CN104233787A - Preparation method of nano silicon dioxide-modified compound fabric - Google Patents
Preparation method of nano silicon dioxide-modified compound fabric Download PDFInfo
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- CN104233787A CN104233787A CN201410469361.0A CN201410469361A CN104233787A CN 104233787 A CN104233787 A CN 104233787A CN 201410469361 A CN201410469361 A CN 201410469361A CN 104233787 A CN104233787 A CN 104233787A
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Abstract
The invention discloses a preparation method of nano silicon dioxide-modified compound fabric. The method comprises the steps of mixing absolute ethyl alcohol, deionized water and ammonia water, evenly mixing at the reaction temperature of 25-30 DEG C, and adding mixed liquid of absolute ethyl alcohol and ethyl orthosilicate to obtain silicon dioxide reaction liquid, wherein the ratio of absolute ethyl alcohol to ethyl orthosilicate in the mixed liquid is 4: 1; stirring the reaction liquid for 3-5 minutes, and then carrying out a reaction for 24-32 hours to obtain colloid microsphere suspension liquid; carrying out centrifugal separation on the colloid microsphere suspension liquid to obtain silicon dioxide colloidal particles; diluting the silicon dioxide colloidal particles by using absolute ethyl alcohol to obtain suspension liquid of the silicon dioxide colloidal particles; dipping the base fabric in the suspension liquid of the silicon dioxide colloidal particles, and carrying out gel ageing and supercritical drying to obtain the silicon dioxide-modified compound fabric, wherein the concentration of the ammonia water in the silicon dioxide reaction liquid is 0.28-0.54mol/L, the concentration of water in the silicon dioxide reaction liquid is 4.15-6.68mol/ L, and the concentration of ethyl orthosilicate in the silicon dioxide reaction liquid is 0.10-0.35mol/L. The silicon dioxide colloidal particles evenly cover the surface of the fabric, so that the obtained silicon dioxide-modified compound fabric also has good flame retardant property.
Description
Technical field
The present invention relates to chemical synthesis fabric technology, especially relate to a kind of preparation method of nano-silicon dioxide modified composite fabric.
Background technology
Due to " small-size effect ", " interfacial effect ", " quantum size effect " and " macro quanta tunnel effect " that nano material has, nano material is made to show the specificity different from common material in structure, photoelectricity, magnetic and chemical property etc.
Silica (SiO
2) aeroge is typical nano-pore ultra heat insulating material, it is the nano-porous materials that a kind of nano particle is assembled mutually, having much special character, as high-specific surface area, low-density, high porosity, lower thermal conductivity, is the lightest, the solid material that effect of heat insulation is best that find at present.
Work as SiO
2aeroge colloid micro ball is that the achievement in research that construction unit builds colloidal crystal by self-assembling method has had a large amount of report, colloidal crystal structure is the dielectric material that a class has periodic arrangement structure, its the most significant feature has forbidden photon band, when visible ray falls into this forbidden band, the light of specific wavelength will not by, and coherent diffraction is there is on surface, produce gorgeous schemochrome, there is high brightness, high saturation, the feature such as will never fade.
Therefore, how by control SiO
2aerogel particles and textiles compound, control the color of composite fabric, becomes current and be badly in need of one of technical barrier solved.
Summary of the invention
For overcoming the defect of prior art, the present invention proposes a kind of preparation method of nano-silicon dioxide modified composite fabric, by control SiO
2aerogel particles particle diameter adjusts the color of modification composite fabric.
The present invention adopts following technical scheme to realize: a kind of preparation method of nano-silicon dioxide modified composite fabric, and it comprises step:
A, prepare silicon dioxide colloid particulate: after absolute ethyl alcohol, deionized water and ammoniacal liquor being mixed, stir at reaction temperature 25 DEG C ~ 30 DEG C, add absolute ethyl alcohol and the ethyl orthosilicate mixed liquor of 4:1, obtain silicon dioxde reaction liquid, react 24 ~ 32 hours after above-mentioned reactant liquor being stirred 3-5min, the colloid micro ball suspension obtained, centrifugation obtains silicon dioxide colloid particulate;
B, silicon dioxide colloid particulate absolute ethyl alcohol to be diluted, obtain silicon dioxide colloid microparticle suspending liquid, substrate fabric is immersed in this suspension, keep 48 ~ 84 hours under constant-temperature constant-humidity environment, until after etoh solvent volatilizees completely, and carry out the aging and supercritical drying of gel, obtain silica modified composite fabric;
In above-mentioned silicon dioxde reaction liquid, the concentration of ammoniacal liquor is 0.28 ~ 0.54mol/L, and the concentration of water is 4.15 ~ 6.68mol/L, and the concentration of ethyl orthosilicate is 0.10 ~ 0.35mol/L.
Wherein, substrate fabric is that terylene, cotton or high strength synthetic fibre are made.
