CN109354028A - A method of mixing silicon source copolymerization prepares flexible aeroge compound insulating material - Google Patents

A method of mixing silicon source copolymerization prepares flexible aeroge compound insulating material Download PDF

Info

Publication number
CN109354028A
CN109354028A CN201811344883.2A CN201811344883A CN109354028A CN 109354028 A CN109354028 A CN 109354028A CN 201811344883 A CN201811344883 A CN 201811344883A CN 109354028 A CN109354028 A CN 109354028A
Authority
CN
China
Prior art keywords
silicon source
insulating material
compound insulating
acid
aeroge compound
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201811344883.2A
Other languages
Chinese (zh)
Inventor
纪冠丞
张磊
李季
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Jiangxi Acer Baixin Materials Ltd By Share Ltd
Original Assignee
Jiangxi Acer Baixin Materials Ltd By Share Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Jiangxi Acer Baixin Materials Ltd By Share Ltd filed Critical Jiangxi Acer Baixin Materials Ltd By Share Ltd
Priority to CN201811344883.2A priority Critical patent/CN109354028A/en
Publication of CN109354028A publication Critical patent/CN109354028A/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/113Silicon oxides; Hydrates thereof
    • C01B33/12Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/14Colloidal silica, e.g. dispersions, gels, sols
    • C01B33/157After-treatment of gels
    • C01B33/158Purification; Drying; Dehydrating
    • C01B33/1585Dehydration into aerogels

Abstract

A method of mixing silicon source copolymerization prepares flexible aeroge compound insulating material, it is related to the preparation method of aeroge compound insulating material.The preparation method that it will solve existing aerosil is cumbersome, the period is long, solvent displacement causes the technical problem more than waste liquid amount.This method: one, with positive esters of silicon acis and silicon source containing hydrophobic grouping silica solution is prepared;Two, after silica solution adjusts pH value, chemical seasoning controlling agent, microwave drying is added;Three, it is replaced with alcohols solvent;Four, it washs;Five, dry, obtain flexible aeroge compound insulating material.The material is flexible and 0~60 ° of energy is bent, no picking.It reaches 140~143 ° with hydrophobicity, contact angle, is 0.035~0.036W/ (m × k) in average 300 DEG C of its thermal coefficients, is 0.065~0.066W/ (m × k) in average 500 DEG C of its thermal coefficients.It can be used for field of thermal insulation.

