CN102677471A - Method for preparing temperature regulation textile by sol-gel technology - Google Patents
Method for preparing temperature regulation textile by sol-gel technology Download PDFInfo
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- CN102677471A CN102677471A CN2012101724660A CN201210172466A CN102677471A CN 102677471 A CN102677471 A CN 102677471A CN 2012101724660 A CN2012101724660 A CN 2012101724660A CN 201210172466 A CN201210172466 A CN 201210172466A CN 102677471 A CN102677471 A CN 102677471A
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Abstract
The invention discloses a method for preparing temperature regulation textile by a sol-gel technology. The method for preparing the temperature regulation textile by the sol-gel technology comprises the steps of adding tetraethoxysilane into mixed liquid of ethanol and water to prepare tetraethoxysilane liquid preparation liquid, and adjusting pH value to 2-4; respectively adding paraffin wax, water and an emulsifying agent into a high-speed emulsion machine to prepare paraffin core emulsion; slowly dropping the tetraethoxysilane liquid preparation liquid into the paraffin core emulsion, and adding synthetic latex to prepare phase change micro-capsule finishing liquid; settling the phase change micro-capsule finishing liquid on the textile through a two-soaking and two-rolling method, and baking to obtain the temperature regulation textile. According to the invention, by adopting the sol-gel method and the phase change micro-capsule finishing liquid taking tetraethoxysilane as wall material and paraffin as core material to prepare the temperature regulation textile, the defect that polymers such as urea resin and the like are taken as the wall material is solved, the heat conduction efficiency and the physical and chemical stability are improved, and the excellent non-toxic and harmless performances are provided.
Description
Technical field
The invention belongs to chemical technology field, be specifically related to a kind of method of sol-gel technology preparing temperature adjustment fabric.
Background technology
The solid-liquid phase change material has that Volume Changes is little in phase transition process, heat content is big, so each field is more relatively to its research, and uses also extensive relatively.But solid-liquid phase change material form in phase transition process is unstable, has limited its application.In order to address this problem, adopt microencapsulated technology more, phase-change material is coated in the wall material, thereby restriction liquid phase-change material is mobile.Microcapsules are often referred to the molecule of diameter between the 1-1000 micron, and along with the development of technology, capsule diameter also can reach nanoscale.Because capsule for receiving microstage, makes microcapsules when solving solid-liquid phase change material leakage problem, and big heat transfer area also is provided, and has effectively improved heat transfer efficiency.Prevent contacting of phase-change material and other materials simultaneously, prevented the change of material character, increased the number of times that utilizes of phase-change material.The research of microcapsules technology starts from the fifties in last century, and 1954 by the B.KGreen of American National cash handler company (NCR) invention and be used to produce NCR, thereby has started the epoch of microcapsules new technologies.The eighties in last century, US National Aeronautics and Space Administration (NASA) is applied to the thermal conditioning protective clothes with microencapsulated phase change material and avoids the interference of space high temperature with protection space precision instrument, and so far, microencapsulated phase change material becomes the focus that the countries in the world researcher pays close attention to.The nineties in 20th century, U.S. Triangle company has synthesized the microcapsules with heat absorption and release function, and it is organized in fabric face, has obtained having the textiles of temp regulating function.At present, phase-change microcapsule has obtained in a plurality of fields such as weaving, building, industrial afterheat recovery using widely.
At present, phase-change microcapsule adopts situ aggregation method or interfacial polymerization to coat more, is the wall material like Liu Xing, Wang Shujun etc. with the melamine urea-formaldehyde resin, and paraffin is core, adopts situ aggregation method to prepare the phase-changing and temperature-regulating microcapsules.Lai Maobai, Sun Rong etc. use paraffin to be core, and methyl methacrylate is the wall material, adopt interfacial polymerization to prepare phase-change microcapsule.The monomer wide range of situ aggregation method be soluble but require monomer, and polymer is insoluble.Advantages such as interfacial polymerization requires not tight to proportioning raw materials, reaction rate is fast, and is effective, can carry out at normal temperatures, and temperature control is simple are carried out polycondensation reaction but the monomer of its use must have higher activity.In addition; Adopt situ aggregation method and interfacial polymerization production phase-change microcapsule, mostly cyst wall is high polymer, like the copolymer of Lauxite, melamine and formaldehyde etc.; This analog copolymer has combustibility; And this type wall material has certain harm to human body, has increased potential safety hazard, is unfavorable for the weaving face fabric application.In addition, this analog copolymer makes between the phase-change microcapsule for preparing inter-adhesive, and thermal conductivity is low, has limited the performance of phase-change material thermoregulatory effect.Based on above present situation, the people's wall material of other preparation methods of phase-change microcapsule material more remarkable that begin one's study as phase-change material with adopting more environmental protection, performance.
