A thermal insulation composite fabric and its production process

Abstract

The invention relates to a thermal insulation composite fabric and a production process thereof, belonging to the technical field of functional fabrics. The thermal insulation composite fabric is composited with a densely woven base fabric and a thermal insulation adhesive. The thermal insulation adhesive uses aerogel micropowder as thermal insulation particles, is modified by introducing epoxy groups through a silane coupling agent KH560, is ring-opened by 2-(1-methylethyl)-3-oxazoline ethanol and epoxy groups, introduces oxazolidine structures on the surfaces of aerogel microparticles, and synthesizes a polyurethane prepolymer containing a polyether segment from polyether diol and diisocyanate as an adhesive material. During the fumigation curing process, the polyether segment is hydrophilic and preferentially infiltrated and diffused, and the oxazolidine structure on the surface of the modified aerogel powder is promoted to hydrolyze, expose active amine groups and hydroxyl groups, and promote the cross-linking of isocyanate in the prepolymer in the near-surface layer of the modified aerogel powder, so that the aerogel microparticles are uniformly fixed with the polyether segment of the prepolymer as a template, and are segmented in the adhesive layer to form intricate and tortuous heat conduction channels, thereby increasing the thermal resistance of the adhesive layer and having a good thermal insulation effect.

Description

Technical Field

[0001] The present invention belongs to the technical field of functional fabrics, and in particular, relates to a thermal insulation composite fabric and a production process thereof. Background Art

[0002] In the absence of effective protection, the human body's body temperature will drop when exposed to severe cold, causing frostbite or even death. Wearing warm clothing is an important way to overcome severe cold, which can effectively reduce the transfer of human heat to the outside world and maintain a stable body temperature.

[0003] Traditional thermal clothing is mostly filled with cotton, down, etc., forming a fluffy air insulation layer in the fabric, thereby slowing down the loss of heat. However, this thermal clothing is usually bulky, causing inconvenience in movement, and the thermal insulation performance of these thermal clothing is limited, and it is difficult to maintain human body temperature in some extremely cold environments. Aerogel is a porous material with nanopores formed by the mutual aggregation of polymer molecules or colloidal particles, and its nanopores are filled with gaseous dispersion medium, with low density and extremely low thermal conductivity. Aerogel is a hard material and cannot be directly applied to fabrics. In the prior art, aerogel is made into powder and dispersed in adhesive materials, and then coated and compounded in fabrics to give fabrics certain thermal insulation properties; however, the dispersion stability of aerogel in adhesive materials is poor, and it is difficult to form a uniform thermal insulation barrier, resulting in limited effect of aerogel on improving the thermal insulation performance of fabrics. Adding a large amount of aerogel material is conducive to the formation of a continuous thermal insulation layer, but it has a great impact on the softness and comfort of the fabric, which does not meet the comfort design requirements. Summary of the invention

[0004] In order to solve the technical problems mentioned in the background technology, the purpose of the present invention is to provide a thermal insulation composite fabric and a production process thereof.

[0005] The purpose of the present invention can be achieved through the following technical solutions:

[0006] A thermal insulation composite fabric is composited by a densely woven base fabric and a thermal insulation adhesive, wherein the thermal insulation adhesive is prepared by the following method:

[0007] Step A1: Mix silane coupling agent KH560 and deionized water, add formic acid to adjust the pH value to 5, hydrolyze for 20-30 minutes, then add silicon-based aerogel powder and mix, heat to 35-45°C, stir at 180-240 rpm for 1-1.5 hours, then neutralize with ammonia water, filter and vacuum dry to obtain coupling aerogel powder;

[0008] Furthermore, the dosage ratio of silicon-based aerogel micropowder, silane coupling agent KH560 and deionized water is 50g:2.2-3.5g:60-80mL. The silicon-based aerogel micropowder contains a large number of hydroxyl groups on its surface in a water environment. The silane coupling agent KH560 condenses with the hydroxyl groups on its surface after hydrolysis, thereby introducing epoxy group modification into the surface of the silicon-based aerogel micropowder.

[0009] Furthermore, the average particle size of the silicon-based aerogel powder is no more than 50 μm, at which particle size it is easy to disperse evenly to form a thermal insulation barrier.

