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CN114318860B - Warm-keeping polyester fabric based on tourmaline powder and preparation method thereof - Google Patents

Warm-keeping polyester fabric based on tourmaline powder and preparation method thereof Download PDF

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CN114318860B
CN114318860B CN202111360362.8A CN202111360362A CN114318860B CN 114318860 B CN114318860 B CN 114318860B CN 202111360362 A CN202111360362 A CN 202111360362A CN 114318860 B CN114318860 B CN 114318860B
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tourmaline powder
polyester fabric
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preparation
silane coupling
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CN114318860A (en
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詹志兰
鲁婷婷
周凡雨
李强
蔡亚君
张圣祖
董会杰
蔡映杰
王强
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Yiwu Runting Knitting Co.,Ltd.
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Wuhan Textile University
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Abstract

The invention relates to a thermal polyester fabric based on tourmaline powder and a preparation method thereof. The thermal polyester fabric can be prepared by the following method: firstly, preparing nano tourmaline powder; secondly, preparing a silane coupling agent KH-570 hydrolysate; thirdly, reacting the silane coupling agent KH-570 hydrolysate with the nano-grade tourmaline powder to prepare a cross-linked modified nano-grade tourmaline powder solution; and finally, putting the polyester fabric into finishing liquid for finishing and drying to obtain the thermal polyester fabric. The air permeability range of the terylene fabric prepared by the invention is 876.1-892.5 mm/s, the Crohn value range is 1.08-1.18, and the terylene fabric prepared by the invention has better heat preservation performance on the premise of not influencing air permeability.

Description

一种基于电气石粉的保暖涤纶面料及其制备方法A kind of warm polyester fabric based on tourmaline powder and preparation method thereof

技术领域Technical Field

本发明属于涤纶面料的制备技术领域,具体涉及一种基于电气石粉的保暖涤纶面料及其制备方法。The invention belongs to the technical field of preparation of polyester fabrics, and in particular relates to a tourmaline powder-based thermal insulation polyester fabric and a preparation method thereof.

背景技术Background Art

随着时代快速发展与人口巨大增幅,纺织品更新换代的速度不断加快,对纺织品多功能化整理以增加其附加值成为当下不可避免的趋势。近年来,开发保暖性能优越的纺织衣物受到了极大的关注。With the rapid development of the times and the huge increase in population, the speed of textile renewal is accelerating, and the multifunctional finishing of textiles to increase their added value has become an inevitable trend. In recent years, the development of textile clothing with excellent thermal insulation performance has received great attention.

织物的保暖机制是指服装面料、纺织品等保持被包覆者体温度的性能。当人体处于热平衡时,感觉舒适的温度是33.4℃左右,超过37.9℃,人体将有冷暖感。按照纤维的结构形态,保温面料可分为中空纤维、超细纤维和太空织物纤维。中空纤维中中空涤纶占比最大,在保暖服装行业的应用也最为广泛。从填充材料、保暖衣、保暖裤到特殊防护服以及航空航天服,中空涤纶在未来与其他学科的交叉发展前景值得期待。The warmth-keeping mechanism of fabrics refers to the performance of clothing fabrics, textiles, etc. in maintaining the body temperature of the person being covered. When the human body is in thermal equilibrium, the comfortable temperature is around 33.4°C. If it exceeds 37.9°C, the human body will feel cold or warm. According to the structural morphology of the fiber, thermal insulation fabrics can be divided into hollow fibers, microfibers, and space fabric fibers. Hollow polyester accounts for the largest proportion of hollow fibers and is also the most widely used in the thermal clothing industry. From filling materials, thermal clothing, thermal pants to special protective clothing and aerospace clothing, the cross-development prospects of hollow polyester with other disciplines in the future are worth looking forward to.

经文献调查研究表明,关于涤纶面料的保暖性能受到了广泛的关注,如:中国发明专利申请号201820520803.3公布了一种疏水双中空保暖涤纶长丝:本发明的截面外轮廓采用具有夹角的仿“T”字形结构,使横边具有倾斜面,因而水珠难以在表面吸附,从而更好地利于水珠等的滚动移走,达到表面疏水的效果,仿“T”字形的结构通过喷丝板挤出膨化,叶子相互连接到一块,与内层中空形成三个中空室,保暖效果更好,同时截面外轮廓为类六边形,使纤维蓬松度更好。但是该制备工艺的中空度较难把握,可能会影响整体纤维的服用性能。Literature research shows that the thermal insulation performance of polyester fabrics has received widespread attention, such as: China Invention Patent Application No. 201820520803.3 discloses a hydrophobic double hollow thermal insulation polyester filament: The cross-sectional outer contour of the present invention adopts an angled "T"-shaped structure, so that the horizontal edge has an inclined surface, so that water droplets are difficult to adsorb on the surface, thereby better facilitating the rolling and removal of water droplets, etc., to achieve the effect of surface hydrophobicity, and the "T"-shaped structure is extruded and expanded through a spinneret, and the leaves are connected to each other to form three hollow chambers with the inner hollow layer, which has a better thermal insulation effect. At the same time, the cross-sectional outer contour is a hexagonal shape, which makes the fiber fluffiness better. However, the hollowness of this preparation process is difficult to grasp, which may affect the overall fiber wearability.