Summary of the invention
The method that the purpose of this invention is to provide a kind of sol-gel coated phase-change microcapsules makes phase-change microcapsule have good heat-conductive characteristic and better chemical stability.
In order to achieve the above object, the invention provides a kind of method of sol-gel technology preparing temperature adjustment fabric, it is characterized in that, may further comprise the steps:
The first step: take by weighing paraffin 5-15 part, ethyl orthosilicate 5-15 part, emulsifying agent 20-30 part, synthetic latex 10-20 part, ethanol 10-20 part and water 50-70 part respectively in mass fraction, for use;
Second step: under churned mechanically condition, 5-15 part ethyl orthosilicate is joined in the mixed liquor of 10-20 part ethanol and 10-20 part water, be mixed with ethyl orthosilicate liquid system liquid, the pH value is adjusted to 2-4;
The 3rd step: respectively 5-15 part paraffin, remaining water and 20-30 part emulsifying agent are joined in the high-speed emulsifying machine, be mixed with the paraffin core emulsion;
The 4th step: under 55-60 ℃, churned mechanically condition, the ethyl orthosilicate liquid system liquid that second step was obtained adds synthetic latex after slowly being added drop-wise in the paraffin core emulsion that the 3rd step obtained, and stirring is mixed with the phase-change microcapsule dressing liquid;
The 5th step: the phase-change microcapsule dressing liquid that the 4th step obtained is put in order on the fabric through two two methods of rolling of soaking, processed the temperature adjustment fabric, pressure is 2-3kg/cm
2, liquid carrying rate is 60-70%;
The 6th step: the temperature adjustment fabric that the 5th step made is dried down at 70-80 ℃, under 100-180 ℃, baked 3-5 minute again.
Preferably, the emulsifying agent in the described first step is nonionic fatty alcohols APEO or nonionic fatty alcohols APEO propylene ether.
Preferably, the synthetic latex in the described first step is acrylic latex or aqueous emulsion of polyurethane.
Preferably, the churned mechanically parameter in described second step is: rotating speed 300-500 rev/min, and mixing time 2-4 hour.
Preferably, the rotating speed of the high-speed emulsifying machine in described the 3rd step is 10000 rev/mins, and emulsification times is 20-30 minute.
Preferably, the mixing speed in described the 4th step is 300-500 rev/min, and mixing time is 2 hours.
The present invention adopts sol-gal process; With ethyl orthosilicate (TEOS) is the wall material; Paraffin is the little glue dressing liquid of the phase transformation of core material, the temperature adjustment fabric that makes, and having solved polymer such as Lauxite is the shortcoming of wall material; Improve heat transfer efficiency, physical and chemical stability, and had good nontoxic premium properties.Technological process of the present invention is simple, and condition is prone to control, and production cost is lower, and applicability is wide; The cost of material that adopts is cheap, wide material sources, but industrial applications.
Description of drawings
Fig. 1 is for adopting the intensification performance test figure of temperature adjustment fabric before and after extraneous variation of ambient temperature of the present invention's preparation;
Fig. 2 is for adopting the temperature reduction performance resolution chart of temperature adjustment fabric before and after extraneous variation of ambient temperature of the present invention's preparation.
The specific embodiment
Below in conjunction with embodiment the present invention is set forth in detail.
Paraffin among the embodiment 1-4 is available from Shanghai China paraffin Co., Ltd forever; Ethyl orthosilicate is available from Shanghai chemical reagent Co., Ltd of Chinese Medicine group; The emulsifying agent emulsifying agent adopts AEO, available from Basf China Co., Ltd; Synthetic latex adopts acrylic latex, available from available from Basf China Co., Ltd.
