CN103332696A - Method for manufacturing water glass aerogel product by using freeze-drying method and application of product - Google Patents
Method for manufacturing water glass aerogel product by using freeze-drying method and application of product Download PDFInfo
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Abstract
The invention discloses a method for manufacturing a water glass aerogel product by using a freeze-drying method and an application of the product. The method comprises the following steps of: preparing silica wet gel; modifying the surface; cleaning; performing freeze-drying; and moving from a die; the freeze-drying process includes the specific steps of: freezing a water glass aerogel product until a liquid substance in the product is crystallized, and then heating at a vacuum degree of 10 to 30Pa until all the ice crystals in the frozen product are sublimated, thus accomplishing the drying; and the drying is carried out at twice. An aerogel plate manufactured by the method is lightweight, appears white and light yellow, has no cracks on the surface, is completely hydrophobic, is at the fire rating A and completely noncombustible, and has an extreme effect on sound absorbing and insulating. The product can be prepared into a structure of a large block which is convenient for practical application. The product manufactured by the method has a large specific surface area, high porosity, low density and low heat conductivity coefficient. According to the method, massive industrial production can be carried out, and the cost is reduced. A thermal insulation material prepared from the aerogel product can be widely applied to thermal insulation and sound insulation of a compartment body of a vehicle, thermal insulation of petro-chemical pipelines, thermal insulation of wall bodies of a building, etc.
Description
Technical field
The present invention relates to the heat insulating energy saving material field, specifically is a kind of method and application thereof of making water glass aerogel goods of freeze-drying.
Background technology
Aerogel is to be assembled mutually by colloidal particle or high-polymer molecular to constitute the nanoporous network structure, and is full of a kind of high dispersive solid-state material of gaseous state dispersion medium in hole.The nanostructure of aerogel uniqueness makes it have many characteristics, as lower thermal conductivity, the low velocity of sound, low density and high-specific surface area etc., has the material of excellent heat insulation, sound-proofing properties.SiO
2Aerogel is most typical a kind of nano-porous materials wherein, transmitance with low-down thermal conductivity and good visible light and near infrared light, the solar radiant energy transmitance is higher than 90%, and centering far infrared rays barrier property is good, can effectively intercept winter indoor heat to the loss of outdoor radiant heat transfer, and heat preservation and insulation is better than existing any material again, is northern China cold district desirable transparent heat-insulated lagging material in winter.Yet SiO
2The intensity of aerogel is lower, wear no resistance, whole aerogel material cost height, and existing industrialization product mostly is powder body material, and this brings limitation for application of SiO2 aerogel, is difficult to large-scale promotion application.
Chinese patent CN100386260C discloses the preparation method that a kind of brucite fiber strengthens the aerosil lagging material.This method serves as the preparation raw material with process water glass or silicon sol and natural brucite staple fibre.But to the dispersion of brucite fiber and more loaded down with trivial details to forming solvent exchange and hydrophobic treatment process that gel carries out, limited practical application to a certain extent.
Chinese patent CN101823867A provides a kind of preparation method of silicon dioxide silica aerogel composite material of doped with aramid fibre, this method is used silicon source and alcoholic solvent mixed preparing silicon sol, mix aramid fiber and tensio-active agent again, leave standstill treat its gel after, again through aging and solvent replacing, classification drying under the normal pressure namely gets the silicon dioxide silica aerogel composite material of required doped with aramid fibre.But this method requires that aramid fiber is had good dispersion, also will add tensio-active agent, and need to carry out loaded down with trivial details solvent exchange before the constant pressure and dry.
For fear of the subsiding of its inner skeleton structure, all adopt the method for supercritical drying traditionally in the aerogel preparation process.Though supercutical fluid can effectively be eliminated the fluid of capillary force and avoids the contraction of gel skeleton in the drying process, the expensive and dangerous large-scale production and application that greatly limit aerogel material of supercritical drying as a kind of.Lyophilize can avoid subsiding of aerogel skeleton well, and cost is lower owing to do not have curved liquid surface in its drying process, is a kind of Perfected process that can be used for large-scale production and application.