电气石粉是把电气石原矿经过去除杂质后,经过机械粉碎得到的粉体。电气石粉用于纺织行业,可做环保炭布,超细电气石粉制成超细纤维,可制成防磁、防潮、保暖棉被、棉垫、防电磁辐射衬衫、背心、鞋垫等,还可用于岩盘浴、汗蒸房、光波房、桑拿浴设施以及环保家居装修。当前,将电气石粉应用于保暖涤纶面料的研制开发,是一个具有发展和应用前景的方向。Tourmaline powder is a powder obtained by mechanically crushing tourmaline ore after removing impurities. Tourmaline powder is used in the textile industry to make environmentally friendly carbon cloth. Ultrafine tourmaline powder is made into ultrafine fibers, which can be made into anti-magnetic, moisture-proof, warm quilts, cotton pads, anti-electromagnetic radiation shirts, vests, insoles, etc. It can also be used in bedrock baths, steam rooms, light wave rooms, sauna facilities and environmentally friendly home decoration. At present, the application of tourmaline powder in the research and development of warm polyester fabrics is a direction with development and application prospects.

发明内容Summary of the invention

本发明的目的在于提供一种基于电气石粉的保暖涤纶面料及其制备方法,以解决现有技术中存在的不足,该涤纶面料含有电气石粉,电气石粉在人体温度的影响下,其可以有效的发热,从而,实现涤纶面料的保暖功能。The purpose of the present invention is to provide a warm-keeping polyester fabric based on tourmaline powder and a preparation method thereof, so as to solve the deficiencies in the prior art. The polyester fabric contains tourmaline powder, which can effectively generate heat under the influence of human body temperature, thereby realizing the warm-keeping function of the polyester fabric.

本发明的目的在于提供一种基于电气石粉的保暖涤纶面料,该保暖棉质面料可由下述制备方法制得:首先,纳米电气石粉的制备;其次,制备制得硅烷偶联剂KH-570水解液;再次,将硅烷偶联剂KH-570水解液与纳米级电气石粉反应,制得交联改性的纳米级电气石粉溶液;最后,将涤纶面料放入整理液整理,烘干,制得保暖涤纶面料。The purpose of the present invention is to provide a thermal insulation polyester fabric based on tourmaline powder. The thermal insulation cotton fabric can be prepared by the following preparation method: first, preparing nano tourmaline powder; second, preparing a silane coupling agent KH-570 hydrolyzate; third, reacting the silane coupling agent KH-570 hydrolyzate with nano-level tourmaline powder to obtain a cross-linked modified nano-level tourmaline powder solution; finally, putting the polyester fabric into a finishing liquid for finishing, drying, and preparing the thermal insulation polyester fabric.

本发明的另一目的在于提供上述所述一种基于电气石粉的保暖涤纶面料的制备方法,所述制备方法包括如下步骤:Another object of the present invention is to provide a method for preparing the above-mentioned tourmaline powder-based thermal insulation polyester fabric, the preparation method comprising the following steps:

(1)纳米电气石粉的制备:将电气石粉进行研磨,制得粒径为纳米级的电气石粉粒子。(1) Preparation of nano-tourmaline powder: Grind the tourmaline powder to obtain tourmaline powder particles with a particle size of nanometers.

作为优选地,所述粒径范围为500~2000纳米。Preferably, the particle size ranges from 500 to 2000 nanometers.

(2)水解:在室温下,将乳化剂司班80溶于去离子水,搅拌均匀,加入硅烷偶联剂KH-570,进行乳化,制得硅烷偶联剂KH-570水解液。(2) Hydrolysis: At room temperature, dissolve the emulsifier Span 80 in deionized water, stir evenly, add the silane coupling agent KH-570, emulsify, and prepare the silane coupling agent KH-570 hydrolyzate.

作为优选地,所述乳化剂司班80、硅烷偶联剂KH-570和去离子水的的用量比为1g∶(1~2)g∶(200~400)mL;所述搅拌时间为10~20min;所述乳化时间为10~20min。Preferably, the usage ratio of the emulsifier Siban 80, the silane coupling agent KH-570 and the deionized water is 1g: (1-2)g: (200-400)mL; the stirring time is 10-20min; and the emulsification time is 10-20min.