Embodiment 1
The first step: the 7g ethyl orthosilicate under 400 rev/mins mechanical agitation, is dissolved in the mixed liquor of 14.3g ethanol and 15g water, and using the salt acid for adjusting pH value is 2.6, stirs 3 hours, forms the ethyl orthosilicate liquid system liquid of stable uniform;
Second step: in high-speed emulsifying machine, add 6g paraffin, 37.8g water and 13g emulsifying agent, emulsification is 30 minutes under 10000 rev/mins condition, forms the paraffin core emulsion of stable uniform;
The 3rd step: under 60 ℃, 400 rev/mins mechanical agitation; After the ethyl orthosilicate liquid system liquid that the first step is obtained slowly is added drop-wise in the paraffin core emulsion that second step obtained; Add the 10g acrylic latex, be mixed with the phase-change microcapsule dressing liquid, evenly stirred 2 hours.
Embodiment 2
The first step: the 5g ethyl orthosilicate under 400 rev/mins mechanical agitation, is dissolved in the mixed liquor of 11g ethanol and 11g water, and using the salt acid for adjusting pH value is 2.6, stirs 3 hours, forms the ethyl orthosilicate liquid system liquid of stable uniform;
Second step: in high-speed emulsifying machine, add 5g paraffin, 29g water and 10g emulsifying agent, emulsification is 30 minutes under 10000 rev/mins condition, forms the paraffin core emulsion of stable uniform;
The 3rd step: under 60 ℃, 400 rev/mins mechanical agitation; After the ethyl orthosilicate liquid system liquid that the first step is obtained slowly is added drop-wise in the paraffin core emulsion that second step obtained; Add the 8g acrylic latex, be mixed with the phase-change microcapsule dressing liquid, evenly stirred 2 hours.
Embodiment 3
The first step: the 10g ethyl orthosilicate under 400 rev/mins mechanical agitation, is dissolved in the mixed liquor of 26g ethanol and 24g water, and using the salt acid for adjusting pH value is 3.1, stirs 3 hours, forms the ethyl orthosilicate liquid system liquid of stable uniform;
Second step: in high-speed emulsifying machine, add 13g paraffin, 68g water and 24g emulsifying agent, emulsification is 30 minutes under 10000 rev/mins condition, forms the paraffin core emulsion of stable uniform;
The 3rd step: under 60 ℃, 400 rev/mins mechanical agitation; After the ethyl orthosilicate liquid system liquid that the first step is obtained slowly is added drop-wise in the paraffin core emulsion that second step obtained; Add the 19g acrylic latex, be mixed with the phase-change microcapsule dressing liquid, evenly stirred 2 hours.
Embodiment 4
The phase-change microcapsule dressing liquid that embodiment 1-3 is made is put the plain woven cotton in order through two two methods of rolling of soaking respectively, and (grammes per square metre is 140g/m
2) on, process the temperature adjustment fabric, pressure is 3kg/cm
2, liquid carrying rate is 70%; Then, 70 ℃ of oven dry in convection oven bake at 150 ℃ at last and got final product in 3 minutes.
Respectively original fabrics and above-mentioned temperature adjustment fabric are tested its heat-insulating property through GB/T 11048-1989, utilize SFJJ-606PC type fabric heat-insulation property testing appearance, according to constant temperature difference cooling method, insulation rate, heat transfer coefficient and the clo value of test and acquisition fabric.Test result is tabulated as follows:
Fabric heat-insulation performance test before and after table 1 arrangement
Visible by table 1, the heat insulating ability of temperature adjustment fabric all has apparent in view raising than original fabrics.Along with the insulation rate for preparing the increase fabric of microcapsule content in the liquid also has tangible increase, the also corresponding increase of clo value, heat transfer coefficient reduces with the increase of microcapsule content in the preparation liquid.
Test original fabrics and the above-mentioned temperature adjustment fabric lifting/lowering warm nature ability before and after extraneous variation of ambient temperature, method of testing is following:
1, heating and cooling performance test: (temperature is 20 ± 2 ℃ respectively original fabrics and above-mentioned temperature adjustment fabric to be placed in the environment of constant temperature and humidity balance 24h; Relative humidity 65 ± 3%); Be placed on then on 36 ℃ the warming plate; With the temperature of infrared radiation thermometer mensuration fabric face, every separated 10s record once is depicted as the fabric heating curve.