Wherein, high strength synthetic fibre is the wherein a kind of of aramid fiber, carbon fiber and high-strength polyethylene fiber.
Wherein, described supercritical drying carries out under temperature is 40-75 DEG C and pressure is the environment of 15-30MPa.
Wherein, gel ageing time is 2 ~ 12 hours.
Compared with prior art, the present invention has following beneficial effect:
The present invention is by preparing the particle size of silicon dioxide colloid particulate, adopt gravitational sedimentation self-assembly method on substrate fabric, silicon dioxide colloid particle size evenly and smooth in appearance, fabric face can be covered uniformly, and the color of modification composite fabric can be adjusted by the particle size of adjustment silicon dioxide colloid particulate.In addition, because the parcel of silicon dioxide colloid to silica modified composite fabric surface makes itself nonflammable, that is, silica modified composite fabric provided by the invention also has good fire resistance.
Detailed description of the invention
Further explanation and description of the technical solution of the present invention are carried out below in conjunction with specific embodiments.
The present invention includes following steps:
First, SiO is prepared
2aeroge (i.e. silicon dioxide colloid) particulate.
By absolute ethyl alcohol, deionized water and ammoniacal liquor, open constant temperature blender with magnetic force, 10min (300r/min) is stirred at controlling reaction temperature 25 DEG C ~ 30 DEG C, absolute ethyl alcohol and the ethyl orthosilicate mixed liquor of 4:1 is added after mixing, obtain silicon dioxde reaction liquid, wherein, in above-mentioned reactant liquor, the concentration of ammoniacal liquor is 0.28 ~ 0.54mol/L, the concentration of water is 4.15 ~ 6.68mol/L, and the concentration of ethyl orthosilicate is 0.10 ~ 0.35mol/L; Under certain rotating speed (300r/min) and temperature (25 DEG C), 24-32 hour is reacted, until reaction terminates by after above-mentioned reactant liquor rapid stirring 3-5min; Utilize centrifuge in 6000r/min centrifugation the colloid micro ball suspension obtained, be separated rear deionized water and absolute ethyl alcohol respectively cleans three times, and in temperature 80 DEG C ~ 90 DEG C oven dry, obtained SiO
2aerogel particles.
Wherein, ammoniacal liquor prepares SiO as catalyst poly-condensation and hydrolysis
2aerogel particles, therefore, the increase of ammoniacal liquor concentration in above-mentioned reactant liquor will accelerate hydrolysis rate and the polycondensation speed of ethyl orthosilicate, easily make large weight oligomers be polymerized the SiO generating greater particle size
2aerogel particles, but the ammonia concn of too high levels will cause, in accumulation process, SiO occurs
2the sedimentation of aerogel particles, therefore, the present invention selects the content of ammoniacal liquor in above-mentioned reactant liquor to be 0.28 ~ 0.54mol/L, is beneficial to generate the suitable SiO of particle diameter
2aerogel particles.
The increase of water content in above-mentioned reactant liquor, the hydrolysis rate of ethyl orthosilicate accelerates, and nucleation number and rate of polymerization increase simultaneously, the SiO of generation
2the particle diameter of aerogel particles also increases thereupon.But too high water content meeting weak ammonia and the concentration of ethyl orthosilicate, easily make SiO on the contrary
2the particle diameter of aerogel particles reduces.Therefore, the present invention selects the content of water in above-mentioned reactant liquor to be 4.15 ~ 6.68mol/L, both can synthesize monodispersed SiO
2aerogel particles, can avoid again the SiO that water consumption too high generation particle diameter is too small
2aerogel particles.
The increase of ethyl orthosilicate content in above-mentioned reactant liquor, the SiO of generation
2the particle diameter of aerogel particles also increases thereupon.But in mixed liquor, the teos hydrolysis of too high levels can produce a large amount of ions after reacting, and these ion concentrations increase with ethyl orthosilicate concentration and increase, and reduces SiO
2aerogel particles surface elecrtonegativity, increase the possibility occurring to assemble, therefore the ethyl orthosilicate content of excessive concentrations can cause SiO
2the reduction of aerogel particles monodispersity with and there is sedimentation, therefore the present invention selects the content of ethyl orthosilicate in above-mentioned reactant liquor to be 0.10 ~ 0.35mol/L.
Secondly, the silicon dioxide colloid particulate absolute ethyl alcohol prepared is diluted, obtains SiO
2aerogel particles suspension.
Finally, using as the textile impregnation of substrate at SiO
2aerogel particles suspension, under constant-temperature constant-humidity environment (25 DEG C, relative humidity 60%) keep 48 ~ 84 hours, until after etoh solvent volatilizees completely, and it is aging to carry out gel, finally carry out supercritical drying (temperature of described drying is 40-75 DEG C, and pressure is 15-30MPa), obtain silica modified composite fabric.