[0010] Step A2: 2-(1-methylethyl)-3-oxazolineethanol, triethylamine and anhydrous dimethylacetamide were mixed under a dry nitrogen atmosphere, coupled aerogel powder was added and mixed, the temperature was raised to 85-95° C., and stirred at 60-90 rpm for 2.5-3 h. After the reaction was completed, the modified aerogel powder was filtered, washed and vacuum dried to obtain the modified aerogel powder;

[0011] Furthermore, the usage ratio of the coupled aerogel powder, 2-(1-methylethyl)-3-oxazolineethanol, triethylamine and anhydrous dimethylacetamide is 50g:1.5-2.3g:5-7mL:40-50mL. Under the promotion of triethylamine, the primary hydroxyl group of 2-(1-methylethyl)-3-oxazolineethanol and the epoxy group introduced on the surface of the coupled aerogel powder are ring-opened, and the oxazolidine structure of 2-(1-methylethyl)-3-oxazolineethanol is grafted onto the surface of the aerogel micropowder.

[0012] Step A3: premix polyether diol and isophorone diisocyanate as a substrate, introduce dry nitrogen protection, heat to 65-75°C, stir at 40-60 rpm, slowly add dibutyltin dilaurate and react for 1.2-1.6 hours, add ethyl acetate to cool and dilute after the reaction, and obtain a prepolymerized primer;

[0013] Further, the molar ratio of the hydroxyl group to the isocyanate group of the polyether diol and isophorone diisocyanate is 1:1.35-1.5, the amount of dibutyltin dilaurate is 0.06-0.08wt% of the substrate, and the amount of ethyl acetate is 32-40wt% of the substrate;

[0014] Furthermore, the polyether diol is selected from propylene glycol polyether, and the average molecular weight is 800-1500.

[0015] Step A4: the prepolymerized primer, modified aerogel powder, defoamer and leveling agent are mixed evenly, and vacuum degassing is performed to obtain a thermal insulation adhesive.

[0016] Furthermore, the mass ratio of the prepolymerized primer, the modified aerogel powder, the defoamer and the leveling agent is 100:8.5-10:0.12-0.14:0.1-0.12.

[0017] A production process of a thermal insulation composite fabric includes the following steps:

[0018] Step S1: coating a thermal insulation adhesive on one side of a densely woven base fabric, laminating and cold-pressing the fabric to obtain a composite grey fabric;

[0019] Step S2: transferring the composite grey fabric into a steam box, curing it by steam fumigation, and drying it with hot air to obtain a heat-insulating composite fabric.

[0020] Beneficial effects of the present invention:

[0021] The invention discloses a thermal insulation adhesive, which uses aerogel micropowder as thermal insulation particles, introduces epoxy groups into the surface of the aerogel particles by using a silane coupling agent KH560 for modification, and then introduces an oxazolidine structure into the surface of the aerogel particles by opening the ring through the primary hydroxyl group of 2-(1-methylethyl)-3-oxazoline ethanol and the introduced epoxy groups, so as to obtain the modified aerogel micropowder; a polyurethane prepolymer containing a polyether chain segment is synthesized from polyether diol and diisocyanate as an adhesive material, and a fumigation process is performed, and in the curing and compounding process, the hydrophilic polyether segments in the prepolymer chain segments are preferentially infiltrated and diffused, and these impregnated The moist water promotes the hydrolysis of the oxazolidine structure on the surface of the modified aerogel powder, exposing active amine groups and hydroxyl groups, promoting the cross-linking of the isocyanate in the prepolymer near the surface of the modified aerogel powder, and fixing the modified aerogel powder, so that the aerogel particles are evenly fixed with the polyether segment of the prepolymer as a template. The aerogel particles have high thermal insulation properties and are divided in the adhesive layer to form intricate and tortuous heat conduction channels, which increase the thermal resistance of the adhesive layer and have a lower thermal conductivity and thermal insulation effect. At the same time, the evenly dispersed aerogel particles make the mechanical properties of the adhesive layer more uniform, and the fabric is more comfortable to wear. DETAILED DESCRIPTION

[0022] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0023] Example 1: This example prepares a thermal insulation composite fabric. The specific implementation process is as follows:

[0024] (1) Preparation of thermal insulation adhesive

[0025] Step A1: Mix silane coupling agent KH560 and deionized water, add formic acid to adjust the pH value to 5 and hydrolyze for 20 minutes, then add silicon-based aerogel powder and mix, heat to 45°C, stir at 240rpm for 1 hour, then neutralize with ammonia water, filter and vacuum dry to obtain coupled aerogel powder, wherein the silicon-based aerogel powder is TEP-D20 raw material from Suzhou Thermal Image Nanotechnology Co., Ltd., with an average particle size of about 15 μm, and the amount ratio of silicon-based aerogel powder, silane coupling agent KH560 and deionized water is 50g:2.2g:60mL.

