CN104760965A - Promoter special for silicon dioxide aerogel and preparation method thereof - Google Patents
Promoter special for silicon dioxide aerogel and preparation method thereof Download PDFInfo
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- CN104760965A CN104760965A CN201510212783.4A CN201510212783A CN104760965A CN 104760965 A CN104760965 A CN 104760965A CN 201510212783 A CN201510212783 A CN 201510212783A CN 104760965 A CN104760965 A CN 104760965A
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- aerosil
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Abstract
The invention discloses a preparation method of a promoter special for silicon dioxide aerogel. The method comprises the steps that 1, stronger ammonia water with the mass percent not smaller than 25 percent and alcohols solvents are evenly mixed, a solution A is obtained, and the volume ratio of the stronger ammonia water to the alcohols solvents is 1:10-20; 2, silane coupling agent by-products and the solution A with the volume ratio of 1:3-8 are mixed evenly and react for 10 to 30 minutes under the temperature condition of 5 DEG C to 15 DEG C, and the promoter special for the silicon dioxide aerogel is prepared. The invention further discloses the promoter special for the silicon dioxide aerogel. Compared with the prior art, the reutilization problem of the silane coupling agent by-products is solved, production, inventory and environmental protection pressure caused by overstock of a large number of by-products is eliminated, and the source of raw materials needed by the silicon dioxide aerogel and preparation of the promoter special for the silicon dioxide aerogel is expanded; meanwhile, the preparation process is simplified, efficiency is improved, and cost is lowered.
Description
Technical field
The present invention relates to the synthesis field of silane material and silane, be specifically related to a kind of aerosil special assistant and preparation method thereof.
Background technology
Aerosil belongs to ceramic, has high chemical stability, extremely wide temperature resistant range, extremely low thermal conductivity, and do not burn, nontoxic, physiological inertia.Especially after 2000, rapidly being developed, be widely used in the fields such as space flight, petrochemical industry, electric power, building, medicine, environmental protection, new forms of energy, is heat-insulating material the most excellent at present.
Aerosil generally adopts silicone grease, water glass, silicon sol etc. to obtain gel for silicon source body sol-gel method, then uses modifier treatment gel, then dry obtained.Utilize the auxiliary agent that silane coupling agent by product after cut is obtained, there is not yet bibliographical information at home and abroad.
And the by product after cut of organo-silicon coupling agent γ-amine propyl trialkoxy silane accounts for about 10% of this coupling agent output, this by product is mixture, and its main component is secondary amine and cyclammonium, and composition is not simple, lack effective application and process, form stock and environmental protection pressure.
Summary of the invention
For the problems referred to above and defect, the object of the present invention is to provide a kind of aerosil special assistant and preparation method thereof, aerosil special assistant is obtained by utilizing the by product after cut of silane coupling agent, thus both solved the defect existed in existing production aerosil special assistant technology, stock and the environmental protection pressure problem of the existence of organo-silicon coupling agent by product after cut can be alleviated again simultaneously.
A kind of aerosil special assistant preparation method provided by the invention, comprises step:
1) strong aqua mass percent being not less than 25% mixes with alcoholic solvent, obtained solution A, and the volume ratio of described strong aqua and described alcoholic solvent is 1:10-20;
2) be that the silane coupling agent by product of 1:3-8 mixes with described solution A by volume ratio, at 5-15 DEG C of temperature condition reaction 10-30 minute, obtained aerosil special assistant.
Preferably, described strong aqua mass percent is 25-28%.
Preferably, described alcoholic solvent is any one in methyl alcohol, ethanol.
Preferably, described silane coupling agent by product is produce any one in the after cut of γ-amine propyl trimethoxy silicane or γ-amine propyl-triethoxysilicane.
Another object of the present invention is to provide a kind of aerosil special assistant obtained by above-mentioned preparation method.
The reaction formula of main chemical reactions of the present invention is as follows:
Note: R is methyl or ethyl
As can be seen from the above technical solutions, the embodiment of the present invention has the following advantages:
By utilizing silane coupling agent by product after cut to prepare aerosil special assistant, solve the recycling problem of silane coupling agent by product, eliminate this by product overstock in a large number bring production, stock and environmental protection pressure; Extend aerosil and the raw material sources needed for special assistant preparation thereof, meanwhile, simplify preparation technology, improve efficiency, reduce cost.
Accompanying drawing explanation
Fig. 1 is the TEM photo of aerosil obtained in the embodiment of the present invention 5;
Fig. 2 is the TEM photo of aerosil obtained in the embodiment of the present invention 10;
Fig. 3 is the TEM photo of aerosil obtained in the embodiment of the present invention 12.
