CN102836678A

CN102836678A - Preparing method of transparent aerogel

Info

Publication number: CN102836678A
Application number: CN201210308471XA
Authority: CN
Inventors: 翟传伟; 李壮贤
Original assignee: Qingdao Creek New Environmental Materials Co Ltd
Current assignee: Qingdao Creek New Environmental Materials Co Ltd
Priority date: 2012-08-28
Filing date: 2012-08-28
Publication date: 2012-12-26

Abstract

The invention discloses a preparing method of a transparent aerogel. The preparing method of the transparent aerogel is characterized in that composition and content of the transparent aerogel are 5-15 weight parts of a silicon source, 15-25 weight parts of a solvent, , 1-10 weight parts of a surface modifier, and 1-3 weight parts of water. The weight ratios of the transparent aerogel to a treatment agent, a catalyst, and a fibre are respectively in a range of 1-5%o, 1-5%o, and less than 2%. The method of preparing craftsmanship sequentially comprises the steps of mixing, stirring, standing, hydrolyzing of the silicon resource, the solvent, the treatment agent, the surface modifier, the fibre, and the water, adding the catalyst to proceed with polycondensation, putting into a mould to proceed with aging, cleaning, and drying. The preparing method of the transparent aerogel has the advantages that a thermal coefficient of the transparent aerogel is very low, particularities of vacuum glasses are matched with the transparent aerogel to meet the requirement of energy saving, the strength of the transparent aerogel is very high, the ability of bearing ambient pressure is big, the whole strength is greatly improved, and the transparent aerogel is not easily damaged.

Description

The preparation method of transparency aerogel

Technical field

The present invention relates to a kind of preparation method of transparency aerogel, transparency aerogel is mainly used in the sandwich material of transparency aerogel vacuum glass.

Background technology

Can satisfy in the prior art energy-saving design standard can with material be double-deck or three layers of vacuum of the two frames/hollow energy-saving glass of single frame, rely on to support the support outside pressure.In case receive the external force effect, damaged easily, produce gas leakage and cause thermal and insulating performance to decline to a great extent afterwards, can not reach national energy conservation standard.

Summary of the invention

The preparation method that the purpose of this invention is to provide a kind of transparency aerogel; The transparency aerogel of making is used for the sandwich material of transparency aerogel vacuum glass; To solve the easy breakage that prior art hollow energy-saving glass exists, produce the problem that causes thermal and insulating performance to decline to a great extent after the gas leakage.

Technical scheme of the present invention is: a kind of preparation method of transparency aerogel; It is characterized in that, the composition of described transparency aerogel and content be the part by weight of part by weight 1-5 ‰, fiber of parts by weight 1-10, the catalyst of part by weight 1-5 ‰, the surface modifier of parts by weight 15-25, the inorganic agent of parts by weight 5-15, the solvent in silicon source less than 2%, the parts by weight 1-3 of water; Manufacturing process steps is followed successively by: above-mentioned each raw material that will be except that inorganic agent mixes stirrings, static hydrolysis, adding inorganic agent and carries out polycondensation reaction, puts into that mould wears out, cleans, drying.

Described silicon source is an ethyl orthosilicate, and solvent is an ethanol, and inorganic agent is an ammoniacal liquor, and surface modifier is a trim,ethylchlorosilane, and catalyst is a hydrochloric acid, and fiber is diameter 3-10nm, < 3mm, water are deionized water to length.

After earlier silicon source, solvent, surface modifier, catalyst, fiber and water being stirred according to said mixed, static certain hour is with its abundant hydrolysis; Add inorganic agent then and carry out polycondensation reaction; Put into mould and wear out, ageing time is 72-84h; After treating that solution is transformed into gel, use deionized water rinsing 10min, remove the soluble ion that dereaction stays; With the methanol solvate flushing, displace the aqueous solution wherein again; Wet gel is put into the supercritical drying equipment that preliminary filling has the carbon dioxide of 7.5-8Mpa, and temperature is higher than 40 ℃, keeps 2-5h, again with the speed release pressure of 1-2Mpa/h; Dash with carbon dioxide at last and sweep 5-10min, the transparency aerogel that gets product.