Summary of the invention
Goal of the invention: the object of the present invention is to provide a kind of method of making water glass aerogel goods with freeze-drying, in the hope of realizing good mechanical property, cost is low, and the present invention also provides the application of these goods on lagging material.
Technical scheme: in order to realize the foregoing invention purpose, the technical solution adopted in the present invention is:
A kind of method of making water glass aerogel goods with freeze-drying comprises the steps: to prepare silica wet gel, surface modification modification, cleaning, lyophilize, depanning; Described lyophilize is for to be refrigerated to fluent meterial crystallization in the goods with water glass wet gel goods, again vacuum tightness 10～30Pa by heating, ice crystal all distils in refrigerated products, finishes drying; Described drying is twice drying.
Concrete steps are:
(1) preparation silica wet gel: the deionized water dilution that adds 4～5 times of amounts of volume under the normal temperature in the service water glass, service water glass is preferably M3.2 level service water glass, salt acid for adjusting pH value to the pH value that adds mass concentration 10% again is 9～10, pour mould into after evenly stirring, place the cotton felt of layer of glass in the mould, be warming up to 60 ℃ and accelerate gel, leave standstill 2h and namely make silica wet gel, cotton felt plays the skeleton supporting role, makes end article can form bulk, en-block construction;
(2) surface modification is modified: pour the mixing solutions of the normal hexane of volume ratio 1:1 and trimethylchlorosilane the mould of step (1) into, flood wet gel, leave standstill 24～36h under room temperature, reclaim waste liquid; Modification theory is: nonpolar normal hexane is replaced out the water in the wet gel hole, and trimethylchlorosilane is modified internal surface of hole, and after surface hydroxyl was replaced by alkyl, gel became hydrophobic gel.
(3) clean: in mould, add dehydrated alcohol, drowning wet gel surface, soaking and washing 24～36h under the normal temperature has cleaned the back and has collected waste liquid, cleans 1～2 time with distilled water again, reclaims waste liquid;
(4) lyophilize: goods in the mould are placed on the freeze drying box median septum frozen cooling fluent meterial crystallization gelation body to the wet gel goods; Open vacuum pump, heat up in the vacuum environment, ice crystal all distils and diffuses to water vessel in freezing body, and drying is finished;
(5) be described water glass aerogel goods after the depanning.
Described drying is twice drying; For the first time dryly heat up for keep 6～10h under vacuum tightness 20～30Pa, freeze that moisture diffusion is to water vessel in the body, the water vessel temperature reduces, and continues heated barrier, and the crystal distillation is finished until distillation; It is dry for dividing plate is warming up to 40～60 ℃ for the second time,, the water vessel temperature is controlled at-50～-70 ℃, keeps vacuum tightness 1～2h of 10～30Pa, finishes redrying.
It is constant and be not 0 to keep freezing the pressure reduction of surface vapour pressure and water vessel surface vapor pressure during described lyophilize.
The temperature head of freezing surface temperature and water vessel surface temperature during described lyophilize is constant.
Described when freezing temperature be lower than the eutectic point of all substances in the mould.
Described when freezing temperature be lower than the eutectic point of all substances in the mould, and be not less than following 5 ℃ of the eutectic point of all substances.