(3)交联反应:将步骤(2)制得的硅烷偶联剂KH-570水解液溶于二甲基甲酰胺,制得稀释液;将步骤(1)制得的纳米级电气石粉加入稀释液,搅拌反应,制得交联改性的纳米级电气石粉溶液。(3) Cross-linking reaction: dissolving the hydrolyzate of silane coupling agent KH-570 obtained in step (2) in dimethylformamide to obtain a diluent; adding the nano-scale tourmaline powder obtained in step (1) to the diluent, stirring and reacting, to obtain a cross-linked modified nano-scale tourmaline powder solution.

作为优选地,所述KH-570交联剂水解液(mL)与二甲基甲酰胺(mL)的用量比为:1∶10~20;所述纳米级电气石粉(g)与稀释液(mL)的用量比为:1∶100~200。Preferably, the usage ratio of the KH-570 crosslinking agent hydrolyzate (mL) to dimethylformamide (mL) is 1:10-20; the usage ratio of the nano-level tourmaline powder (g) to the diluent (mL) is 1:100-200.

作为优选地,所述反应温度为:60~80℃,反应时间为:3~5h。Preferably, the reaction temperature is 60-80° C., and the reaction time is 3-5 h.

本步骤涉及的作用机理分析:硅烷偶联剂KH-570改性电气石粉颗粒表面的反应模型包括以下几步:1.Si-X在水分子的作用下生成Si-OH。2.经水解后的硅烷偶联剂分子之间发生脱水缩合反应,生成了具有一定聚合度的低聚硅氧烷;3.将低聚硅氧烷末端的Si-OH与电气石粉颗粒表面的Si-OH之间形成氢键;4.当达到反应所需的温度时,脱水缩合反应,低聚硅氧烷接枝到电气石粉颗粒表层。Analysis of the mechanism of action involved in this step: The reaction model of the surface of tourmaline powder particles modified by silane coupling agent KH-570 includes the following steps: 1. Si-X generates Si-OH under the action of water molecules. 2. Dehydration condensation reaction occurs between the hydrolyzed silane coupling agent molecules to generate oligosiloxane with a certain degree of polymerization; 3. Hydrogen bonds are formed between the Si-OH at the end of the oligosiloxane and the Si-OH on the surface of the tourmaline powder particles; 4. When the temperature required for the reaction is reached, dehydration condensation reaction occurs, and the oligosiloxane is grafted to the surface of the tourmaline powder particles.

(4)整理液的配制:将偶氮二异丁腈溶解于步骤(3)制得的交联改性的纳米级电气石粉溶液,搅拌配制整理液。(4) Preparation of finishing liquid: Dissolve azobisisobutyronitrile in the cross-linked modified nano-scale tourmaline powder solution prepared in step (3), and stir to prepare a finishing liquid.

作为优选地,所述偶氮二异丁腈与步骤(3)制得的交联改性的纳米级电气石粉溶液用量比为:1g∶(100~200)mL。Preferably, the dosage ratio of the azobisisobutyronitrile to the cross-linked modified nano-scale tourmaline powder solution prepared in step (3) is: 1 g: (100-200) mL.

(5)整理:将步骤(4)制得的整理液加热到90~100℃,将涤纶面料放入整理液浸渍1~2小时;取出浸渍后的涤纶面料用大量自来水清洗,烘干,制得保暖涤纶面料。(5) Finishing: heating the finishing liquid obtained in step (4) to 90-100° C., and immersing the polyester fabric in the finishing liquid for 1-2 hours; taking out the immersed polyester fabric, washing it with a large amount of tap water, and drying it to obtain a warm polyester fabric.

作为优选地,所述涤纶面料(g)与整理液(mL)的用量比为:1∶20~40。Preferably, the usage ratio of the polyester fabric (g) to the finishing liquid (mL) is 1:20-40.

本发明的相关作用机理:硅烷偶联剂KH-570中的一部分官能团可与涤纶面料反应,另一部分官能团可与电气石粉反应,形成牢固的粘合。The relevant mechanism of action of the present invention is that a part of the functional groups in the silane coupling agent KH-570 can react with the polyester fabric, and another part of the functional groups can react with the tourmaline powder to form a strong bond.

本发明具有如下显著特点:The present invention has the following notable features:

(1)电气石粉具有发热功能,但是其用于织物面料存在难题。本申请的发明人意外地发现,本发明实现了电气石粉附着于涤纶面料,从而达到涤纶面料发热保暖功能的目的;该发现可以在不破坏涤纶织物的基础上,实现将电气石粉附着于织物表面。(1) Tourmaline powder has a heating function, but there are difficulties in using it on fabrics. The inventor of the present application unexpectedly discovered that the present invention achieves the purpose of attaching tourmaline powder to polyester fabrics, thereby achieving the purpose of the heating and warmth-keeping function of polyester fabrics; this discovery can achieve the attachment of tourmaline powder to the surface of fabrics without damaging polyester fabrics.