Description

A method of mixing silicon source copolymerization prepares flexible aeroge compound insulating material
Technical field
The present invention relates to the preparation methods of aeroge compound insulating material, belong to heat insulating material technical field.
Background technique
Aeroge, English name are " aerogel ", mean " gel of flight ", are a kind of with nano-porous structure New material shows superior performance in various fields, referred to as changes the magical material in the world, be with huge applications valence The dual-use technology of value.Aeroge mainly has aerosil, alumina aerogels, zirconium oxide gas because of ingredient difference Gel and carbon aerogels etc..Wherein aerosil is because having a nanoporous network structure, and porosity is up to 80%~ 99.8% and hole typical sizes be 1~100nm, its room temperature thermal coefficient can have excellent down to 0.013w/ (mk) Heat-insulating property in aerospace, petrochemical industry, electric power metallurgy, ship vehicle, precision instrument, refrigerator freezer, clothes tent, is built Having broad application prospects for the fields such as energy conservation is built, is traditional insulation materials revolutionary character substitute products.
The preparation method of existing aerosil is usually with waterglass, silane etc. for silicon source, and acidity, which is added, to be had After solvent is reacted, silica solution is prepared, using gel, aging, drying process, obtains aerosil material Material.
Application No. is 201410270352.9 Chinese patents to disclose a kind of silica aerogel material and its preparation Method, this method using waterglass as silicon source, by add not chloride ion-containing and fluorine ion containing sour organic solvent, generate sodium from The precipitating of son, potassium ion and other ionizable metal salts removes precipitating using the mode of filter, acquisition high-purity silicasol, after pass through Sol-gel, aging, acidification, modification, drying process, obtain silica aerogel material, and this method needs aging and modification Etc. complex processes, it is cumbersome, and modifying agent is expensive, causes the cost of entire product excessively high.
Application No. is 201510347057.3 Chinese patents to disclose a kind of flexible aerosil of low cost Preparation method, this method makees silicon source with three kinds of siloxanes with alkyl, waterglass, hydroxy silicon oil raw material mixing, with organic solvent For dispersing agent, bronsted lowry acids and bases bronsted lowry is prepared through supercritical fluid drying technique with excellent respectively as hydrolysis, polycondensation catalyst Good bulk silicon dioxide aeroge flexible.Resulting aerosil sample rate is low, and elasticity is good, and performance is stablized, and dredges It is aqueous good.This method is dried using supercritical process, and equipment investment is prohibitively expensive.
Application No. is the Chinese patents of CN201710740613.2 to disclose a kind of flexible aerosil base phase change The preparation method of composite material, this method introduce trimethylmethoxysilane as a kind of new presoma, by adjusting different silicon The ratio of alkane presoma and solvent prepares flexible aerosil, suitable phase transformation core material is then selected, using Vaccum Permeating Stain method obtains aerosil base phase change composite material.The present invention has the advantages that by the way that trimethyl methoxy silicon is added Alkane changes the degree of cross linking inside aeroge, so that aeroge be made to have flexibility;Trimethylmethoxysilane, which is added, makes aeroge Porosity increases, and pore size is adjustable;Prepared flexible silica aerogel material, can be compound due to its porosity Phase transformation core material prepares phase change composite material;Prepared phase change composite material can effectively prevent leakage problem, and have machine Tool performance is good.The solvent that the solvent replacement process of this method needs is more, and wash time is long, a large amount of waste liquid can be generated, at the later period Energy consumption is high for reason.
Summary of the invention
That the present invention is to solve the preparation methods of existing aerosil is cumbersome, the period is long, solvent displacement The technical problem more than waste liquid amount is caused, and a kind of side of the flexible aeroge compound insulating material of mixing silicon source copolymerization preparation is provided Method.
The method that mixing silicon source copolymerization of the invention prepares flexible aeroge compound insulating material, sequentially includes the following steps:
One, be 1:(1~40 by the molar ratio of positive esters of silicon acis and the silicon source containing hydrophobic grouping), by positive esters of silicon acis with contain The silicon source of hydrophobic grouping is uniformly mixed, and obtains mixing silicon source;Organic acid, surfactant and alcohols is added into mixing silicon source again Solvent, wherein it is 1:(10 that the amount of positive esters of silicon acis and the molar ratio of organic acid, which is added,-3~10-2), total silicon source and surfactant Mass ratio is 1:(0.005~0.08), the molar ratio of positive esters of silicon acis and alcohols solvent is 1:(8~30);Under agitation plus Heat reacts, and obtains silica solution;
