-terminal epoxy polyether silicone oil, 70-160 parts of Y-type structure intermediate, and 300-500 parts of solvent are added to a reaction vessel equipped with a condensation reflux device, stirring is started, and the reaction vessel is heated to 80-83° C., and the temperature is kept in this temperature range for 6-9 hours to obtain a hydrophilic fluffy dendritic block silicone oil, and the reaction formula is as follows;

[0011]

[0012] In the formula, m is an integer between 27 and 80, and n is an integer between 20 and 25.

[0013] Preferably, the number average molecular weight of the double-terminal epoxy polyether silicone oil is one of 4000 to 9000, and the polyether segment in its structure is an ethylene oxide (EO) segment.

[0014] Preferably, the solvent is isopropanol.

[0015] Due to the application of the above technical solution, the present invention has the following advantages:

[0016] The invention prepares a hydrophilic and fluffy dendritic block silicone oil by reacting a self-made Y-shaped structure intermediate with a double-ended epoxy polyether silicone oil. The self-made intermediate structure contains three secondary amine groups, which can react with the double-ended epoxy silicone oil to obtain a dendritic structure. The product not only has the characteristics of high branching, low viscosity, high solubility and high reactivity, but also can give the finished fabric excellent fluffy performance. In addition, compared with traditional alkyl tertiary amines and polyether tertiary amines (EA structure series), the Y-shaped structure intermediate contains a large number of hydroxyl groups in the polymer structure after the reaction, which can make the polymer self-emulsified while also giving the fabric excellent hydrophilicity and antistatic properties. Implementation

[0017] The present invention is further described below through specific implementation modes.

[0018] Example 1

[0019] 1. Add 190 parts of monoethanolamine to a reaction vessel equipped with a condensing reflux device, start stirring, raise the temperature to 65°C, and then uniformly add 260 parts of propylene glycol triglycidyl ether to the reaction vessel through a constant pressure dropping funnel. After the addition is completed, keep the temperature for 2 hours to obtain a Y-type structure intermediate.

[0020] 2. Add 1000 parts of double-ended epoxy polyether silicone oil with a number average molecular weight of 5000, 130 parts of Y-type structure intermediate, and 350 parts of isopropanol into a reaction vessel equipped with a condensation reflux device, start stirring, heat the reaction vessel to 80°C, and keep the reaction in this temperature range for 7 hours to obtain a hydrophilic fluffy dendritic block silicone oil.

[0021] Example 2

[0022] 1. Add 195 parts of monoethanolamine to a reaction vessel equipped with a condensing reflux device, start stirring, raise the temperature to 70°C, and then uniformly add 260 parts of propylene glycol triglycidyl ether to the reaction vessel through a constant pressure dropping funnel. After the addition is completed, keep the temperature for 3 hours to obtain a Y-type structure intermediate.

[0023] 2. Add 1000 parts of double-ended epoxy polyether silicone oil with a number average molecular weight of 6000, 110 parts of Y-type structure intermediate, and 400 parts of isopropanol into a reaction vessel equipped with a condensation reflux device, start stirring, heat the reaction vessel to 82°C, and keep the reaction in this temperature range for 8 hours to obtain a hydrophilic fluffy dendritic block silicone oil.

[0024] Example 3

[0025] 1. Add 200 parts of monoethanolamine to a reaction vessel equipped with a condensing reflux device, start stirring, raise the temperature to 75°C, and then uniformly add 260 parts of propylene glycol triglycidyl ether to the reaction vessel through a constant pressure dropping funnel. After the addition is completed, keep the temperature for 4 hours to obtain a Y-type structure intermediate.

[0026] 2. Add 1000 parts of double-ended epoxy polyether silicone oil with a number average molecular weight of 8000, 80 parts of Y-type structure intermediate, and 450 parts of isopropanol into a reaction vessel equipped with a condensation reflux device, start stirring, heat the reaction vessel to 83°C, and keep the reaction in this temperature range for 9 hours to obtain a hydrophilic fluffy dendritic block silicone oil.

[0027] Silicone oil application evaluation process:

[0028] Silicone oil emulsion preparation

[0029] The sample of the embodiment and the comparative sample of the same type and style available on the market were emulsified by the same emulsification process to obtain an emulsion with a solid content of 14% to 15%, and finally the pH was adjusted to 3 to 6 with glacial acetic acid.