[0026] Step A2: Take 2-(1-methylethyl)-3-oxazolineethanol, triethylamine and anhydrous dimethylacetamide, mix them under a dry nitrogen atmosphere, add the coupled aerogel powder and mix, heat to 95°C, apply 90rpm stirring to react for 2.5h, filter after the reaction, wash the filter cake with anhydrous acetone and vacuum dry to obtain modified aerogel powder, wherein the amount ratio of coupled aerogel powder, 2-(1-methylethyl)-3-oxazolineethanol, triethylamine and anhydrous dimethylacetamide is 50g:2.3g:7mL:40mL.

[0027] Step A3: Take a premix of polyether diol and isophorone diisocyanate as a substrate, introduce dry nitrogen protection, heat to 75°C, apply 60rpm stirring, slowly add dibutyltin dilaurate within 30 minutes, continue the constant temperature reaction after complete addition, and control the total reaction time of dibutyltin dilaurate to be 1.2 hours. After the reaction is completed, add ethyl acetate to cool and dilute to obtain a prepolymerized primer, wherein the polyether diol is PPG-1500, the molar ratio of hydroxyl group to isocyanate group of polyether diol and isophorone diisocyanate is 1:1.5, the amount of dibutyltin dilaurate is 0.08wt% of the substrate, and the amount of ethyl acetate is 40wt% of the substrate.

[0028] Step A4: Add the prepolymerized primer, modified aerogel powder, defoamer and leveling agent into a high-speed mixer, mix at 600 rpm for 5 minutes, and vacuum degas for 10 minutes to obtain a thermal insulation adhesive, wherein the defoamer is selected from the DT-650 raw material of Foshan Nanhai Datian Chemical Co., Ltd., and the leveling agent is selected from the RM-2020 raw material of Guangzhou Hengyu Chemical Co., Ltd. The mass ratio of the prepolymerized primer, modified aerogel powder, defoamer and leveling agent is 100:8.5:0.12:0.1.

[0029] (2) Preparation of thermal insulation composite fabrics

[0030] Step S1: Apply thermal insulation adhesive on one side of the densely woven base fabric, and control the amount of adhesive to be 80g / m 2 After lamination, the composite fabric is cold pressed and shaped at 0.5 MPa to obtain a composite fabric.

[0031] Step S2: The composite grey fabric is transferred into a steamer, and is fumigated for 25 minutes under 1.5 bar saturated steam, and the discharged fabric is dried by hot air to obtain a thermal insulation composite fabric.

[0032] Example 2: This example prepares a thermal insulation composite fabric. The specific implementation process is as follows:

[0033] (1) Preparation of thermal insulation adhesive

[0034] Step A1: Mix silane coupling agent KH560 and deionized water, add formic acid to adjust the pH value to 5 and hydrolyze for 30 minutes, then add silicon-based aerogel powder and mix, heat to 35°C, stir at 180rpm for 1.5 hours, then neutralize with ammonia water, filter and vacuum dry to obtain coupled aerogel powder, wherein the silicon-based aerogel powder is TEP-D50 raw material from Suzhou Thermal Image Nanotechnology Co., Ltd., with an average particle size of about 50 μm, and the amount ratio of silicon-based aerogel powder, silane coupling agent KH560 and deionized water is 50g:3.5g:80mL.

[0035] Step A2: Take 2-(1-methylethyl)-3-oxazolineethanol, triethylamine and anhydrous dimethylacetamide, mix them under a dry nitrogen atmosphere, add the coupled aerogel powder and mix, heat to 85°C, apply 60rpm stirring to react for 3h, filter after the reaction, wash the filter cake with anhydrous acetone and vacuum dry to obtain modified aerogel powder, wherein the amount ratio of coupled aerogel powder, 2-(1-methylethyl)-3-oxazolineethanol, triethylamine and anhydrous dimethylacetamide is 50g:1.5g:5mL:50mL.

[0036] Step A3: Take a premix of polyether diol and isophorone diisocyanate as a substrate, introduce dry nitrogen protection, heat to 65°C, apply stirring at 40rpm, slowly add dibutyltin dilaurate within 40min, continue the constant temperature reaction after complete addition, control the total reaction time of dibutyltin dilaurate to be 1.6h, add ethyl acetate to cool and dilute after the reaction is completed, and obtain a prepolymerized primer, wherein the polyether diol is PPG-800, the molar ratio of hydroxyl group to isocyanate group of polyether diol and isophorone diisocyanate is 1:1.35, the amount of dibutyltin dilaurate is 0.06wt% of the substrate, and the amount of ethyl acetate is 32wt% of the substrate.