Two, the pH for the silica solution that step 1 obtains is adjusted to 6.5~11.5 with alkali, chemical seasoning control is then added The molar ratio of agent, positive esters of silicon acis and chemical seasoning controlling agent is 1:(0.1~0.8), after mixing, it is dry to be directly introduced to microwave Solidify perhaps to be impregnated into reinforcing material to place into microwave drying oven in dry case and solidifies to obtain gel or plural gel material Material;
Three, alcohols solvent is added into the gel or composite gel material that step 2 obtains, alcohols solvent is methanol, second The one of which of alcohol, the tert-butyl alcohol, isopropanol, ethylene glycol, glycerine or tert-pentyl alcohol carries out intermittent-heating ultrasonic treatment;
Four, the gel or composite gel material that handle through step 3 are added in organic solvent, at 30~85 DEG C Under the conditions of wash 6~24 hours, wash 2~8 times, complete displacement;
Five, the gel or composite gel material that handle through step 4 are dried, obtain the compound guarantor of flexible aeroge Adiabator.
The present invention uses positive esters of silicon acis and the silicon source that contains hydrophobic grouping as mixing silicon source, the aeroge obtained after copolymerization It can make to be locked in the hydrone inside gel originally so the wet gel of preparation has from hydrophobic function containing hydrophobic grouping It is extruded because of the hydrophobic function of hydrophobic grouping, so not needing to carry out additional aging and modification procedure, greatly reduces Cost, and it is added without modifying agent, while toxic chloride ion and fluorine ion will not be introduced, both environmental protection will not corrode equipment Pipeline.
For the present invention due to the mixing silicon source of selection, the aerogel composite of preparation has certain flexibility, and has certain Elasticity can carry out the bending of 0~60 ° of angle, and the phenomenon that do not lose powder, and it is raw in industry that this performance is conducive to the material It produces and transportational process easily winds unreel in the middle, improve transport and application portability.
Flexible aeroge compound insulating material of the invention is 0.035~0.036W/ in average 300 DEG C of its thermal coefficients (m × k) is 0.065~0.066W/ (m × k) in average 500 DEG C of its thermal coefficients.There is hydrophobicity simultaneously, contact angle reaches To 140~143 °.
Method of the invention carries out solvent displacement washing using single organic solvent, reduces energy consumption, also saves equipment The investment of expense;The production cycle is shorter simultaneously, and whole preparation process was completed at two days or so, compared with the prior art, preparation effect Rate greatly improves;
Method stability of the invention is high, simple to operate simultaneously, cost is relatively low, can be mass produced, and realizes work Industryization preparation.
Flexible aeroge compound insulating material of the invention can be used for field of thermal insulation.
Detailed description of the invention
Fig. 1 is the photo of flexible aeroge compound insulating material prepared by embodiment 1;
The compression test photo of flexible aeroge compound insulating material prepared by Fig. 2 embodiment 1;
Fig. 3 is the photo of flexible aeroge compound insulating material prepared by embodiment 2;
Specific embodiment
Specific embodiment 1: the mixing silicon source copolymerization of present embodiment prepares the side of flexible aeroge compound insulating material Method sequentially includes the following steps:
One, be 1:(1~40 by the molar ratio of positive esters of silicon acis and the silicon source containing hydrophobic grouping), by positive esters of silicon acis with contain The silicon source of hydrophobic grouping is uniformly mixed, and obtains mixing silicon source;Organic acid, surfactant and alcohols is added into mixing silicon source again Solvent, wherein it is 1:(10 that the amount of positive esters of silicon acis and the molar ratio of organic acid, which is added,-3~10-2), total silicon source amount of addition and surface The mass ratio of activating agent be 1:(0.005~0.08), be added positive esters of silicon acis amount and alcohols solvent molar ratio be 1:(8~ 30);Heating reacts under agitation, obtains silica solution;
Two, the pH for the silica solution that step 1 obtains is adjusted to 6.5~11.5 with alkali, chemical seasoning control is then added Agent, the molar ratio of amount and chemical seasoning controlling agent that positive esters of silicon acis is added are 1:(0.1~0.8), after mixing, it is directly placed into Solidify perhaps to be impregnated into reinforcing material to place into microwave drying oven into microwave drying oven and solidifies to obtain gel or multiple Close gel rubber material;
Three, alcohols solvent is added into the gel or composite gel material that step 2 obtains, carries out intermittent-heating ultrasound Processing;
Four, the gel or composite gel material that handle through step 3 are added in organic solvent, at 30~85 DEG C Under the conditions of wash 6~24 hours, wash 2~8 times, complete displacement;
Five, the gel or composite gel material that handle through step 4 are dried, obtain the compound guarantor of flexible aeroge Adiabator.
Specific embodiment 2: the present embodiment is different from the first embodiment in that positive silicic acid described in step 1 Ester is methyl orthosilicate, ethyl orthosilicate, positive isopropyl silicate or butyl silicate;It is other same as the specific embodiment one.