2, temperature reduction performance test: respectively original fabrics and above-mentioned temperature adjustment fabric are placed on heat tracing balance 2h in 40 ℃ the baking oven; Take out then and naturally cool to room temperature (temperature is 20 ± 2 ℃; Relative humidity 65 ± 3%); With the temperature of infrared radiation thermometer mensuration fabric face, every separated 10s record once is depicted as the fabric temperature lowering curve.
Figure is as shown in Figure 1 in the intensification performance test, and the temperature reduction performance resolution chart is as shown in Figure 2.The heating rate of temperature adjustment fabric and rate of temperature fall all descend than source textile to some extent, and the degree that descends increases with the increase for preparing the content of microcapsules in the liquid.As can be seen from Figure 1, through arrangement back fabric to external world variations in temperature played tangible cushioning effect.
Claims (6)
1. the method for a sol-gel technology preparing temperature adjustment fabric is characterized in that, may further comprise the steps:
The first step: take by weighing paraffin 5-15 part, ethyl orthosilicate 5-15 part, emulsifying agent 20-30 part, synthetic latex 10-20 part, ethanol 10-20 part and water 50-70 part respectively in mass fraction, for use;
Second step: under churned mechanically condition, 5-15 part ethyl orthosilicate is joined in the mixed liquor of 10-20 part ethanol and 10-20 part water, be mixed with ethyl orthosilicate liquid system liquid, the pH value is adjusted to 2-4;
The 3rd step: respectively 5-15 part paraffin, remaining water and 20-30 part emulsifying agent are joined in the high-speed emulsifying machine, be mixed with the paraffin core emulsion;
The 4th step: under 55-60 ℃, churned mechanically condition, the ethyl orthosilicate liquid system liquid that second step was obtained adds synthetic latex after slowly being added drop-wise in the paraffin core emulsion that the 3rd step obtained, and stirring is mixed with the phase-change microcapsule dressing liquid;
The 5th step: the phase-change microcapsule dressing liquid that the 4th step obtained is put in order on the fabric through two two methods of rolling of soaking, processed the temperature adjustment fabric, pressure is 2-3kg/cm
2, liquid carrying rate is 60-70%;
The 6th step: the temperature adjustment fabric that the 5th step made is dried down at 70-80 ℃, under 100-180 ℃, baked 3-5 minute again.
2. the method for sol-gel technology preparing temperature adjustment fabric as claimed in claim 1 is characterized in that, the emulsifying agent in the described first step is nonionic fatty alcohols APEO or nonionic fatty alcohols APEO propylene ether.
3. the method for sol-gel technology preparing temperature adjustment fabric as claimed in claim 1 is characterized in that, the synthetic latex in the described first step is acrylic latex or aqueous emulsion of polyurethane.
4. the method for sol-gel technology preparing temperature adjustment fabric as claimed in claim 1 is characterized in that, the churned mechanically parameter in described second step is: rotating speed 300-500 rev/min, and mixing time 2-4 hour.
5. the method for sol-gel technology preparing temperature adjustment fabric as claimed in claim 1 is characterized in that, the rotating speed of the high-speed emulsifying machine in described the 3rd step is 10000 rev/mins, and emulsification times is 20-30 minute.
