CN107151019A - A kind of preparation method of aeroge - Google Patents
A kind of preparation method of aeroge Download PDFInfo
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- CN107151019A CN107151019A CN201710395598.2A CN201710395598A CN107151019A CN 107151019 A CN107151019 A CN 107151019A CN 201710395598 A CN201710395598 A CN 201710395598A CN 107151019 A CN107151019 A CN 107151019A
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- Prior art keywords
- aeroge
- preparation
- gel
- displacement
- drying
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
- C01B33/157—After-treatment of gels
- C01B33/158—Purification; Drying; Dehydrating
- C01B33/1585—Dehydration into aerogels
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/44—Dehydration of aluminium oxide or hydroxide, i.e. all conversions of one form into another involving a loss of water
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/08—Drying; Calcining ; After treatment of titanium oxide
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/10—Solid density
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
- C01P2006/17—Pore diameter distribution
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Medicinal Preparation (AREA)
Abstract
The present invention relates to a kind of preparation method of aeroge, glycerine and polyethylene glycol oxide are used for displacement liquid, gel prepad fluid is entered into line replacement in displacement slot, are formed wet gel, are further dried, obtain aeroge.Beneficial effects of the present invention are：The preparation method selection glycerine and polyethylene glycol oxide of the aeroge of the present invention are displacement liquid, substituted for n-hexane and ethanol；Using only a step replacing process, you can obtain performance and service life all good aeroges.The preparation method of the aeroge of the present invention, use the raw material of safety and environmental protection, reduce the use and disposal of pollutants of hazardous chemical, make the production of aeroge more safe and environment-friendly, production cost is reduced simultaneously, it is ensured that the safety operation of production, reduce the pollution of volatile chemical among production environment, the air quality of production environment is improved, the discharge of pollutant is reduced while simplifying technique.
Description
Technical field
The invention belongs to technological field of biochemistry, and in particular to a kind of preparation method of aeroge.
Background technology
Aeroge is also known as xerogel.When gel sloughs most of solvent, make content liquid in gel fewer than solids content
Much, or in the space net structure of gel the medium being full of is gas, and appearance is in solid-like, also referred to as aeroge.Aeroge
It is one of a kind of solid matter form, the solid of world's upper density very little.
The preparation of aeroge is generally made up of sol-gel process and supercritical drying processing.In sol-gel process,
By controlling the poly-condensation and hydrolysis condition of solution, the phase formed in solution between the nanocluster of different structure, cluster
Mutual Adhesion formation gelinite, and then full of remaining liquid reagent after chemically reacting around the solid-state skeleton of gelinite.In order to
Prevent the surface tension during gel drying in Micro-v oid from causing the destruction of material structure, at supercritical drying process
Reason, is placed in gel to heat in pressure vessel and boosts, the liquid in gel is undergone phase transition into the fluid of above-critical state, gas-liquid circle
Face disappears, and surface tension has not existed, now discharged this supercritical fluid from pressure vessel, you can obtain porous, nothing
Sequence, the low-density aerogel materials with nanometer scale contiguous network structure.Table in the aeroge prepared due to conventional method
Face is with the presence of substantial amounts of hydroxyl, and they can not only cause gel mass to produce additional shrinkage because of polycondensation, moreover it is possible to adsorb in air
Moisture and make aeroge cracking broken, had a strong impact on the performances such as sound, light, electricity, heat, the mechanics of aeroge, limited its
Application scenario；And the time wasted in supercritical drying process is longer, or dry not thoroughly, cause the airsetting being made
Glue poor-performing.
Accordingly, it would be desirable to try to be modified the aeroge of preparation, increase its aerial stability and service life,
In addition, coordinating a series of enhancings, Toughening Measures again, so that more applicable aeroge is made.
In the modification production process of current aeroge, the raw materials used displacement liquid that common process is used is n-hexane and ethanol
It is related to dangerous poisonous chemicals Deng, used raw material, it is totally unfavorable to safety and environmental protection, and solution replacement technique one
As replaced using two steps or three steps, blowdown flow rate is larger.These poisonous ignition control compounds, during production operation to personnel and
Environment has security risk, nor meets the requirement of the green productions such as Environmental Safety.
The content of the invention
In order to solve the problem of prior art is present, the invention provides a kind of aeroge and preparation method thereof, the present invention
Purpose be to provide a kind of production technology of new aeroge, using the raw material of safety and environmental protection, reduce making for hazardous chemical
With and disposal of pollutants, make the production of aeroge more safe and environment-friendly, at the same reduce production cost.The system of the aeroge of the present invention
Preparation Method is applied to the production and processing of the aeroge of silica, aluminum oxide, titanium dioxide etc..
According to the preparation method of the aeroge of the present invention, comprise the following steps：
(1) gel prepad fluid and displacement liquid are sequentially placed into displacement slot and enter line replacement, form wet gel, the displacement liquid
For glycerine and polyethylene glycol oxide；
(2) wet gel is dried, obtains aeroge.