Step (4) is put into freeze drying box with mould and is carried out quick freezing on the dividing plate from level to level specifically, and temperature is lower than the eutectic point (also being lower than the eutectic point of distillation) of all substances in the wet gel when freezing, keeps 1～2h, makes the whole crystallizations of fluent meterial.Carry out drying after freezing, fully dry in order to make, described drying is preferably drying twice.For sublimation drying, under vacuum tightness 20～30Pa, keep 6～10h for the first time.For replenishing the heat of taking away when crystal distils, dividing plate need heat up, and does not make to freeze the lasting reduction of body temperature degree and cause distillation to stop; The distillation moisture diffusion is frozen to the water vessel surface, and the water vessel temperature should be lower than wet gel and freeze the body temperature degree; Dividing plate provides the required heat of distillation to want an amount of, can not be superfluous or not enough, not enoughly can prolong the time of distillation, and surplus can make freezes the body temperature degree and rises and surpass temperature of eutectic point, and crystal is destroyed.It is constant and be not 0 to freeze the pressure reduction of surface vapour pressure and water vessel surface vapor pressure, and lyophilize stopped when pressure reduction was zero, and the temperature head that also need keep freezing surface temperature and water vessel surface temperature is constant.When the temperature of each thermometric layer that temperature probe is surveyed is consistent, illustrate that the ice crystal distillation finishes, the primary drying end can be removed the moisture more than 90%.Be parsing-desiccation for the second time, be used for to remove be adsorbed in the solid matter interstitial void or with the hydrogen bond mode be combined on the polar group in conjunction with water, be specially dividing plate is warming up to 40～60 ℃, improve rapidly and freeze the body temperature degree, the control of water vessel temperature is at-50～-70 ℃, vacuum tightness 1～2h that vacuum tightness remains on 10～30Pa finishes redrying, and redrying finishes to remove 95～100% moisture.
The application of water glass aerogel goods on lagging material that the present invention also provides described method to make.
Beneficial effect: compared with prior art, remarkable advantage of the present invention is: 1) aerogel plate light weight, look Bai Weihuang, the surperficial flawless made of the present invention, hydrophobic fully, fire-protection rating A1 level is not fired fully, and has fabulous sound-absorbing soundproof effect, when adopting the glass cotton block of the pre-hard processing of alumina-coated modification, ultimate compression strength can reach 0.1～0.12MP; When adopting glass cotton felt structure, can make the flexible heat-insulating felt; 2) goods of the present invention can be made into lumpy structure, can cut arbitrarily, are convenient to practical application; 3) gained aerogel of the present invention (when not containing glass fibre cotton) density is 0.12～0.13g/cm
3, aerogel warming plate (felt) density is at 0.3～0.5g/cm
3, porosity is 91～94%, and thermal conductivity is 0.015-0.020W/ (mK), and the specific surface area when making the powdery aerogel is 550～800m
2/ g.And generally have aerogel warming plate (felt) density now at 0.6～0.8g/cm
3, porosity is 85～90%, and thermal conductivity is 0.025-0.050W/ (mK), and the specific surface area when making the powdery aerogel is 200～400m
2/ g illustrates that the aerogel specific surface area that the present invention makes is bigger, and porosity is higher, and density is lower; The heat insulating products thermal conductivity is lower; 4) the present invention can mass industrialized production; 5) comprehensive cost of the present invention is lower, is embodied in: raw materials cost low (adopt cheap service water glass, cost is far below silicon sources such as positive tetraethyl orthosilicate, poly silicon, silicon sol); Time cost low (normal temperature and pressure prepares the general needs 7～14d of aerogel, and the present invention only needs 2.5～5d, prepares aerogel than normal temperature and pressure and shortens the time over half); Equipment cost is low, and (traditional supercritical drying device mainly is made up of air supply system, refrigeration system, flow control system, temperature controlling system, pressure-controlling regulation system, drying installation, tripping device electrical control, support casing etc., the equipment complexity, the cost height, and the present invention only needs freeze drying equipment, and freeze drying equipment is that multilayered structure can once load goods in enormous quantities, loading capacity is saved the factory building of tens times of volumes considerably beyond supercritical drying device); 6) lagging material made of aerogel goods of the present invention can be widely used in vehicle cabinet insulation and sound insulation, oil and chemical pipeline insulation, facility insulation more than-250 ℃, the thermal source below 1000 ℃ is heat insulation, the civil building wall thermal insulating of severe cold area, and industrial goods are heat insulation etc.
Embodiment
The present invention is further described below by specific embodiment; should be pointed out that for the person of ordinary skill of the art, under the prerequisite that does not break away from the principle of the invention; can also make some modification and improvement, these also should be considered as belonging to protection scope of the present invention.