(2)本发明制备的含电气石粉涤纶面料具有制备方法简单,原料来源广泛等特点,具有很好的应用前景。(2) The tourmaline powder-containing polyester fabric prepared by the present invention has the characteristics of simple preparation method and wide source of raw materials, and has good application prospects.

(3)本发明制备的涤纶面料的透气率范围分别在876.1~892.5mm/s之间,略低于整理前涤纶面料的透气率,该透气率在正常范围内。本发明制备的涤纶面料的克罗值范围分别在1.08~1.18之间,明显高于整理前涤纶面料的克罗值;经过10次水洗后,面料的克罗值仍没有明显减小,这表明:本发明制备的涤纶面料在不影响透气性的前提下具有较好的保暖性能。(3) The air permeability of the polyester fabric prepared by the present invention ranges from 876.1 to 892.5 mm/s, which is slightly lower than the air permeability of the polyester fabric before finishing and is within the normal range. The Krog value of the polyester fabric prepared by the present invention ranges from 1.08 to 1.18, which is significantly higher than the Krog value of the polyester fabric before finishing; after 10 times of washing, the Krog value of the fabric still does not decrease significantly, which shows that the polyester fabric prepared by the present invention has good thermal insulation performance without affecting the air permeability.

具体实施方式DETAILED DESCRIPTION

主要原料来源:KH-570交联剂(化学名称:γ-甲基丙烯酰氧基丙基三甲氧基硅烷)购于武汉市华伦有机硅有限公司;未整理的涤纶面料购于泰州市三泰织造厂。Sources of main raw materials: KH-570 crosslinking agent (chemical name: γ-methacryloxypropyltrimethoxysilane) was purchased from Wuhan Hualun Silicone Co., Ltd.; unfinished polyester fabric was purchased from Taizhou Santai Weaving Factory.

以下所述实施例和对比例详细说明了本发明。The following examples and comparative examples illustrate the present invention in detail.

实施例1Example 1

在本实施例中,一种基于电气石粉的保暖涤纶面料采用如下方法制备而成,包括如下步骤:In this embodiment, a warm polyester fabric based on tourmaline powder is prepared by the following method, comprising the following steps:

(1)纳米电气石粉的制备:将电气石粉进行研磨,制得粒径为1000~2000纳米级的电气石粉粒子。(1) Preparation of nano-tourmaline powder: Grind the tourmaline powder to obtain tourmaline powder particles with a particle size of 1000 to 2000 nanometers.

(2)水解:在室温下,将1g乳化剂司班80溶于300mL去离子水,搅拌均匀,搅拌时间为15min,加入1.5g硅烷偶联剂KH-570,进行乳化,乳化时间为15min,制得硅烷偶联剂KH-570水解液。(2) Hydrolysis: At room temperature, dissolve 1 g of emulsifier Span 80 in 300 mL of deionized water and stir evenly for 15 min. Add 1.5 g of silane coupling agent KH-570 and emulsify for 15 min to obtain a hydrolyzate of silane coupling agent KH-570.

(3)交联反应:将10mL硅烷偶联剂KH-570水解液溶于150mL二甲基甲酰胺,制得稀释液;将1g步骤(1)制得的纳米级电气石粉加入150mL稀释液,搅拌反应,反应温度为70℃,反应时间为4h,制得交联改性的纳米级电气石粉溶液。(3) Cross-linking reaction: Dissolve 10 mL of silane coupling agent KH-570 hydrolyzate in 150 mL of dimethylformamide to prepare a diluent; add 1 g of the nano-scale tourmaline powder prepared in step (1) to 150 mL of the diluent, and stir to react at a reaction temperature of 70° C. for 4 h to obtain a cross-linked modified nano-scale tourmaline powder solution.

(4)整理液的配制:将1g偶氮二异丁腈溶解于150mL步骤(3)制得的交联改性的纳米级电气石粉溶液,搅拌配制整理液。(4) Preparation of finishing liquid: Dissolve 1 g of azobisisobutyronitrile in 150 mL of the cross-linked modified nano-scale tourmaline powder solution prepared in step (3), and stir to prepare a finishing liquid.

(5)整理:将步骤(4)制得的整理液加热到95℃,将10g涤纶面料放入300mL整理液浸渍1.5小时;取出浸渍后的涤纶面料用大量自来水清洗,烘干,制得保暖涤纶面料。(5) Finishing: The finishing liquid obtained in step (4) is heated to 95° C., and 10 g of polyester fabric is placed in 300 mL of the finishing liquid and immersed for 1.5 hours; the immersed polyester fabric is taken out and washed with a large amount of tap water, and dried to obtain a warm polyester fabric.