Specific embodiment 3: the present embodiment is different from the first and the second embodiment in that described in step 1 contain The silicon source for having hydrophobic grouping is methyltrimethoxysilane, dimethyldimethoxysil,ne, trimethylmethoxysilane, methyl three Ethoxysilane, vinyl trichlorosilane, positive silicic acid propyl ester, trimethylethoxysilane, hexamethyldisilazane, hexamethyl two A kind of or in which several combination in siloxanes;It is other the same as one or two specific embodiments.
Specific embodiment 4: unlike one of present embodiment and specific embodiment one to three described in step 1 Organic acid be thionothiolic acid (RCOSH), sulfinic acid (RSOOH), sulfonic acid (R-SO3) or carboxylic acid (R-COOH) H;Other and specific reality It is identical to apply one of mode one to three.
Specific embodiment 5: present embodiment carboxylic acid (R-COOH) described unlike specific embodiment four is Formic acid, acetic acid, benzoic acid, citric acid, n-butyric acie or oxalic acid;It is other identical as one of specific embodiment four.
Specific embodiment 6: unlike one of present embodiment and specific embodiment one to five described in step 1 Surfactant be cetyl trimethylammonium bromide, hexadecyltrimethylammonium chloride, octadecyltrimethylammonium chloride Or myristyl-lutidines ammonium bromide;It is other identical as one of specific embodiment one to five.
Specific embodiment 7: unlike one of present embodiment and specific embodiment one to six described in step 1 Alcohols solvent be methanol, ethyl alcohol, the tert-butyl alcohol, isopropanol, ethylene glycol, glycerine or tert-pentyl alcohol;Other and specific embodiment One of one to six is identical.
Specific embodiment 8: described in step 1 unlike one of present embodiment and specific embodiment one to seven Heating, is heated to 50~80 DEG C, the reaction time is 2~3 hours;It is other identical as one of specific embodiment one to seven.
Specific embodiment 9: unlike one of present embodiment and specific embodiment one to eight described in step 2 Chemical seasoning controlling agent be formamide, acetamide, n,N-Dimethylformamide (DMF), n,N-dimethylacetamide (DMA), Glycerine, ethylene glycol or polyethylene glycol;It is other identical as one of specific embodiment one to eight.
Specific embodiment 10: unlike one of present embodiment and specific embodiment one to nine described in step 2 Microwave drying oven power be 200W~650W, curing time be 15~30 minutes;Other and specific embodiment one to nine One of it is identical.
Specific embodiment 11: institute in step 3 unlike one of present embodiment and specific embodiment one to ten The alcohols solvent stated is methanol, ethyl alcohol, the tert-butyl alcohol, isopropanol, ethylene glycol, glycerine or tert-pentyl alcohol;Other and specific embodiment party One of formula one to ten is identical.
Specific embodiment 12: present embodiment from unlike specific embodiment one to one of 11 in step 3 The intermittent-heating ultrasonic treatment refers to that under conditions of temperature is 20~40 DEG C, every ultrasonic treatment is stood after 20~30 minutes 10~15 minutes;It is other identical as specific embodiment one to one of 11.
Wherein specific embodiment 13: present embodiment and step unlike specific embodiment one to one of 12 In five, drying mode is dry gradient increased temperature, freeze-drying or microwave drying;Other and specific embodiment one to one of 12 It is identical.
Specific embodiment 14: present embodiment and the microwave unlike specific embodiment one to one of 13 Dry to refer to microwave negative pressure drying, vacuum degree is -0.01~-0.05MPa, and the power of microwave is 10KW~60KW;;Other and tool Body embodiment one to one of 13 is identical.
Specific embodiment 15: present embodiment from unlike specific embodiment one to one of 14 in step 4 The organic solvent is methanol, ethyl alcohol, the tert-butyl alcohol, isopropanol, ethylene glycol, glycerine or tert-pentyl alcohol;Other and specific implementation Mode one to one of 14 is identical.
Beneficial effects of the present invention are verified with the following examples:
Embodiment 1: the method that the mixing silicon source copolymerization of the present embodiment prepares flexible aeroge compound insulating material, by following Step carries out:
One, 160.3g butyl silicate is uniformly mixed to the round bottom for being added to 2L with 74.1g dimethyl diethoxysilane In four-necked bottle, mixing silicon source is obtained;The 1482.4g tert-butyl alcohol is added into mixing silicon source again, 2.5 milliliters of concentration are added while stirring For the acetic acid and 1.8g cetyl trimethylammonium bromide of 0.2mol/L, it is heated to 55 DEG C of reaction 2h under agitation, obtains Silica solution;The silica solution pH value that step 1 obtains is 1.6;
Two, the pH of the silica solution obtained with the ammonium hydroxide alkali step 1 of 1mol/L is adjusted to 9.5, and the N, N- of 8.7g is then added Dimethyl acetamide (DMA) is directly introduced in microwave drying oven after mixing, solid in the condition that microwave power is 300W Change 10 minutes, obtains wet gel;
Three, the tert-butyl alcohol is added into the wet gel that step 2 obtains, carries out intermittent-heating ultrasonic treatment, wherein intermittent-heating Ultrasonic treatment refers to that every ultrasonic treatment after twenty minutes, stands 10 minutes, coprocessing 3h under conditions of temperature is 30 DEG C;
Four, the wet gel handled through step 3 is added in the tert-butyl alcohol, washs 8 hours under conditions of 80 DEG C, washes altogether It washs 4 times, completes displacement;