Embodiment 1
The deionized water dilution that adds 4 times of amounts of volume under the normal temperature in the M3.2 level service water glass, salt acid for adjusting pH value to the pH value that adds mass concentration 10% again is 9, pour mould into after evenly stirring, place one deck in the mould and coat reinforcing glass cellucotton felt in advance, be warming up to 60 ℃ and accelerate gel, leave standstill 2h and namely make silica wet gel; Pour the normal hexane of volume ratio 1:1 and the mixing solutions of trimethylchlorosilane into mould, flood wet gel, under room temperature, leave standstill 24h exchange modification; In mould, add dehydrated alcohol, drowning wet gel surface, soaking and washing 24h under the normal temperature has cleaned the back and has collected waste liquid, cleans 1 time with distilled water again, reclaims waste liquid; Goods in the mould are placed on the freeze drying box median septum frozen cooling fluent meterial crystallization gelation body to the wet gel goods; Open vacuum pump, heat up in the vacuum environment, fully dry in order to make, carry out drying twice; For the first time dryly heat up for keep 6h under vacuum tightness 20Pa, freeze that moisture diffusion is to water vessel in the body, the water vessel temperature reduces, and continues heated barrier, and the crystal distillation is finished until distillation, and primary drying finishes to remove 90% moisture; It is dry for dividing plate is warming up to 40 ℃ for the second time,, the water vessel temperature is controlled at-50 ℃, keeps the vacuum tightness 1h of 10Pa, finishes redrying, and redrying finishes to remove 95% moisture.After drying was finished, depanning namely got water glass aerogel goods.These aerogel goods are made warming plate.
The significant parameter of the aerogel goods that present embodiment makes sees the following form.
Embodiment 2
The deionized water dilution that adds 5 times of amounts of volume under the normal temperature in the M3.2 level service water glass, salt acid for adjusting pH value to the pH value that adds mass concentration 10% again is 10, pour mould into after evenly stirring, place one deck in the mould and coat reinforcing glass cellucotton felt in advance, be warming up to 60 ℃ and accelerate gel, leave standstill 2h and namely make silica wet gel; Pour the normal hexane of volume ratio 1:1 and the mixing solutions of trimethylchlorosilane into mould, flood wet gel, under room temperature, leave standstill 36h exchange modification; In mould, add dehydrated alcohol, drowning wet gel surface, soaking and washing 36h under the normal temperature has cleaned the back and has collected waste liquid, cleans 2 times with distilled water again, reclaims waste liquid; Goods in the mould are placed on the freeze drying box median septum frozen cooling fluent meterial crystallization gelation body to the wet gel goods; Open vacuum pump, heat up in the vacuum environment, fully dry in order to make, carry out drying twice; For the first time dryly heat up for keep 10h under vacuum tightness 30Pa, freeze that moisture diffusion is to water vessel in the body, the water vessel temperature reduces, and continues heated barrier, and the crystal distillation is finished until distillation, and primary drying finishes to remove 94% moisture; It is dry for dividing plate is warming up to 60 ℃ for the second time,, the water vessel temperature is controlled at-70 ℃, keeps the vacuum tightness 2h of 30Pa, finishes redrying, and redrying finishes to remove 99.92% moisture.After drying was finished, depanning namely got water glass aerogel goods.These aerogel goods are made warming plate.
The significant parameter of the aerogel goods that present embodiment makes sees the following form.
Embodiment 3
The deionized water dilution that adds 4.5 times of amounts of volume under the normal temperature in the M3.2 level service water glass, salt acid for adjusting pH value to the pH value that adds mass concentration 10% again is 9～10, pour mould into after evenly stirring, place one deck in the mould and coat reinforcing glass cellucotton felt in advance, be warming up to 60 ℃ and accelerate gel, leave standstill 2h and namely make silica wet gel; Pour the normal hexane of volume ratio 1:1 and the mixing solutions of trimethylchlorosilane into mould, flood wet gel, under room temperature, leave standstill 30h exchange modification; In mould, add dehydrated alcohol, drowning wet gel surface, soaking and washing 30h under the normal temperature has cleaned the back and has collected waste liquid, cleans 2 times with distilled water again, reclaims waste liquid; Goods in the mould are placed on the freeze drying box median septum frozen cooling fluent meterial crystallization gelation body to the wet gel goods; Open vacuum pump, heat up in the vacuum environment, fully dry in order to make, carry out drying twice; For the first time dryly heat up for keep 8h under vacuum tightness 25Pa, freeze that moisture diffusion is to water vessel in the body, the water vessel temperature reduces, and continues heated barrier, and the crystal distillation is finished until distillation, and primary drying finishes to remove 91% moisture; It is dry for dividing plate is warming up to 50 ℃ for the second time,, the water vessel temperature is controlled at-60 ℃, keeps the vacuum tightness 2h of 20Pa, finishes redrying, and redrying finishes to remove 97% moisture.After drying was finished, depanning namely got water glass aerogel goods.These aerogel goods are made warming plate.