实施例2Example 2

在本实施例中,一种基于电气石粉的保暖涤纶面料采用如下方法制备而成,包括如下步骤:In this embodiment, a warm polyester fabric based on tourmaline powder is prepared by the following method, comprising the following steps:

(1)纳米电气石粉的制备:将电气石粉进行研磨,制得粒径为500~1500纳米级的电气石粉粒子。(1) Preparation of nano-tourmaline powder: Grind the tourmaline powder to obtain tourmaline powder particles with a particle size of 500 to 1500 nanometers.

(2)水解:在室温下,将1g乳化剂司班80溶于200mL去离子水,搅拌均匀,搅拌时间为10min,加入1.0g硅烷偶联剂KH-570,进行乳化,乳化时间为10min,制得硅烷偶联剂KH-570水解液。(2) Hydrolysis: At room temperature, dissolve 1 g of emulsifier Span 80 in 200 mL of deionized water and stir evenly for 10 min. Add 1.0 g of silane coupling agent KH-570 and emulsify for 10 min to obtain a hydrolyzate of silane coupling agent KH-570.

(3)交联反应:将10mL硅烷偶联剂KH-570水解液溶于100mL二甲基甲酰胺,制得稀释液;将1g步骤(1)制得的纳米级电气石粉加入100mL稀释液,搅拌反应,反应温度为60℃,反应时间为3h,制得交联改性的纳米级电气石粉溶液。(3) Cross-linking reaction: dissolve 10 mL of silane coupling agent KH-570 hydrolyzate in 100 mL of dimethylformamide to prepare a diluent; add 1 g of the nano-scale tourmaline powder prepared in step (1) to 100 mL of the diluent, stir and react at a reaction temperature of 60° C. for 3 h to obtain a cross-linked modified nano-scale tourmaline powder solution.

(4)整理液的配制:将1g偶氮二异丁腈溶解于100mL步骤(3)制得的交联改性的纳米级电气石粉溶液,搅拌配制整理液。(4) Preparation of finishing liquid: Dissolve 1 g of azobisisobutyronitrile in 100 mL of the cross-linked modified nano-scale tourmaline powder solution prepared in step (3), and stir to prepare a finishing liquid.

(5)整理:将步骤(4)制得的整理液加热到90℃,将10g涤纶面料放入200mL整理液浸渍1.0小时;取出浸渍后的涤纶面料用大量自来水清洗,烘干,制得保暖涤纶面料。(5) Finishing: The finishing liquid obtained in step (4) is heated to 90° C., and 10 g of polyester fabric is placed in 200 mL of the finishing liquid and immersed for 1.0 hour; the immersed polyester fabric is taken out and washed with a large amount of tap water, and dried to obtain a warm polyester fabric.

实施例3Example 3

在本实施例中,一种基于电气石粉的保暖涤纶面料采用如下方法制备而成,包括如下步骤:In this embodiment, a warm polyester fabric based on tourmaline powder is prepared by the following method, comprising the following steps:

(1)纳米电气石粉的制备:将电气石粉进行研磨,制得粒径为800~2000纳米级的电气石粉粒子。(1) Preparation of nano-tourmaline powder: Grind the tourmaline powder to obtain tourmaline powder particles with a particle size of 800 to 2000 nanometers.

(2)水解:在室温下,将1g乳化剂司班80溶于400mL去离子水,搅拌均匀,搅拌时间为20min,加入2g硅烷偶联剂KH-570,进行乳化,乳化时间为20min,制得硅烷偶联剂KH-570水解液。(2) Hydrolysis: At room temperature, dissolve 1 g of emulsifier Span 80 in 400 mL of deionized water and stir evenly for 20 min. Add 2 g of silane coupling agent KH-570 and emulsify for 20 min to obtain a hydrolyzate of silane coupling agent KH-570.

(3)交联反应:将10mL硅烷偶联剂KH-570水解液溶于200mL二甲基甲酰胺,制得稀释液;将1g步骤(1)制得的纳米级电气石粉加入200mL稀释液,搅拌反应,反应温度为80℃,反应时间为5h,制得交联改性的纳米级电气石粉溶液。(3) Cross-linking reaction: Dissolve 10 mL of silane coupling agent KH-570 hydrolyzate in 200 mL of dimethylformamide to obtain a diluent; add 1 g of the nano-scale tourmaline powder obtained in step (1) to 200 mL of the diluent and stir to react at a reaction temperature of 80° C. for 5 h to obtain a cross-linked modified nano-scale tourmaline powder solution.