Embodiment
Embodiments provide a kind of aerosil special assistant and preparation method thereof, aerosil special assistant is prepared by utilizing silane coupling agent by product after cut, for solving the problem of silane coupling agent by product recycling, eliminate this by product overstock in a large number bring production, stock and environmental protection pressure, extend aerosil and the raw material sources needed for special assistant preparation thereof, meanwhile, simplify preparation technology, improve efficiency, reduce cost.
For making goal of the invention of the present invention, feature, advantage can be more obvious and understandable, below in conjunction with the specific embodiment of the invention and accompanying drawing, technical solution of the present invention is clearly and completely described, obviously, the embodiments described below are only the present invention's part embodiments, and the embodiment of not all.Based on the embodiment in the present invention, those of ordinary skill in the art, not making other embodiments all obtained under creative work prerequisite, belong to the scope of protection of the invention.
Below in conjunction with specific embodiment, summary of the invention of the present invention is set forth.
Embodiment 1
2L strong aqua is added in 20L methyl alcohol, stirs, obtained A1, for subsequent use;
Strong aqua in the embodiment of the present invention is chemical pure, and mass percent concentration is 25%;
Getting 5L silane coupling agent by product (after cut of γ-amine propyl trimethoxy silicane) adds in A1, stirs, and reacts 20 minutes under 10 DEG C of temperature condition, and obtained B1, B1 are aerosil special assistant.
Embodiment 2
1) 2L strong aqua is added in 40L methyl alcohol, stir, obtained A2, for subsequent use;
Strong aqua in the embodiment of the present invention is chemical pure, and mass percent concentration is 26%;
2) getting 14L silane coupling agent by product (after cut of γ-amine propyl trimethoxy silicane) adds in A2, stirs, and reacts 22 minutes under 12 DEG C of temperature condition, and obtained B2, B2 are aerosil special assistant.
Embodiment 3
1) 2L strong aqua is added in 22L methyl alcohol, stir, obtained A3, for subsequent use;
Strong aqua in the embodiment of the present invention is chemical pure, and mass percent concentration is 27%;
2) getting 8L silane coupling agent by product (after cut of γ-amine propyl trimethoxy silicane) adds in A3, stirs, and reacts 30 minutes under 5 DEG C of temperature condition, and obtained B3, B3 are aerosil special assistant.
Embodiment 4
1) 2L strong aqua is added in 22L methyl alcohol, stir, obtained A4, for subsequent use;
Strong aqua in the embodiment of the present invention is chemical pure, and mass percent concentration is 28%;
2) getting 3L silane coupling agent by product (after cut of γ-amine propyl trimethoxy silicane) adds in A4, stirs, and reacts 10 minutes under 15 DEG C of temperature condition, and obtained B4, B4 are aerosil special assistant.
Embodiment 5
1) add in 30L methyl alcohol by 2L strong aqua, limit is stirred, obtained A5, for subsequent use;
Strong aqua in the embodiment of the present invention is chemical pure, and mass percent concentration is 30%;
2) get 5L silane coupling agent by product (after cut of γ-amine propyl trimethoxy silicane) slowly to add in A5, and stir, react 10 minutes under 15 DEG C of temperature condition, obtained B5, for subsequent use, B5 is aerosil special assistant;
3) limit is stirred, and adds in 30L methyl alcohol respectively successively by 1L deionized water, 4L tetramethoxy-silicane, obtained C5;
4) getting 12L B5 adds in C5, stirs 5 minutes, leaves standstill, obtained alcogel;
5) airtight, ageing is after 3 hours, and dislocation is in autoclave, and be heated to temperature 246 DEG C, the supercritical state of pressure 9.0Mpa, constant temperature, slowly discharges solvent, within 4 hours, obtains aerosil.
After testing, aerosil is hydrophobicity, specific surface area 858m2/g, empty capacity rate 95%, thermal conductivity 0.013W/m.k.
Embodiment 6
1), 2) with embodiment 5
3) limit is stirred, and adds in 30L methyl alcohol respectively successively by 3L deionized water, 6L tetramethoxy-silicane, obtained C6;
4) getting 8L B5 adds in C6, and limit is stirred, 5 minutes, leaves standstill, obtained alcogel;
5) airtight, ageing is after 3 hours, and dislocation is in autoclave, and be heated to temperature 260 DEG C, the supercritical state of pressure 9.0Mpa, constant temperature, slowly discharges solvent, within 6 hours, obtains aerosil.
Aerosil is hydrophobicity after testing, specific surface area 833m
2/ g, empty capacity rate 94.4%, thermal conductivity 0.015W/m.k.