6. the method for sol-gel technology preparing temperature adjustment fabric as claimed in claim 1 is characterized in that, the mixing speed in described the 4th step is 300-500 rev/min, and mixing time is 2 hours.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103088647A (en) * | 2012-12-12 | 2013-05-08 | 吴江麦道纺织有限公司 | Processing technology of heat-storage and temperature-regulation cloth |
| CN103320096A (en) * | 2013-07-11 | 2013-09-25 | 中国科学院广州能源研究所 | Phase change energy storage capsule and preparation method thereof |
| CN103806285A (en) * | 2013-10-11 | 2014-05-21 | 天津市中科健新材料技术有限公司 | Method for manufacturing constant-temperature non-woven cloth for sanitary product |
| GB2544395A (en) * | 2015-09-25 | 2017-05-17 | Mitsubishi Materials Corp | Precious metal clay regeneration solution and method for regenerating precious metal clay |
| CN106833540A (en) * | 2017-01-19 | 2017-06-13 | 苏州鸿凌达电子科技有限公司 | Phase-changing energy storage material microcapsules and its manufacture craft |
| CN107384328A (en) * | 2017-08-11 | 2017-11-24 | 中国科学院化学研究所 | A kind of preparation method of phase-change microcapsule of inorganic material coating and its product and application |
| CN107475860A (en) * | 2017-07-10 | 2017-12-15 | 青田起步儿童用品有限公司 | A kind of cotton fibre material of constant-temperature warm-keeping and preparation method thereof |
| CN107513375A (en) * | 2017-08-11 | 2017-12-26 | 中国科学院化学研究所 | A kind of phase-change microcapsule of coated with silica and its preparation method and application |
| CN109554919A (en) * | 2018-12-04 | 2019-04-02 | 江苏金太阳纺织科技股份有限公司 | A kind of skin care antibacterial microcapsule finishing agent and its preparation method and application |
| WO2020077555A1 (en) * | 2018-10-17 | 2020-04-23 | Dow Global Technologies Llc | Gel comprising hybrid phase change materials |
| CN114687076A (en) * | 2022-03-15 | 2022-07-01 | 冠和卫生用品有限公司 | Temperature-adjusting non-woven fabric and preparation method thereof |
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103088647A (en) * | 2012-12-12 | 2013-05-08 | 吴江麦道纺织有限公司 | Processing technology of heat-storage and temperature-regulation cloth |
| CN103320096A (en) * | 2013-07-11 | 2013-09-25 | 中国科学院广州能源研究所 | Phase change energy storage capsule and preparation method thereof |
| CN103320096B (en) * | 2013-07-11 | 2015-06-24 | 中国科学院广州能源研究所 | Phase change energy storage capsule and preparation method thereof |
| CN103806285A (en) * | 2013-10-11 | 2014-05-21 | 天津市中科健新材料技术有限公司 | Method for manufacturing constant-temperature non-woven cloth for sanitary product |
| CN103806285B (en) * | 2013-10-11 | 2016-05-11 | 天津市中科健新材料技术有限公司 | A kind of constant temperature nonwoven preparation method for hygienic articles |
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| US9868669B2 (en) | 2015-09-25 | 2018-01-16 | Mitsubishi Materials Corporation | Precious metal clay regeneration solution and method for regenerating precious metal clay |
| GB2544395A (en) * | 2015-09-25 | 2017-05-17 | Mitsubishi Materials Corp | Precious metal clay regeneration solution and method for regenerating precious metal clay |
| CN106833540A (en) * | 2017-01-19 | 2017-06-13 | 苏州鸿凌达电子科技有限公司 | Phase-changing energy storage material microcapsules and its manufacture craft |
| CN107475860A (en) * | 2017-07-10 | 2017-12-15 | 青田起步儿童用品有限公司 | A kind of cotton fibre material of constant-temperature warm-keeping and preparation method thereof |
| CN107384328A (en) * | 2017-08-11 | 2017-11-24 | 中国科学院化学研究所 | A kind of preparation method of phase-change microcapsule of inorganic material coating and its product and application |
| CN107513375A (en) * | 2017-08-11 | 2017-12-26 | 中国科学院化学研究所 | A kind of phase-change microcapsule of coated with silica and its preparation method and application |
| WO2020077555A1 (en) * | 2018-10-17 | 2020-04-23 | Dow Global Technologies Llc | Gel comprising hybrid phase change materials |
| CN109554919A (en) * | 2018-12-04 | 2019-04-02 | 江苏金太阳纺织科技股份有限公司 | A kind of skin care antibacterial microcapsule finishing agent and its preparation method and application |
| WO2020113903A1 (en) * | 2018-12-04 | 2020-06-11 | 江苏金太阳纺织科技股份有限公司 | Skincare and antibacterial microcapsule finishing agent, and preparation method therefor and application thereof |
| CN114687076A (en) * | 2022-03-15 | 2022-07-01 | 冠和卫生用品有限公司 | Temperature-adjusting non-woven fabric and preparation method thereof |
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Application publication date: 20120919 |