Five, the gel handled through step 4 is put into vacuum oven, the heat preservation drying 3 under conditions of temperature is 60 DEG C Hour, it then heats to 80 DEG C of heat preservations and dries 3 hours, then be warming up to 90 DEG C of heat preservations and dry 3 hours, be finally warming up to 100 DEG C of guarantors Temperature drying 3 hours, obtains flexible aeroge compound insulating material.
The photo for the flexible aeroge compound insulating material that the present embodiment obtains is as shown in Figure 1, by manufactured in the present embodiment After flexible aeroge compound insulating material is torn, also without the phenomenon that losing powder.
The compression test photo of the flexible aeroge compound insulating material that the present embodiment obtains is as shown in Fig. 2, can be with from Fig. 2 Find out, which has certain elasticity, after being compressed into can fast its original state of quick-recovery, recovery rate 100%.The material can also It is bent, allows to arbitrary change shape.
The flexible aeroge compound insulating material that the present embodiment obtains has hydrophobic performance, and contact angle reaches 144 °, rolls 7 ° of angle can improve service life so that the thermal insulation material has hydrophobic humidity resistance.
The flexible aeroge compound insulating material density that the present embodiment obtains is 0.083g/cm-3, this thermal insulation material density It is low, it is very light.
The flexible aeroge compound insulating material that the present embodiment obtains has good heat insulating effect, average 300 DEG C its thermal coefficient is 0.035W/ (m × k), is 0.065W/ (m × k) in average 500 DEG C of its thermal coefficients.
The present embodiment preparation method is easy to operate, the period is short, displacement solvent usage is few.
Embodiment 2: the method that the mixing silicon source copolymerization of the present embodiment prepares flexible aeroge compound insulating material, by following Step carries out:
One, 132.2g positive silicic acid propyl ester and 110.2g methyl tripropoxy silane mixture are even added to the round bottom four of 2L In neck bottle, mixing silicon source is obtained;1201.2g isopropanol is added into mixing silicon source again, 1 milliliter of concentration is added while stirring is The acetic acid and 2.1g octadecyltrimethylammonium chloride of 0.5mol/L is heated to 575 DEG C of reaction 3h under agitation, obtains silicon Colloidal sol;The silica solution pH value that step 1 obtains is 1.9;
Two, the pH for the silica solution that step 1 obtains is adjusted to 8.5 with the ammonium hydroxide of 3mol/L, the N, N- of 7.3g is then added Dimethylformamide is poured into the container for being pre-placed organic fiber cloth after mixing, then places into container In microwave drying oven, solidifies 15 minutes in the condition that microwave power is 200W, obtain composite gel material;
Three, isopropanol is added into the composite gel material that step 2 obtains, carries out intermittent-heating ultrasonic treatment, among it Heating ultrasonic treatment of having a rest refers to that every ultrasonic treatment after twenty minutes, stands 10 minutes, coprocessing 3h under conditions of temperature is 35 DEG C;
Four, the composite gel material handled through step 3 is added in isopropanol, it is small that 10 is washed under conditions of 65 DEG C When, it washs 2 times altogether, completes displacement;
Five, the gel composite gel material handled through step 4 is put into vacuum oven, the item for being 50 DEG C in temperature Heat preservation drying 3 hours under part, then heat to 70 DEG C of heat preservations and dry 3 hours, then are warming up to 100 DEG C of heat preservations drying 3 hours, finally It is warming up to 120 DEG C of heat preservations to dry 3 hours, obtains flexible aeroge compound insulating material.
The photo for the flexible aeroge compound insulating material that the present embodiment obtains is as shown in figure 3, from figure 3, it can be seen that originally After the flexible aeroge compound insulating material cutting of embodiment preparation, the phenomenon that picking, while there is certain elasticity, energy Enough it is bent.
The flexible aeroge compound insulating material that the present embodiment obtains has good heat insulating effect, average 300 DEG C its thermal coefficient is 0.036W/ (m × k), is 0.066W/ (m × k) in average 500 DEG C of its thermal coefficients, and service life Up to 20 years or more, heat-resisting and insulation effect will not change.There is hydrophobicity simultaneously, contact angle reaches 143 °.It can The water absorption rate of the shortcomings that overcoming Conventional insulation, such as rock wool, rock wool is big, and moisture is easy to be accumulated in rock wool board, meeting for a long time Increase heat preservation layer weight, insulating layer is caused to fall off, repair rate is high, and service life is low;With flexible aeroge manufactured in the present embodiment Compound insulating material is good update material.
The flexible aeroge compound insulating material that the present embodiment obtains has extraordinary corrosion resistance, and itself will not be rotten Carbon steel and stainless steel are lost, it is safe and reliable;This aeroge compound insulating material quality is light, has flexibility, is easy cutting, sewing To adapt to various pipelines of different shapes, insulation of equipment.
The present embodiment preparation method is easy to operate, the period is short, displacement solvent usage is few.