[0037] Step A4: Add the prepolymerized primer, modified aerogel powder, defoamer and leveling agent into a high-speed mixer, mix at 600 rpm for 5 minutes, and vacuum degas for 10 minutes to obtain a thermal insulation adhesive, wherein the defoamer is selected from the DT-650 raw material of Foshan Nanhai Datian Chemical Co., Ltd., and the leveling agent is selected from the RM-2020 raw material of Guangzhou Hengyu Chemical Co., Ltd. The mass ratio of the prepolymerized primer, modified aerogel powder, defoamer and leveling agent is 100:10:0.14:0.12.

[0038] (2) Preparation of thermal insulation composite fabrics

[0039] Step S1: Apply thermal insulation adhesive on one side of the densely woven base fabric, and control the amount of adhesive to be 90g / m 2 After lamination, the composite fabric is cold pressed and shaped at 0.5 MPa to obtain a composite fabric.

[0040] Step S2: The composite grey fabric is transferred into a steamer, and is fumigated for 20 minutes under 1.5 bar saturated steam, and the discharged fabric is dried by hot air to obtain a thermal insulation composite fabric.

[0041] Example 3: This example prepares a thermal insulation composite fabric. The specific implementation process is as follows:

[0042] (1) Preparation of thermal insulation adhesive

[0043] Step A1: Mix silane coupling agent KH560 and deionized water, add formic acid to adjust the pH value to 5 and hydrolyze for 30 minutes, then add silicon-based aerogel powder and mix, heat to 30°C, stir at 240rpm for 1.3 hours, then neutralize with ammonia water, filter and vacuum dry to obtain coupled aerogel powder, wherein the silicon-based aerogel powder is TEP-D20 raw material from Suzhou Thermal Image Nanotechnology Co., Ltd., with an average particle size of about 15 μm, and the amount ratio of silicon-based aerogel powder, silane coupling agent KH560 and deionized water is 50g:2.8g:70mL.

[0044] Step A2: Take 2-(1-methylethyl)-3-oxazolineethanol, triethylamine and anhydrous dimethylacetamide, mix them under a dry nitrogen atmosphere, add the coupled aerogel powder and mix, heat to 90°C, apply 90rpm stirring to react for 2.8h, filter after the reaction, wash the filter cake with anhydrous acetone and vacuum dry to obtain modified aerogel powder, wherein the amount ratio of coupled aerogel powder, 2-(1-methylethyl)-3-oxazolineethanol, triethylamine and anhydrous dimethylacetamide is 50g:2.1g:6mL:50mL.

[0045] Step A3: Take a premix of polyether diol and isophorone diisocyanate as a substrate, introduce dry nitrogen protection, heat to 70°C, apply 60rpm stirring, slowly add dibutyltin dilaurate within 40 minutes, continue the constant temperature reaction after complete addition, control the total reaction time of dibutyltin dilaurate to be 1.5 hours, add ethyl acetate to cool and dilute after the reaction is completed, and obtain a prepolymerized primer, wherein the polyether diol is PPG-1200, the molar ratio of hydroxyl group to isocyanate group of polyether diol and isophorone diisocyanate is 1:1.42, the amount of dibutyltin dilaurate is 0.07wt% of the substrate, and the amount of ethyl acetate is 35wt% of the substrate.

[0046] Step A4: Add the prepolymerized primer, modified aerogel powder, defoamer and leveling agent into a high-speed mixer, mix at 600 rpm for 5 minutes, and vacuum degas for 10 minutes to obtain a thermal insulation adhesive, wherein the defoamer is selected from the DT-650 raw material of Foshan Nanhai Datian Chemical Co., Ltd., and the leveling agent is selected from the RM-2020 raw material of Guangzhou Hengyu Chemical Co., Ltd. The mass ratio of the prepolymerized primer, modified aerogel powder, defoamer and leveling agent is 100:9.2:0.13:0.11.

[0047] (2) Preparation of thermal insulation composite fabrics

[0048] Step S1: Apply thermal insulation adhesive on one side of the densely woven base fabric, and control the amount of adhesive to be 85g / m 2 After lamination, the composite fabric is cold pressed and shaped at 0.5 MPa to obtain a composite fabric.

[0049] Step S2: The composite grey fabric is transferred into a steamer, and is fumigated for 22 minutes under 1.5 bar saturated steam, and the discharged fabric is dried by hot air to obtain a thermal insulation composite fabric.

[0050] Comparative Example 1

[0051] In this comparative example, polyurethane glue and the coupled aerogel powder in Example 3 are compounded to prepare a thermal insulation adhesive. The specific formula is: 100 parts of polyurethane glue, using APU-9-100C raw material from Taiwan Piu Industrial Co., Ltd.; 10 parts of coupled aerogel powder; 0.14 parts of defoaming agent; 0.12 parts of leveling agent; the specific process for preparing the fabric is the same as Example 3.