Embodiment 7
1) by 2L mass percent concentration be 25% strong aqua add in 40L methyl alcohol, stir, obtained A7, for subsequent use;
2) get 7L silane coupling agent by product (after cut of γ-amine propyl trimethoxy silicane) slowly to add in A7, stir, react 15 minutes at temperature 10 DEG C, obtained B7, for subsequent use; B7 is aerosil special assistant;
3) limit is stirred, and adds in 20L methyl alcohol respectively successively by 1L deionized water, 3L tetramethoxy-silicane, obtained C7;
4) getting 10L B7 adds in C7, and limit is stirred, 5 minutes, leaves standstill, obtained alcogel;
5) airtight, ageing is after 3 hours, and dislocation is in autoclave, and be heated to temperature 250 DEG C, the supercritical state of pressure 8.5Mpa, constant temperature, slowly discharges solvent, within 3 hours, obtains aerosil.
After testing, aerosil is hydrophobicity, specific surface area 812m
2/ g, empty capacity rate 93.8%, thermal conductivity 0.014W/m.k.
Embodiment 8
1), 2) with embodiment 7
3) limit is stirred, and adds in 40L methyl alcohol respectively successively by 2L deionized water, 5L tetramethoxy-silicane, obtained C8;
4) getting 15L B7 adds in C8, and limit is stirred, 5 minutes, leaves standstill, obtained alcogel;
5) airtight, ageing is after 2 hours, and dislocation is in autoclave, and be heated to temperature 250 DEG C, the supercritical state of pressure 8.5Mpa, constant temperature, slowly discharges solvent, within 3 hours, obtains aerosil.
Aerosil is hydrophobicity after testing, specific surface area 834m2/g, empty capacity rate 94.5%, thermal conductivity 0.015W/m.k.
Embodiment 9
1) by 2L mass percent concentration be 28% strong aqua add in 30L ethanol, stir obtained A9, for subsequent use;
2) get 6L silane coupling agent by product (after cut of γ-amine propyl-triethoxysilicane) slowly to add in A9, react 30 minutes under 15 DEG C of conditions after stirring, obtained B9, for subsequent use; B9 is aerosil special assistant;
3) under agitation, respectively 1L deionized water, 6L tetraethoxysilane are added in 15L ethanol successively, obtained C9;
4) getting 8L B9 adds in C9, stirs 5 minutes, leaves standstill, obtained alcogel;
5) airtight, ageing is after 6 hours, and dislocation is in autoclave, and be heated to temperature 245 DEG C, the supercritical state of pressure 7.0Mpa, constant temperature, slowly discharges solvent, within 3 hours, obtains aerosil.
After testing, aerosil is hydrophobicity, specific surface area 833m
2/ g, empty capacity rate 94%, thermal conductivity 0.014W/m.k.
Embodiment 10
1) by 2L mass percent concentration be 30% strong aqua add in 24L ethanol, stir obtained A10, for subsequent use;
2) get 8L silane coupling agent by product (after cut of γ-amine propyl-triethoxysilicane) slowly to add in A10, stir, react 25 minutes under 15 DEG C of temperature condition, obtained B10, for subsequent use; B10 is aerosil special assistant;
3) under agitation, respectively 1L deionized water, 5L tetraethoxysilane are added in 15L ethanol successively, obtained C10;
4) getting 12L B10 adds in C10, stirs 5 minutes, leaves standstill, obtained alcogel;
5) airtight, ageing is after 4 hours, and dislocation is in autoclave, and be heated to temperature 252 DEG C, the supercritical state of pressure 7.5Mpa, constant temperature, slowly discharges solvent, within 3 hours, obtains aerosil.
Aerosil is hydrophobicity after testing, specific surface area 837m
2/ g, empty capacity rate 94.3%, thermal conductivity 0.012W/m.k.
Embodiment 11
1) by 2L mass percent concentration be 28% strong aqua add in 30L methyl alcohol, stir, obtained A11, for subsequent use;
2) get 10L silane coupling agent by product (after cut of γ-amine propyl-triethoxysilicane) slowly to add in A11, stir, react 15 minutes under 15 DEG C of temperature condition, obtained B11, for subsequent use; B11 is aerosil special assistant;
3) limit is stirred, and adds in 20L methyl alcohol respectively successively by 2L deionized water, 5L tetramethoxy-silicane, obtained C11;
4) getting 8L B11 adds in C11, stirs 5 minutes, leaves standstill, obtained alcogel;
5) airtight, ageing is after 3 hours, and dislocation is in autoclave, and be heated to temperature 240 DEG C, the supercritical state of pressure 9.0Mpa, constant temperature, slowly discharges solvent, within 4 hours, obtains aerosil.