Wherein, substrate fabric also can be high strength synthetic fibre, is such as the one in aramid fiber, carbon fiber, high-strength polyethylene fiber.
The present invention is further illustrated below with a preferred embodiment:
Preparation SiO
2during aerogel particles, by absolute ethyl alcohol, deionized water and ammoniacal liquor, open constant temperature blender with magnetic force, stir 10min (300r/min) at controlling reaction temperature 25 DEG C, add absolute ethyl alcohol and the ethyl orthosilicate mixed liquor of 4:1 after mixing, obtain silicon dioxde reaction liquid, wherein, in above-mentioned reactant liquor, the content of ammoniacal liquor is 0.48mol/L, and the content of water is 6.38mol/L, and the content of ethyl orthosilicate is 0.32mol/L; React after above-mentioned reactant liquor rapid stirring 3min 24 hours under certain rotating speed (300r/min) and temperature (25 DEG C), until reaction terminates; Utilize centrifuge in 6000r/min centrifugation the colloid micro ball suspension obtained, be separated rear deionized water and absolute ethyl alcohol respectively cleans three times, and in temperature 80 DEG C oven dry, obtained SiO
2aerogel particles.
Through particle size analyzer test SiO
2aerogel particles, finds SiO
2the average grain diameter of aerogel particles is between 215.6nm ~ 282.3nm.At electric Microscopic observation SiO
2aerogel particles, finds the SiO prepared
2aerogel particles smooth surface, good sphericity, size is homogeneous, has good monodispersity.
The SiO just prepared
2aerogel particles absolute ethyl alcohol is diluted to 1.0wt%, and ultrasonic disperse is even; First using the dacron deionized water ultrasonic cleaning 10min as substrate, then by textile impregnation at SiO
2aerogel particles suspension, under constant-temperature constant-humidity environment, (25 DEG C, relative humidity 60%) keep 64 hours, until after etoh solvent volatilizees completely, and it is aging to carry out gel, finally carries out supercritical drying.Obtain silica modified composite fabric.
Can be found by the silica modified composite fabric of 3 D video microscopic examination, SiO
2aerogel particles uniform fold is on dacron surface.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (5)
1. a preparation method for nano-silicon dioxide modified composite fabric, is characterized in that, comprises step:
A, prepare silicon dioxide colloid particulate: after absolute ethyl alcohol, deionized water and ammoniacal liquor being mixed, stir at reaction temperature 25 DEG C ~ 30 DEG C, add absolute ethyl alcohol and the ethyl orthosilicate mixed liquor of 4:1, obtain silicon dioxde reaction liquid, react 24 ~ 32 hours after above-mentioned reactant liquor being stirred 3-5min, the colloid micro ball suspension obtained, centrifugation obtains silicon dioxide colloid particulate;
B, silicon dioxide colloid particulate absolute ethyl alcohol to be diluted, obtain silicon dioxide colloid microparticle suspending liquid, substrate fabric is immersed in this suspension, keep 48 ~ 84 hours under constant-temperature constant-humidity environment, until after etoh solvent volatilizees completely, and carry out the aging and supercritical drying of gel, obtain silica modified composite fabric;
In above-mentioned silicon dioxde reaction liquid, the concentration of ammoniacal liquor is 0.28 ~ 0.54mol/L, and the concentration of water is 4.15 ~ 6.68mol/L, and the concentration of ethyl orthosilicate is 0.10 ~ 0.35mol/L.
2. the preparation method of nano-silicon dioxide modified composite fabric according to claim 1, it is characterized in that, substrate fabric is that terylene, cotton or high strength synthetic fibre are made.
3. the preparation method of nano-silicon dioxide modified composite fabric according to claim 2, is characterized in that, high strength synthetic fibre is the wherein a kind of of aramid fiber, carbon fiber and high-strength polyethylene fiber.
4. the preparation method of nano-silicon dioxide modified composite fabric according to claim 1, it is characterized in that, described supercritical drying carries out under temperature is 40-75 DEG C and pressure is the environment of 15-30MPa.