[0052] Comparative Example 2

[0053] In the reference example of comparative example 3, the modified aerogel powder was replaced with the coupled aerogel powder of the same weight in this example during the implementation process, and the rest of the implementation process was exactly the same.

[0054] Take the fabric prepared as above, use TPS-2500S thermal constant analyzer to test the thermal conductivity of the fabric; use KES-F fabric style meter to test the wearing performance of the fabric; the specific test results are shown in the following table:

[0055]

[0056] It can be seen from the test results in the above table that the fabric prepared in the embodiment has a lower thermal conductivity, and has a good thermal insulation effect when used in clothing fabrics. The shear stiffness and shear hysteresis as well as the bending stiffness and bending hysteresis are all maintained within a good range, and has good softness and shape retention.

[0057] In the description of the specification, the description with reference to the terms "one embodiment", "example", "specific example", etc. means that the specific features, structures, materials or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic representation of the above terms does not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described can be combined in any one or more embodiments or examples in a suitable manner.

[0058] The above contents are merely examples and explanations of the present invention. Those skilled in the art may make various modifications or additions to the specific embodiments described or replace them in a similar manner. As long as they do not deviate from the invention or exceed the scope defined by the claims, they shall all fall within the protection scope of the present invention.

Claims

1. A thermal insulation composite fabric, which is composed of a densely woven base fabric and a thermal insulation adhesive, characterized in that: The thermal insulation adhesive is prepared by the following method: Step A1: Mix silane coupling agent KH560 and deionized water, add formic acid to adjust the pH value to 5, and hydrolyze for 20-30 minutes, then add silicon-based aerogel powder and mix, heat to 35-45°C, stir and react for 1-1.5 hours, then neutralize with ammonia water, filter and vacuum dry to obtain coupling aerogel powder; Step A2: Mix 2-(1-methylethyl)-3-oxazolineethanol, triethylamine and anhydrous dimethylacetamide under a dry nitrogen atmosphere, add the coupled aerogel powder and mix, heat to 85-95° C. and stir to react for 2.5-3 h. After the reaction is completed, filter, wash and vacuum dry to obtain modified aerogel powder; Step A3: premix polyether diol and isophorone diisocyanate as a substrate, introduce dry nitrogen protection, heat to 65-75°C, stir and slowly add dibutyltin dilaurate to react for 1.2-1.6h, add ethyl acetate to cool and dilute after the reaction to obtain a prepolymerized primer; Step A4: the prepolymerized primer, modified aerogel powder, defoamer and leveling agent are mixed evenly, and vacuum degassing is performed to obtain a thermal insulation adhesive.

2. The thermal insulation composite fabric according to claim 1, characterized in that: The dosage ratio of silicon-based aerogel powder, silane coupling agent KH560 and deionized water is 50g:2.2-3.5g:60-80mL.

3. The thermal insulation composite fabric according to claim 2, characterized in that: The average particle size of the silicon-based aerogel powder is not higher than 50 μm.

4. The thermal insulation composite fabric according to claim 3, characterized in that: The usage ratio of the coupling aerogel powder, 2-(1-methylethyl)-3-oxazolineethanol, triethylamine and anhydrous dimethylacetamide is 50g:1.5-2.3g:5-7mL:40-50mL.

5. The thermal insulation composite fabric according to claim 1, characterized in that: The molar ratio of the hydroxyl group to the isocyanate group of the polyether diol and isophorone diisocyanate is 1:1.35-1.5, the amount of dibutyltin dilaurate is 0.06-0.08wt% of the substrate, and the amount of ethyl acetate is 32-40wt% of the substrate.

6. The thermal insulation composite fabric according to claim 5, characterized in that: The polyether diol is selected from propylene glycol polyether and has an average molecular weight of 800-1500.

7. The thermal insulation composite fabric according to claim 1, characterized in that: The mass ratio of the prepolymerized primer, the modified aerogel powder, the defoamer and the leveling agent is 100:8.5-10:0.12-0.14:0.1-0.

12.

8. A production process for a thermal insulation composite fabric according to any one of claims 1 to 7, characterized in that: Including the following processes: Step S1: coating a thermal insulation adhesive on one side of a densely woven base fabric, laminating and cold-pressing the fabric to obtain a composite grey fabric; Step S2: transferring the composite grey fabric into a steam box, curing it by steam fumigation, and drying it with hot air to obtain a heat-insulating composite fabric.

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