After testing, aerosil is hydrophobicity, specific surface area 802m
2/ g, empty capacity rate 93.5%, thermal conductivity 0.015W/m.k.
Embodiment 12
1) by 2L mass percent concentration be 28% strong aqua add in 24L methyl alcohol, stir, obtained A12, for subsequent use;
2) get 6L silane coupling agent by product (after cut of γ-amine propyl-triethoxysilicane) slowly to add in A12, stir, react 15 minutes under 15 DEG C of temperature condition, obtained B12, for subsequent use; B12 is aerosil special assistant;
3) obtained 20LC12, slowly adds 20L B12 while stirring, continues stirring 5 minutes, leaves standstill, obtained alcogel;
4) airtight, ageing is after 4 hours, and dislocation is in autoclave, and be heated to temperature 245 DEG C, the supercritical state of pressure 8.5Mpa, constant temperature, slowly discharges solvent, within 4 hours, obtains aerosil.
After testing, aerosil is hydrophobicity, specific surface area 822m
2/ g, empty capacity rate 94.5%, thermal conductivity 0.012W/m.k.
The above, above embodiment only in order to technical scheme of the present invention to be described, is not intended to limit; Although with reference to previous embodiment to invention has been detailed description, those of ordinary skill in the art is to be understood that: it still can be modified to the technical scheme described in foregoing embodiments, or carries out equivalent replacement to wherein portion of techniques feature; And these amendments or replacement, do not make the essence of appropriate technical solution depart from the spirit and scope of various embodiments of the present invention technical scheme.
Claims (5)
1. an aerosil special assistant preparation method, is characterized in that, comprises step:
1) strong aqua mass percent being not less than 25% mixes with alcoholic solvent, obtained solution A, and the volume ratio of described strong aqua and described alcoholic solvent is 1:10-20;
2) be that the silane coupling agent by product of 1:3-8 mixes with described solution A by volume ratio, at 5-15 DEG C of temperature condition reaction 10-30 minute, obtained aerosil special assistant.
2. a kind of aerosil special assistant preparation method according to claim 1, it is characterized in that, described strong aqua mass percent is 25-28%.
3. a kind of aerosil special assistant preparation method according to claim 1, it is characterized in that, described alcoholic solvent is any one in methyl alcohol, ethanol.
4. a kind of aerosil special assistant preparation method according to claim 1, is characterized in that, described silane coupling agent by product is produce any one in the after cut of γ-amine propyl trimethoxy silicane or γ-amine propyl-triethoxysilicane.
5. the aerosil special assistant that obtains of the preparation method as described in any one of Claims 1-4.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510212783.4A CN104760965B (en) | 2015-04-29 | 2015-04-29 | Promoter special for silicon dioxide aerogel and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510212783.4A CN104760965B (en) | 2015-04-29 | 2015-04-29 | Promoter special for silicon dioxide aerogel and preparation method thereof |
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| CN104760965A true CN104760965A (en) | 2015-07-08 |
| CN104760965B CN104760965B (en) | 2017-01-11 |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030009045A1 (en) * | 2001-06-01 | 2003-01-09 | Degussa Ag | Cleavage of cyclic organosilanes in the preparation of aminofunctional organoalkoxysilanes |
| CN103706342A (en) * | 2013-12-17 | 2014-04-09 | 南京工业大学 | Amino hybrid SiO2 aerogel material and application thereof |
-
2015
- 2015-04-29 CN CN201510212783.4A patent/CN104760965B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030009045A1 (en) * | 2001-06-01 | 2003-01-09 | Degussa Ag | Cleavage of cyclic organosilanes in the preparation of aminofunctional organoalkoxysilanes |
| CN103706342A (en) * | 2013-12-17 | 2014-04-09 | 南京工业大学 | Amino hybrid SiO2 aerogel material and application thereof |
Non-Patent Citations (5)
| Title |
|---|
| A. SOLEIMANI DORCHEH ET A.: "Silica aerogel;synthesis, properties and characterization", 《JOURNAL OF MATERIALS PROCESSING TECHNOLOGY》 * |
| DYLAN J. BODAY ET AL.: "Strong, Low-Density Nanocomposites by Chemical Vapor Deposition and Polymerization of Cyanoacrylates on Aminated Silica Aerogels", 《ACS APPLIED MATERIALS&INTERFACES》 * |
| 刘红艳 等: "硅氢加成一步合成γ-氨基丙基三甲氧基硅烷", 《石油化工》 * |
| 王妮 等: "不同硅源制备二氧化硅气凝胶的研究进展", 《材料导报A：综述篇》 * |
| 赵明 等: "γ-氨丙基三乙氧基硅烷合成新工艺", 《化学工程师》 * |
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