5. the preparation method of nano-silicon dioxide modified composite fabric according to claim 1, it is characterized in that, gel ageing time is 2 ~ 12 hours.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105369600A (en) * | 2015-12-24 | 2016-03-02 | 西南大学 | Preparation method of cotton fabric with electrical conductivity, electromagnetic shielding and flame-retardant functions |
| CN106436285A (en) * | 2016-07-28 | 2017-02-22 | 东华大学 | Preparation and application of intumescent flame retardant system doped silica sol |
| CN107287979A (en) * | 2016-03-30 | 2017-10-24 | 新材料与产业技术北京研究院 | A kind of nano silicon compound pulp and preparation method thereof and page |
| CN108823968A (en) * | 2018-05-28 | 2018-11-16 | 江苏阳光股份有限公司 | A kind of preparation method of flame resistant wool fabric |
| CN109457485A (en) * | 2018-10-11 | 2019-03-12 | 浙江鹏辰新材料有限公司 | A kind of thermally protective materials and preparation method thereof of aeroge Composite aramid fiber non-woven cloth |
| CN110150776A (en) * | 2019-05-20 | 2019-08-23 | 义乌市迪源服饰有限公司 | A kind of water-fastness massaging vest processing method and its vest structure |
| CN110846891A (en) * | 2019-11-26 | 2020-02-28 | 鑫创新材料科技(徐州)有限公司 | Manufacturing method and application of aerogel composite fiber |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1807750A (en) * | 2006-01-13 | 2006-07-26 | 浙江理工大学 | Method for in-situ generating inorganic nanoparticles in textile |
| CN102390926A (en) * | 2011-07-28 | 2012-03-28 | 东华大学 | Method for preparing glass fibre with structural colors |
| CN102587123A (en) * | 2011-12-31 | 2012-07-18 | 潘雪峰 | Production method for nanometer SiO2 additive waterproof antistatic cloth |
| CN103352363A (en) * | 2013-07-15 | 2013-10-16 | 陕西盟创纳米新型材料股份有限公司 | Manufacturing method of compound fabric, compound fabric and shoes with compound fabric |
| CN103397516A (en) * | 2013-07-15 | 2013-11-20 | 陕西盟创纳米新型材料股份有限公司 | Silicon dioxide aerogel compound fabric, preparation method and military tent cloth |
| CN103496706A (en) * | 2013-09-24 | 2014-01-08 | 北京艾若格科技发展有限公司 | Preparation method of aerogel composite material |
-
2014
- 2014-09-15 CN CN201410469361.0A patent/CN104233787A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1807750A (en) * | 2006-01-13 | 2006-07-26 | 浙江理工大学 | Method for in-situ generating inorganic nanoparticles in textile |
| CN102390926A (en) * | 2011-07-28 | 2012-03-28 | 东华大学 | Method for preparing glass fibre with structural colors |
| CN102587123A (en) * | 2011-12-31 | 2012-07-18 | 潘雪峰 | Production method for nanometer SiO2 additive waterproof antistatic cloth |
| CN103352363A (en) * | 2013-07-15 | 2013-10-16 | 陕西盟创纳米新型材料股份有限公司 | Manufacturing method of compound fabric, compound fabric and shoes with compound fabric |
| CN103397516A (en) * | 2013-07-15 | 2013-11-20 | 陕西盟创纳米新型材料股份有限公司 | Silicon dioxide aerogel compound fabric, preparation method and military tent cloth |
| CN103496706A (en) * | 2013-09-24 | 2014-01-08 | 北京艾若格科技发展有限公司 | Preparation method of aerogel composite material |
Non-Patent Citations (2)
| Title |
|---|
| 董仁威: "《新世纪青年百科全书》", 30 April 2007, 四川辞书出版社 * |
| 赵丽 等: "单分散二氧化硅球形颗粒的制备与形成机理", 《化学学报》 * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105369600A (en) * | 2015-12-24 | 2016-03-02 | 西南大学 | Preparation method of cotton fabric with electrical conductivity, electromagnetic shielding and flame-retardant functions |
| CN107287979A (en) * | 2016-03-30 | 2017-10-24 | 新材料与产业技术北京研究院 | A kind of nano silicon compound pulp and preparation method thereof and page |
| CN107287979B (en) * | 2016-03-30 | 2019-10-25 | 新材料与产业技术北京研究院 | A kind of nano silica compound pulp and preparation method thereof and page |
| CN106436285A (en) * | 2016-07-28 | 2017-02-22 | 东华大学 | Preparation and application of intumescent flame retardant system doped silica sol |
| CN108823968A (en) * | 2018-05-28 | 2018-11-16 | 江苏阳光股份有限公司 | A kind of preparation method of flame resistant wool fabric |
| CN109457485A (en) * | 2018-10-11 | 2019-03-12 | 浙江鹏辰新材料有限公司 | A kind of thermally protective materials and preparation method thereof of aeroge Composite aramid fiber non-woven cloth |
| CN109457485B (en) * | 2018-10-11 | 2021-03-23 | 浙江鹏辰造纸研究所有限公司 | Thermal protection material of aerogel composite aramid fiber non-woven fabric and preparation method thereof |
| CN110150776A (en) * | 2019-05-20 | 2019-08-23 | 义乌市迪源服饰有限公司 | A kind of water-fastness massaging vest processing method and its vest structure |
| CN110846891A (en) * | 2019-11-26 | 2020-02-28 | 鑫创新材料科技(徐州)有限公司 | Manufacturing method and application of aerogel composite fiber |
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Application publication date: 20141224 |