Claims (10)

1. a kind of method that the copolymerization of mixing silicon source prepares flexible aeroge compound insulating material, it is characterised in that this method is by following Step carries out:
One, be 1:(1~40 by the molar ratio of positive esters of silicon acis and the silicon source containing hydrophobic grouping), by positive esters of silicon acis with contain it is hydrophobic The silicon source of group is uniformly mixed, and obtains mixing silicon source;It is molten that organic acid, surfactant and alcohols is added into mixing silicon source again Agent, wherein it is 1:(10 that the amount of positive esters of silicon acis and the molar ratio of organic acid, which is added,-3~10-2), total silicon source amount of addition and surface are living Property agent mass ratio be 1:(0.005~0.08), be added positive esters of silicon acis amount and alcohols solvent molar ratio be 1:(8~30); Heating reacts under agitation, obtains silica solution;
Two, the pH for the silica solution that step 1 obtains is adjusted to 6.5~11.5 with alkali, chemical seasoning controlling agent is then added, adds The molar ratio of the amount and chemical seasoning controlling agent that enter positive esters of silicon acis is 1:(0.1~0.8), after mixing, it is directly introduced to micro- Solidify perhaps to be impregnated into reinforcing material to place into microwave drying oven in wave drying box and solidifies to obtain gel or compound solidifying Glue material;
Three, alcohols solvent is added into the gel or composite gel material that step 2 obtains, carries out intermittent-heating ultrasonic treatment;
Four, the gel or composite gel material that handle through step 3 are added in organic solvent, in 30~85 DEG C of condition Lower washing 6~24 hours, is washed 2~8 times, completes displacement;
Five, the gel or composite gel material that handle through step 4 are dried, obtain flexible aeroge complex heat-preservation material Material.
2. the method that a kind of mixing silicon source copolymerization according to claim 1 prepares flexible aeroge compound insulating material, It is characterized in that positive esters of silicon acis described in step 1 is methyl orthosilicate, ethyl orthosilicate, positive isopropyl silicate or positive silicic acid fourth Ester.
3. the method that a kind of mixing silicon source copolymerization according to claim 1 or 2 prepares flexible aeroge compound insulating material, It is characterized in that the silicon source described in step 1 containing hydrophobic grouping is methyltrimethoxysilane, dimethylformamide dimethyl oxygroup silicon Alkane, trimethylmethoxysilane, methyltriethoxysilane, vinyl trichlorosilane, positive silicic acid propyl ester, front three base oxethyl silicon Alkane, hexamethyldisilazane, a kind of or in which several combination in hexamethyldisiloxane.
4. the method that a kind of mixing silicon source copolymerization according to claim 1 or 2 prepares flexible aeroge compound insulating material, It is characterized in that organic acid described in step 1 is thionothiolic acid, sulfinic acid, sulfonic acid or carboxylic acid.
5. the method that a kind of mixing silicon source copolymerization according to claim 4 prepares flexible aeroge compound insulating material, It is characterized in that the carboxylic acid is formic acid, acetic acid, benzoic acid, citric acid, n-butyric acie or oxalic acid.
6. the method that a kind of mixing silicon source copolymerization according to claim 1 or 2 prepares flexible aeroge compound insulating material, It is characterized in that surfactant described in step 1 is cetyl trimethylammonium bromide, cetyl trimethyl chlorination Ammonium, octadecyltrimethylammonium chloride or myristyl-lutidines ammonium bromide.
7. the method that a kind of mixing silicon source copolymerization according to claim 1 or 2 prepares flexible aeroge compound insulating material, It is characterized in that alcohols solvent described in step 1 is methanol, ethyl alcohol, the tert-butyl alcohol, isopropanol, ethylene glycol, glycerine or uncle penta Alcohol.
8. the method that a kind of mixing silicon source copolymerization according to claim 1 or 2 prepares flexible aeroge compound insulating material, It is characterized in that heating described in step 1, is heated to 50~80 DEG C, the reaction time is 2~3 hours.
9. the method that a kind of mixing silicon source copolymerization according to claim 1 or 2 prepares flexible aeroge compound insulating material, It is characterized in that chemical seasoning controlling agent described in step 2 is formamide, acetamide, n,N-Dimethylformamide, N, N- bis- Methylacetamide, glycerine, ethylene glycol or polyethylene glycol.
10. the side that a kind of mixing silicon source copolymerization according to claim 1 or 2 prepares flexible aeroge compound insulating material Method, it is characterised in that the power of microwave drying oven described in step 2 is 200W~650W, and curing time is 15~30 minutes.
CN201811344883.2A 2018-11-13 2018-11-13 A method of mixing silicon source copolymerization prepares flexible aeroge compound insulating material Pending CN109354028A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201811344883.2A CN109354028A (en) 2018-11-13 2018-11-13 A method of mixing silicon source copolymerization prepares flexible aeroge compound insulating material