[0030] 2. Finishing process

[0031] Fabrics used: white pure cotton knitted fabric, black polyester knitted fabric, black polyester-cotton knitted fabric.

[0032] Finishing process: padding working solution (hydrophilic fluffy dendritic block silicone oil emulsion 40g / L, one dip and one padding, padding rate (white pure cotton knitted fabric 80%~90%, black polyester knitted fabric 60%~80%, black polyester-cotton knitted fabric 70%~80%) → baking (white pure cotton knitted fabric 165 o C×50s, black polyester knitted fabric 190 o C×60s, black polyester-cotton knitted fabric 170 o C×80s) → Cool and rehumidify for 24 hours → Test performance.

[0033] 3. Application performance testing

[0034] 3.1 Fluffiness evaluation

[0035] The compression ratio of fabrics was tested using KES-FB3 style instrument (N﹒cm / cm 2 ), the larger the value, the better the fluffiness.

[0036] 3.2 Hydrophilicity evaluation

[0037] Hydrophilicity evaluation: Use a standard dropper to drop a drop of water from a height of 10 cm from the fabric to the horizontally spread fabric surface, and measure the time it takes for the water drop to completely wet, diffuse and penetrate the fabric surface under static conditions. The shorter the time, the better the hydrophilic effect.

[0038] 3.3 Antistatic evaluation

[0039] The finished fabric was balanced at 25°C and RH 30% for 24 hours, and then the peak voltage and half-life were tested according to the standard using a YG (B) 342D fabric static tester.

[0040] The evaluation results of the fluffy application performance of the hydrophilic fluffy dendritic block silicone oil emulsion of the present invention and the comparative silicone oil emulsion are shown in Table 1:

[0041] Table 1 Comparison of the bulkiness of the example samples and the comparative samples

[0042]

[0043] It can be seen from Table 1 that after the fabric is finished with the emulsion made of the hydrophilic and fluffy dendritic block silicone oil of the present invention, the fluffiness is significantly better than that of the control sample.

[0044] The hydrophilic performance evaluation results of the hydrophilic fluffy dendritic block silicone oil emulsion of the present invention and the comparative silicone oil emulsion are shown in Table 2:

[0045] Table 2 Comparison of hydrophilicity of example samples and comparative samples

[0046]

[0047] It can be seen from Table 2 that after the fabric is finished with the emulsion made of the hydrophilic fluffy dendritic block silicone oil of the present invention, the hydrophilicity is significantly better than that of the control sample.

[0048] The antistatic performance comparison results of the hydrophilic fluffy dendritic block silicone oil emulsion of the present invention and the comparative silicone oil emulsion are shown in Table 3:

[0049] Table 3 Comparison of antistatic properties of example samples and comparative samples

[0050]

[0051] It can be seen from Table 3 that after the fabric is finished with the emulsion made of the hydrophilic fluffy dendritic block silicone oil of the present invention, the peak voltage and half-life are lower than those of the original fabric and the control example.

Claims

1. A method for preparing a hydrophilic fluffy dendritic block silicone oil, characterized in that The steps include: A: According to the mass ratio, 190-200 parts of monoethanolamine are added to a reaction vessel equipped with a condensation reflux device, stirring is started, the temperature is raised to 60-80°C, and then 260 parts of propylene glycol triglycidyl ether are uniformly added to the reaction vessel through a constant pressure dropping funnel. After the addition is completed, the reaction is kept warm for 2-4 hours to obtain a Y-type structure intermediate. B: Add 1000 parts of double-ended epoxy polyether silicone oil, 70-160 parts of Y-type structure intermediate, and 300-500 parts of solvent into a reaction vessel equipped with a condensation reflux device, start stirring, heat the reaction vessel to 80-83°C, and keep the reaction in this temperature range for 6-9 hours to obtain a hydrophilic fluffy dendritic block silicone oil.

2. The method for preparing a hydrophilic fluffy dendritic block silicone oil according to claim 1, characterized in that: The number average molecular weight of the double-terminal epoxy polyether silicone oil is 4000-9000, and the polyether segment in its structure is an ethylene oxide segment.

3. The method for preparing a hydrophilic fluffy dendritic block silicone oil according to claim 1, characterized in that: The solvent is one of isopropanol, ethylene glycol butyl ether and diethylene glycol butyl ether.

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