The significant parameter of the aerogel goods that present embodiment makes sees the following form.
Claims (9)
1. a method of making water glass aerogel goods with freeze-drying is characterized in that: comprise the steps: to prepare silica wet gel, surface modification modification, cleaning, lyophilize, depanning; Described lyophilize is for to be refrigerated to fluent meterial crystallization in the goods with water glass wet gel goods, again vacuum tightness 10～30Pa by heating, ice crystal all distils in refrigerated products, finishes drying; Described drying is twice drying.
2. method of making water glass aerogel goods with freeze-drying as claimed in claim 1, it is characterized in that: concrete steps are:
(1) preparation silica wet gel: the deionized water dilution that adds 4～5 times of amounts of volume under the normal temperature in the service water glass, salt acid for adjusting pH value to the pH value that adds mass concentration 10% again is 9～10, pour mould into after evenly stirring, place the cotton felt of layer of glass in the mould, be warming up to 60 ℃ and accelerate gel, leave standstill 2h and namely make silica wet gel;
(2) surface modification is modified: the solution of the normal hexane of volume ratio 1:1 and trimethylchlorosilane is mixed, pours into the mould of step (1), flood wet gel, leave standstill 24～36h under room temperature, reclaim waste liquid;
(3) clean: in mould, add dehydrated alcohol, drowning wet gel surface, soaking and washing 24～36h under the normal temperature has cleaned the back and has collected waste liquid, cleans 1～2 time with distilled water again, reclaims waste liquid;
(4) lyophilize: goods in the mould are placed on the freeze drying equipment median septum frozen cooling fluent meterial crystallization gelation body to the wet gel goods; Open vacuum pump, heat up in the vacuum environment, ice crystal all distils and diffuses to water vessel in freezing body, and drying is finished;
(5) be described water glass aerogel goods after the depanning.
3. method of making water glass aerogel goods with freeze-drying as claimed in claim 2, it is characterized in that: described drying is twice drying; For the first time dryly heat up for keep 6～10h under vacuum tightness 20～30Pa, freeze that moisture diffusion is to water vessel in the body, the water vessel temperature reduces, and continues heated barrier, and the crystal distillation is finished until distillation; It is dry for dividing plate is warming up to 40～60 ℃ for the second time,, the water vessel temperature is controlled at-50～-70 ℃, keeps vacuum tightness 1～2h of 10～30Pa, finishes redrying.
4. method of making water glass aerogel goods with freeze-drying as claimed in claim 2 is characterized in that: it is constant and be not 0 to keep freezing the pressure reduction of surface vapour pressure and water vessel surface vapor pressure during described lyophilize.
5. method of making water glass aerogel goods with freeze-drying as claimed in claim 2 is characterized in that: the temperature head of freezing surface temperature and water vessel surface temperature during described lyophilize is constant.
6. method of making water glass aerogel goods with freeze-drying as claimed in claim 2 is characterized in that: described when freezing temperature be lower than the eutectic point of all substances in the mould.
7. method of making water glass aerogel goods with freeze-drying as claimed in claim 2 is characterized in that: described when freezing temperature be lower than the eutectic point of all substances in the mould, and be not less than following 5 ℃ of the eutectic point of all substances.
8. method of making water glass aerogel goods with freeze-drying as claimed in claim 2, it is characterized in that: described service water glass is M3.2 level service water glass.