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201811344883.2A CN109354028A (en) 2018-11-13 2018-11-13 A method of mixing silicon source copolymerization prepares flexible aeroge compound insulating material

Publications (1)

Publication Number Publication Date
CN109354028A true CN109354028A (en) 2019-02-19

Family

ID=65344876

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201811344883.2A Pending CN109354028A (en) 2018-11-13 2018-11-13 A method of mixing silicon source copolymerization prepares flexible aeroge compound insulating material

Country Status (1)

Country Link
CN (1) CN109354028A (en)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111154036A (en) * 2020-01-20 2020-05-15 南京工业大学 Preparation method of ethylene-silane copolymerized composite aerogel
CN114534693A (en) * 2022-02-18 2022-05-27 南京工业大学 Preparation method of transparent hydrophobic spherical silica aerogel adsorbent
CN114560467A (en) * 2022-04-02 2022-05-31 西南大学 Flexible silicon dioxide aerogel and preparation method thereof
CN115043408A (en) * 2022-07-04 2022-09-13 巩义市泛锐熠辉复合材料有限公司 Flexible silicon dioxide aerogel, aerogel felt and preparation method thereof
CN114560467B (en) * 2022-04-02 2024-04-30 西南大学 Flexible silicon dioxide aerogel and preparation method thereof

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102010179A (en) * 2010-12-20 2011-04-13 中钢集团洛阳耐火材料研究院有限公司 Method for preparing fiber-containing silicon dioxide aerogel composite thermal insulation material
CN106745004A (en) * 2017-01-22 2017-05-31 伊科纳诺(北京)科技发展有限公司 A kind of quick method for preparing hydrophobic silica aerogel of low cost
CN108314411A (en) * 2018-01-03 2018-07-24 深圳中凝科技有限公司 The method that silicon dioxide silica aerogel composite material is prepared without alcohol technique using no chlorine
CN108383129A (en) * 2018-01-30 2018-08-10 南京工业大学 A kind of preparation method of flexibility Hydrophobic silica aeroge
CN108689680A (en) * 2018-05-30 2018-10-23 巩义市泛锐熠辉复合材料有限公司 A kind of preparation method of effectively insulating heat preservation aerogel blanket

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102010179A (en) * 2010-12-20 2011-04-13 中钢集团洛阳耐火材料研究院有限公司 Method for preparing fiber-containing silicon dioxide aerogel composite thermal insulation material
CN106745004A (en) * 2017-01-22 2017-05-31 伊科纳诺(北京)科技发展有限公司 A kind of quick method for preparing hydrophobic silica aerogel of low cost
CN108314411A (en) * 2018-01-03 2018-07-24 深圳中凝科技有限公司 The method that silicon dioxide silica aerogel composite material is prepared without alcohol technique using no chlorine
CN108383129A (en) * 2018-01-30 2018-08-10 南京工业大学 A kind of preparation method of flexibility Hydrophobic silica aeroge
CN108689680A (en) * 2018-05-30 2018-10-23 巩义市泛锐熠辉复合材料有限公司 A kind of preparation method of effectively insulating heat preservation aerogel blanket