The invention has the beneficial effects as follows: the thermal conductivity factor of aeroge is extremely low, cooperates the particularity of vacuum glass can satisfy requirements of saving energy.The intensity of aeroge is very high, but fragility is very big, and molding effect is bad, adds an amount of glass fibre, can improve the toughness of aeroge, strengthens the ability to bear of pressure to external world, has improved bulk strength greatly, is not easy breakage.

The specific embodiment

Referring to Fig. 1, the composition of a kind of transparency aerogel of the present invention and content are that the part by weight of part by weight 1-5 ‰ (accounting for the gross weight ratio), fiber of parts by weight 1-10, the catalyst of part by weight 1-5 ‰ (accounting for the gross weight ratio), the surface modifier of parts by weight 15-25, the inorganic agent of parts by weight 5-15, the solvent in silicon source is less than the parts by weight 1-3 of 2% (accounting for the gross weight ratio), water.

Described silicon source is an ethyl orthosilicate, and solvent is an ethanol, and inorganic agent is an ammoniacal liquor; Surface modifier is a trim,ethylchlorosilane, and catalyst is a hydrochloric acid, and fiber is diameter 3-10nm, length < 3mm; Fiber is a glass fibre, can not be transparent, but diameter is very little; Addition is less, is mixed in the colloidal sol almost to can't see.Water is deionized water.

The manufacture craft of transparency aerogel is:

1, silicon source, solvent, surface modifier, catalyst, fiber and water are stirred according to said mixed after, the static 30-60min time is with its abundant hydrolysis.

2, add inorganic agent then and carry out polycondensation reaction, the adding inorganic agent stirs and gets final product 10min (5-30min).

3, put into mould and wear out, ageing time is 72-84h.Aging is a process of polycondensation, is transformed into gel from solution.

4, clean: the gel after will wearing out is used deionized water rinsing 10min, removes the soluble ion that dereaction stays; And then, displace the aqueous solution wherein with the methanol solvate flushing.

5, drying: wet gel is put into the supercritical drying equipment that preliminary filling has the carbon dioxide of 7.5-8Mpa, and temperature is higher than 40 ℃-200 ℃, keeps 2-5h; Again with the speed release pressure of 1-2Mpa/h; Dash with carbon dioxide at last and sweep (sweeping off the ion that remnants adhere to) 5-10min, the transparency aerogel that gets product.

Claims

1. the preparation method of a transparency aerogel; It is characterized in that, the composition of described transparency aerogel and content be the part by weight of part by weight 1-5 ‰, fiber of parts by weight 1-10, the catalyst of part by weight 1-5 ‰, the surface modifier of parts by weight 15-25, the inorganic agent of parts by weight 5-15, the solvent in silicon source less than 2%, the parts by weight 1-3 of water; Manufacturing process steps is followed successively by: above-mentioned each raw material that will be except that inorganic agent mixes stirrings, static hydrolysis, adding inorganic agent and carries out polycondensation reaction, puts into that mould wears out, cleans, drying.

2. the preparation method of transparency aerogel according to claim 1 is characterized in that, described silicon source is an ethyl orthosilicate; Solvent is an ethanol, and inorganic agent is an ammoniacal liquor, and surface modifier is a trim,ethylchlorosilane; Catalyst is a hydrochloric acid, and fiber is diameter 3-10nm, < 3mm, water are deionized water to length.

3. the preparation method of transparency aerogel according to claim 1 is characterized in that, after earlier silicon source, solvent, surface modifier, catalyst, fiber and water being stirred according to said mixed, static certain hour is with its abundant hydrolysis; Add inorganic agent then and carry out polycondensation reaction; Put into mould and wear out, ageing time is 72-84h; After treating that solution is transformed into gel, use deionized water rinsing 10min, remove the soluble ion that dereaction stays; With the methanol solvate flushing, displace the aqueous solution wherein again; Wet gel is put into the supercritical drying equipment that preliminary filling has the carbon dioxide of 7.5-8Mpa, and temperature is higher than 40 ℃, keeps 2-5h, again with the speed release pressure of 1-2Mpa/h; Dash with carbon dioxide at last and sweep 5-10min, the transparency aerogel that gets product.