(4)整理液的配制:将1g偶氮二异丁腈溶解于200mL步骤(3)制得的交联改性的纳米级电气石粉溶液,搅拌配制整理液。(4) Preparation of finishing liquid: Dissolve 1 g of azobisisobutyronitrile in 200 mL of the cross-linked modified nano-scale tourmaline powder solution prepared in step (3), and stir to prepare a finishing liquid.

(5)整理:将步骤(4)制得的整理液加热到100℃,将10g涤纶面料放入400mL整理液浸渍2小时;取出浸渍后的涤纶面料用大量自来水清洗,烘干,制得保暖涤纶面料。(5) Finishing: The finishing liquid obtained in step (4) is heated to 100° C., and 10 g of polyester fabric is placed in 400 mL of the finishing liquid and immersed for 2 hours; the immersed polyester fabric is taken out and washed with a large amount of tap water, and dried to obtain a warm polyester fabric.

对比例AComparative Example A

以实施例1为对比,在本对比例中,减少乳化剂司班80的用量,即将步骤(2)中将“1g乳化剂司班80”改为“0.1g乳化剂司班80”,其它制备方法按实施例1的制备方法实施。In contrast to Example 1, in this comparative example, the amount of the emulsifier Span 80 was reduced, that is, in step (2), "1 g of emulsifier Span 80" was changed to "0.1 g of emulsifier Span 80", and the other preparation methods were carried out according to the preparation method of Example 1.

对比例BComparative Example B

以实施例1为对比,在本对比例中,降低交联反应的温度和时间,即将步骤(3)中“反应温度为70℃,反应时间为4h,”改为“反应温度为30℃,反应时间为1h,”,其它制备方法按实施例1的制备方法实施。In contrast to Example 1, in this comparative example, the temperature and time of the cross-linking reaction were reduced, that is, the reaction temperature of step (3) was changed from "70°C and the reaction time of 4 h" to "30°C and the reaction time of 1 h", and the other preparation methods were carried out according to the preparation method of Example 1.

对比例CComparative Example C

以实施例1为对比,在本对比例中,减少偶氮二异丁腈的用量,即将步骤(4)中的“1g偶氮二异丁腈”改为“0.1g偶氮二异丁腈”,其它制备方法按实施例1的制备方法实施。In this comparative example, the amount of azobisisobutyronitrile was reduced, that is, "1 g azobisisobutyronitrile" in step (4) was changed to "0.1 g azobisisobutyronitrile", and the other preparation methods were carried out according to the preparation method of Example 1.

透气性的测试:Air permeability test:

为了更好地检测本发明中制备的涤纶面料的透气性,选取本发明中上述具体实施例1~3和对比例A~C制备得到的涤纶面料a、b、c、d、e、f和未整理的涤纶面料(购于泰州市三泰织造厂);选取面料的用量为300g/m2。依据GB/T5453-1997测试透气率,试样尺寸20mm×22mm,加压压力100 Pa。测试温度(20±2)℃,湿度(65±2)%,其测试原理为在规定的压差条件下,测定一定时间内垂直通过试样给定面积的气流流量,按下式计算出透气率R。In order to better detect the air permeability of the polyester fabric prepared in the present invention, the polyester fabrics a, b, c, d, e, f and unfinished polyester fabrics (purchased from Taizhou Santai Weaving Factory) prepared in the above specific examples 1 to 3 and comparative examples A to C of the present invention were selected; the amount of the fabric selected was 300g/ m2 . The air permeability was tested according to GB/T5453-1997, the sample size was 20mm×22mm, and the pressure was 100 Pa. The test temperature was (20±2)℃, and the humidity was (65±2)%. The test principle is to measure the air flow rate vertically passing through a given area of the sample within a certain period of time under the specified pressure difference conditions, and calculate the air permeability R according to the following formula.

Figure DEST_PATH_IMAGE001
Figure DEST_PATH_IMAGE001

式中:qv 为平均气流量,A为试验面积,167为换算系数。参照 GB/T 20944.1-2007耐洗色牢度试验机洗涤方法对待测面料进行标准洗涤,测试初始样品和洗涤10次后样品的透气性能,测试结果如表1所示。Where: qv is the average air flow, A is the test area, and 167 is the conversion factor. The fabric to be tested was washed in a standard manner according to the washing method of GB/T 20944.1-2007, and the air permeability of the initial sample and the sample after washing 10 times was tested. The test results are shown in Table 1.