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
孙登科: "TiO2掺杂硅气凝胶的制备及其高温绝热性能研究", 《中国优秀硕士学位论文全文数据库》 *
张明等: "多次疏水改性SiO2气凝胶的制备及其性能表征", 《化学推进剂与高分子材料》 *

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111154036A (en) * 2020-01-20 2020-05-15 南京工业大学 Preparation method of ethylene-silane copolymerized composite aerogel
CN111154036B (en) * 2020-01-20 2021-12-24 南京工业大学 Preparation method of ethylene-silane copolymerized composite aerogel
CN114534693A (en) * 2022-02-18 2022-05-27 南京工业大学 Preparation method of transparent hydrophobic spherical silica aerogel adsorbent
CN114560467A (en) * 2022-04-02 2022-05-31 西南大学 Flexible silicon dioxide aerogel and preparation method thereof
CN114560467B (en) * 2022-04-02 2024-04-30 西南大学 Flexible silicon dioxide aerogel and preparation method thereof
CN115043408A (en) * 2022-07-04 2022-09-13 巩义市泛锐熠辉复合材料有限公司 Flexible silicon dioxide aerogel, aerogel felt and preparation method thereof
CN115043408B (en) * 2022-07-04 2023-11-10 巩义市泛锐熠辉复合材料有限公司 Flexible silica aerogel, aerogel felt and preparation method thereof

Similar Documents

Publication Publication Date Title
CN106629750B (en) A kind of atmospheric preparation method of transparent silicon dioxide block aeroge
CN108314411A (en) The method that silicon dioxide silica aerogel composite material is prepared without alcohol technique using no chlorine
CN102642842B (en) Method for preparing silicon dioxide aerogel by using acidic silica sol
CN109354028A (en) A method of mixing silicon source copolymerization prepares flexible aeroge compound insulating material
CN102765725B (en) Method for preparing hydrophobic silica aerogel with low cost
WO2017152587A1 (en) Method for fabricating composite sio2 aerogel blanket
CN101671029B (en) Method for preparing SiO2 aerogel in normal pressure drying condition
CN104071797B (en) A kind of method preparing low density bigger serface aerosil coating with water glass atmospheric pressure at room
CN108658574A (en) A kind of anti-shedding aeroge complex heat-preservation felt
CN101372337A (en) Method for preparing transparent silicon dioxide aerogel by co-precursor normal atmosphere drying
CN106007652A (en) Preparation method of high-temperature-resistant and hydrophobic SiO2 aerogel felt
CN107263948B (en) A kind of fire-proof thermal-insulation decoration and preparation method thereof
CN109824339A (en) A kind of rock wool/aerogel composite and its preparation process with heat-proof quality
CN106745002B (en) A kind of method that co-precursor method constant pressure and dry prepares block aerosil
CN106120439A (en) A kind of aeroge composite fibre paper and preparation method thereof
CN102992333B (en) Low-cost method for preparing aerosil
CN105819823B (en) A kind of preparation method of aerosil and glass fibre felt composite material
CN104495859A (en) Preparation method of silicon dioxide aerogel
CN104891934A (en) Aerogel thermal insulation material and preparation method thereof and refrigerator
CN104497688A (en) Aerogel thermal insulation coating and preparation method thereof
CN104761235A (en) Preparation method of low-temperature-resistant glass-fiber-reinforced SiO2 aerogel composite material
CN108996985A (en) A kind of preparation method of aerogel blanket heat-insulating heat-preserving material
CN108358212A (en) The preparation method and silica aerogel particles of silica aerogel particles
CN110615663A (en) Solid wood fiber/SiO2Aerogel composite thermal insulation material and preparation method thereof
CN108793173A (en) A method of improved silica aerogel material is prepared using outer circulation mode constant pressure and dry

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
WD01 Invention patent application deemed withdrawn after publication
WD01 Invention patent application deemed withdrawn after publication

Application publication date: 20190219