9. the application of water glass aerogel goods on lagging material that make of the described method of claim 1.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104478395A (en) * | 2014-11-14 | 2015-04-01 | 刘吉海 | Composite SiO2 aerogel heat insulation material and preparation method thereof |
| CN105236420A (en) * | 2015-09-06 | 2016-01-13 | 湖南上懿丰新材料科技有限公司 | Method of preparing regular-shaped SiO2 aerogel granules through mechanical cutting |
| CN105667607A (en) * | 2016-01-15 | 2016-06-15 | 郭一新 | Efficient heat preservation layer of automobile carriage |
| CN106185964A (en) * | 2016-07-20 | 2016-12-07 | 福建远翔新材料股份有限公司 | A kind of preparation method of super insulating material silicon dioxide |
| CN106430224A (en) * | 2016-09-30 | 2017-02-22 | 昆山蓝胜建材有限公司 | Microwave drying oven and method for preparing sodium silicate aerogel by utilizing microwave drying method |
| CN106745003A (en) * | 2017-01-20 | 2017-05-31 | 伊科纳诺（北京）科技发展有限公司 | A kind of one-step method silicon dioxide aerogel powder normal pressure fast preparation method |
| CN107057107A (en) * | 2017-04-13 | 2017-08-18 | 昆明理工大学 | It is a kind of to be freeze-dried the method for preparing cellulose aerogels |
| CN107381581A (en) * | 2017-08-28 | 2017-11-24 | 优澎（嘉兴）新材料科技有限公司 | Hydrophobic silicon dioxide aerogel material and preparation method thereof |
| CN108892404A (en) * | 2018-07-10 | 2018-11-27 | 安徽省神洲建材科技有限公司 | A kind of thermal insulation mortar aeroge-basalt composite fibre and preparation method thereof |
| CN111099876A (en) * | 2019-12-20 | 2020-05-05 | 山东工业陶瓷研究设计院有限公司 | Preparation method of low-cost silicon dioxide aerogel composite flexible heat insulation material |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104478395A (en) * | 2014-11-14 | 2015-04-01 | 刘吉海 | Composite SiO2 aerogel heat insulation material and preparation method thereof |
| CN105236420A (en) * | 2015-09-06 | 2016-01-13 | 湖南上懿丰新材料科技有限公司 | Method of preparing regular-shaped SiO2 aerogel granules through mechanical cutting |
| CN105667607A (en) * | 2016-01-15 | 2016-06-15 | 郭一新 | Efficient heat preservation layer of automobile carriage |
| CN106185964A (en) * | 2016-07-20 | 2016-12-07 | 福建远翔新材料股份有限公司 | A kind of preparation method of super insulating material silicon dioxide |
| CN106430224A (en) * | 2016-09-30 | 2017-02-22 | 昆山蓝胜建材有限公司 | Microwave drying oven and method for preparing sodium silicate aerogel by utilizing microwave drying method |
| CN106745003A (en) * | 2017-01-20 | 2017-05-31 | 伊科纳诺（北京）科技发展有限公司 | A kind of one-step method silicon dioxide aerogel powder normal pressure fast preparation method |
| CN107057107A (en) * | 2017-04-13 | 2017-08-18 | 昆明理工大学 | It is a kind of to be freeze-dried the method for preparing cellulose aerogels |
| CN107057107B (en) * | 2017-04-13 | 2020-03-31 | 昆明理工大学 | Method for preparing cellulose aerogel through freeze drying |
| CN107381581A (en) * | 2017-08-28 | 2017-11-24 | 优澎（嘉兴）新材料科技有限公司 | Hydrophobic silicon dioxide aerogel material and preparation method thereof |
| CN108892404A (en) * | 2018-07-10 | 2018-11-27 | 安徽省神洲建材科技有限公司 | A kind of thermal insulation mortar aeroge-basalt composite fibre and preparation method thereof |
| CN111099876A (en) * | 2019-12-20 | 2020-05-05 | 山东工业陶瓷研究设计院有限公司 | Preparation method of low-cost silicon dioxide aerogel composite flexible heat insulation material |
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