表1 涤纶面料a、b、c、d、e、f和未整理涤纶面料的透气性能Table 1 Air permeability of polyester fabrics a, b, c, d, e, f and unfinished polyester fabrics

Figure DEST_PATH_IMAGE003
Figure DEST_PATH_IMAGE003

从表1可见,涤纶面料a、b、c的透气率范围分别在876.1~892.5mm/s之间,略低于未整理涤纶面料的透气率,该透气率在正常范围内;经过10次水洗后,面料a、b、c的透气率没有明显增加。由此可以认为,本发明制备的涤纶面料具有较好的透气性能。对比例A-C制备的涤纶面料d、e、f的透气性能也表现良好,这表明:乳化剂司班80的用量、交联反应的温度和时间、偶氮二异丁腈的用量均对涤纶面料的透气性能影响不大。As can be seen from Table 1, the air permeability range of polyester fabrics a, b, and c is between 876.1 and 892.5 mm/s, which is slightly lower than the air permeability of unfinished polyester fabrics. The air permeability is within the normal range; after 10 times of washing, the air permeability of fabrics a, b, and c did not increase significantly. It can be considered that the polyester fabric prepared by the present invention has good air permeability. The air permeability of polyester fabrics d, e, and f prepared by comparative examples A-C also shows good performance, which shows that the amount of emulsifier Span 80, the temperature and time of the cross-linking reaction, and the amount of azobisisobutyronitrile have little effect on the air permeability of the polyester fabric.

保暖性的测试:Warmth test:

为了更好地检测本发明中制备的涤纶面料的保暖性,选取本发明中上述具体实施例1~3和对比例A~C制备得到的涤纶面料a、b、c、d、e、f和未整理的涤纶面料(购于泰州市三泰织造厂);选取面料的用量为300g/m2。依据GB/T11048-2008-T《纺织品 生理舒适性 稳态条件下热阻和湿阻的测定》测试材料的保暖性。测试前先根据GB6529-86《恒温恒湿室大气环境标准》对试样进行预调湿和调湿处理。试样在恒温恒湿箱内调湿24 h,温度为(20 ±2) ℃,湿度为(65±2)%;试样尺寸为300mm×300mm,预热时间15分钟。参照 GB/T20944.1-2007耐洗色牢度试验机洗涤方法对待测面料进行标准洗涤,测试初始样品和洗涤10次后样品的保暖性能,测试结果如表2所示。In order to better test the warmth retention of the polyester fabric prepared in the present invention, the polyester fabrics a, b, c, d, e, f and unfinished polyester fabrics (purchased from Taizhou Santai Weaving Factory) prepared in the above-mentioned specific examples 1 to 3 and comparative examples A to C of the present invention were selected; the amount of the fabric selected was 300g/ m2 . The warmth retention of the material was tested according to GB/T11048-2008-T "Determination of thermal resistance and moisture resistance under steady-state conditions for physiological comfort of textiles". Before the test, the sample was pre-humidified and humidified according to GB6529-86 "Standard for atmospheric environment of constant temperature and humidity chamber". The sample was humidified in a constant temperature and humidity chamber for 24 hours, with a temperature of (20 ± 2) ℃ and a humidity of (65 ± 2)%; the sample size was 300mm×300mm, and the preheating time was 15 minutes. The fabrics to be tested were subjected to standard washing according to the washing method of the washing color fastness test machine of GB/T20944.1-2007, and the thermal insulation performance of the initial samples and the samples after washing 10 times was tested. The test results are shown in Table 2.

表2 涤纶面料a、b、c、d、e、f和未整理的涤纶面料的保暖性能Table 2 Thermal insulation properties of polyester fabrics a, b, c, d, e, f and unfinished polyester fabrics

Figure DEST_PATH_IMAGE005
Figure DEST_PATH_IMAGE005

从表2可见,涤纶面料a、b、c的克罗值范围分别在1.08~1.18之间,高于未整理涤纶面料的克罗值;经过10次水洗后,面料a、b、c的克罗值仍没有明显减小。克罗值越高,面料的保暖性越好。由此可以认为,本发明制备的涤纶面料具有较好的保暖性能。对比例A-C制备的涤纶面料d、e、f的保暖性能相对于面料a、b、c略差,这表明:乳化剂司班80的用量、交联反应的温度和时间、偶氮二异丁腈的用量均对涤纶面料的保暖性能有重要影响。As can be seen from Table 2, the Kroger values of polyester fabrics a, b, and c are in the range of 1.08 to 1.18, respectively, which are higher than the Kroger values of unfinished polyester fabrics; after 10 times of washing, the Kroger values of fabrics a, b, and c still do not decrease significantly. The higher the Kroger value, the better the warmth retention of the fabric. It can be considered that the polyester fabric prepared by the present invention has good warmth retention performance. The warmth retention performance of polyester fabrics d, e, and f prepared in comparative examples A-C is slightly worse than that of fabrics a, b, and c, which indicates that the amount of emulsifier Span 80, the temperature and time of the cross-linking reaction, and the amount of azobisisobutyronitrile all have an important influence on the warmth retention performance of the polyester fabric.

综合分析认为,本发明制备的涤纶面料在不影响透气性的前提下具有较好的保暖性能。Comprehensive analysis shows that the polyester fabric prepared by the present invention has good thermal insulation performance without affecting the air permeability.

Claims (3)

1.一种基于电气石粉的保暖涤纶面料的制备方法,其特征在于,所述制备方法包含以下步骤:1. A method for preparing a warm polyester fabric based on tourmaline powder, characterized in that the preparation method comprises the following steps: (1)纳米电气石粉的制备:将电气石粉进行研磨,制得粒径为纳米级的电气石粉粒子;(1) Preparation of nano tourmaline powder: Grinding the tourmaline powder to obtain tourmaline powder particles with a particle size of nanometers; (2)水解:在室温下,将乳化剂司班80溶于去离子水,搅拌均匀,加入硅烷偶联剂KH-570,进行乳化,制得硅烷偶联剂KH-570水解液;(2) Hydrolysis: dissolve the emulsifier Span 80 in deionized water at room temperature, stir evenly, add the silane coupling agent KH-570, emulsify, and prepare the silane coupling agent KH-570 hydrolyzate; (3)交联反应:将步骤(2)制得的硅烷偶联剂KH-570水解液溶于二甲基甲酰胺,制得稀释液;将步骤(1)制得的纳米级电气石粉加入稀释液,搅拌反应,制得交联改性的纳米级电气石粉溶液;(3) Cross-linking reaction: dissolving the hydrolyzate of silane coupling agent KH-570 obtained in step (2) in dimethylformamide to obtain a diluent; adding the nano-scale tourmaline powder obtained in step (1) to the diluent, stirring and reacting, to obtain a cross-linked modified nano-scale tourmaline powder solution; (4)整理液的配制:将偶氮二异丁腈溶解于步骤(3)制得的交联改性的纳米级电气石粉溶液,搅拌配制整理液;(4) Preparation of finishing liquid: dissolving azobisisobutyronitrile in the cross-linked modified nano-scale tourmaline powder solution prepared in step (3), and stirring to prepare a finishing liquid; (5)整理:将步骤(4)制得的整理液加热到90~100℃,将涤纶面料放入整理液浸渍1~2小时;取出浸渍后的涤纶面料用大量自来水清洗,烘干,制得保暖涤纶面料;(5) Finishing: heating the finishing liquid obtained in step (4) to 90-100° C., and immersing the polyester fabric in the finishing liquid for 1-2 hours; taking out the immersed polyester fabric, washing it with a large amount of tap water, and drying it to obtain a warm polyester fabric; 步骤(1)中所述粒径范围为500~2000纳米;The particle size range of step (1) is 500 to 2000 nanometers; 步骤(2)中所述乳化剂司班80、硅烷偶联剂KH-570和去离子水的用量比为1g∶(1~2)g∶(200~400)mL;所述搅拌时间为10~20min;所述乳化时间为10~20min;In step (2), the ratio of the emulsifier Siban 80, the silane coupling agent KH-570 and the deionized water is 1 g: (1-2) g: (200-400) mL; the stirring time is 10-20 min; the emulsification time is 10-20 min; 步骤(3)中所述KH-570交联剂水解液与二甲基甲酰胺的用量比为1mL∶(10~20)mL;所述纳米级电气石粉与稀释液的用量比为1g∶(100~200)mL;In step (3), the ratio of the KH-570 crosslinking agent hydrolyzate to dimethylformamide is 1 mL: (10-20) mL; the ratio of the nano-scale tourmaline powder to the diluent is 1 g: (100-200) mL; 步骤(3)中所述反应温度为60~80℃,反应时间为3~5h;The reaction temperature in step (3) is 60-80°C and the reaction time is 3-5h; 步骤(4)中所述偶氮二异丁腈与步骤(3)制得的交联改性的纳米级电气石粉溶液用量比为1g∶(100~200)mL。The amount ratio of azobisisobutyronitrile in step (4) to the cross-linked modified nano-scale tourmaline powder solution prepared in step (3) is 1 g: (100-200) mL. 2.根据权利要求1所述的一种基于电气石粉的保暖涤纶面料的制备方法,其特征在于,步骤(5)中所述涤纶面料与整理液的用量比为1g∶(20~40)mL。2. The method for preparing a thermal insulation polyester fabric based on tourmaline powder according to claim 1, characterized in that the dosage ratio of the polyester fabric to the finishing liquid in step (5) is 1 g: (20-40) mL. 3.一种基于电气石粉的保暖涤纶面料,其特征在于,采用权利要求1~2中任一项所述方法制备而成。3. A warm-keeping polyester fabric based on tourmaline powder, characterized in that it is prepared by the method described in any one of claims 1 to 2.
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