The configuration of prepad fluid：By organic silicon solution and isopropanol with 1：After 1.5 ratio mixing, it is with acetic acid regulation pH value
3-4。
Glycerine and polyethylene glycol oxide play a part of support gel rubber skeleton, and the acidity in gel is situated between as displacement liquid
Matter is cemented out.
According to the preparation method of the aeroge of the embodiment of the present invention, including：Replaced described in step (1) when
Between be 4.5-5.5 hour, the temperature of the displacement is 65-80 DEG C.
According to the aeroge of the embodiment of the present invention, wherein, the preparation method of the aeroge further comprises：
The time replaced described in step (1) is 5 hours, and the temperature of the displacement is 75 DEG C.Glycerine and polyoxygenated described in step (1)
The mass ratio of ethene is (35-45)：(65-55).
According to the preparation method of the aeroge of the embodiment of the present invention, further comprise, the glycerine and polyoxy
The mass ratio for changing ethene is 42:58.
The gel prepad fluid is the gel prepad fluid that silicate, aluminium hydroxide and titanium oxide are prepared.
Further, the drying is freeze-drying.
It is preferred that, the freeze-drying is vacuum freeze drying.
Further, the temperature of the vacuum freeze drying is subzero 5 DEG C-subzero 25 DEG C, the vacuum freeze drying
Vacuum be 100-50000Pa, time of the vacuum freeze drying is 2-48 hours.
Further, the temperature of the vacuum freeze drying is subzero 15 DEG C, the vacuum of the vacuum freeze drying
For 10000Pa, the time of the vacuum freeze drying is 24 hours.
Beneficial effects of the present invention are：The preparation method of the aeroge of the present invention is applied to silica, aluminum oxide, dioxy
Change production and processing of the aeroge of titanium etc. in modifying process.
Present invention improves over aeroge production technology, selection glycerine and polyethylene glycol oxide are displacement liquid, substituted for n-hexane
And ethanol；Traditional aeroge production technology needs three step solution replacements, and a step replacing process is used only in the present invention, you can
To performance and service life all good aeroges.The preparation method of the aeroge of the present invention, using the raw material of safety and environmental protection, subtracts
The use and disposal of pollutants of few hazardous chemical, make the production of aeroge more safe and environment-friendly, while reducing production cost, protect
The safety operation of production has been demonstrate,proved, the pollution of volatile chemical among production environment has been reduced, improves the air of production environment
Quality, the discharge of pollutant is reduced while simplifying technique.
Glycerine and polyethylene glycol oxide play a part of support gel rubber skeleton, and the acidity in gel is situated between as displacement liquid
Matter is cemented out.The specific surface area that aeroge is made using conventional three-step approach is generally 800-1100m2/ g, using the present invention
Aeroge preparation method made from aeroge the skeleton structure of gel is maintained due to optimizing replacing process, preferably,
The specific surface area of gained can reach 1500m2/ g, improves specific surface area so that supercritical drying more facilitates, and more saves
When, reduce production cost.
Embodiment
To make the object, technical solutions and advantages of the present invention clearer, technical scheme will be carried out below
Detailed description.Obviously, described embodiment is only a part of embodiment of the invention, rather than whole embodiments.Base
Embodiment in the present invention, those of ordinary skill in the art are resulting on the premise of creative work is not made to be owned
Other embodiment, belongs to the scope that the present invention is protected.
Embodiment 1
A kind of preparation method of aeroge, following steps are used during its modification processing：
(1) by organic silicon solution and isopropanol with 1：After 1.5 ratio mixing, it is 3 with acetic acid regulation pH value, obtains gel
Prepad fluid；Gel prepad fluid and displacement liquid are sequentially placed into displacement slot and enter line replacement, wet gel is formed, the displacement liquid is sweet
Oil and polyethylene glycol oxide；
(2) wet gel is dried, obtains aeroge.
Embodiment 2
A kind of preparation method of aeroge, following steps are used during its modification processing：
(1) by organic silicon solution and isopropanol with 1：After 1.5 ratio mixing, it is 4 with acetic acid regulation pH value, obtains gel
Prepad fluid；Gel prepad fluid and displacement liquid are sequentially placed into displacement slot, temperature is progress under conditions of 80 DEG C in displacement slot
Displacement 5.5 hours, forms wet gel, and the displacement liquid is glycerine and polyethylene glycol oxide；
(2) wet gel is dried, obtains aeroge.
Embodiment 3
A kind of preparation method of aeroge, following steps are used during its modification processing：
(1) by organic silicon solution and isopropanol with 1：After 1.5 ratio mixing, it is 3.5 with acetic acid regulation pH value, is coagulated
Glue prepad fluid；Gel prepad fluid and displacement liquid are sequentially placed into displacement slot, in displacement slot temperature be 65 DEG C under conditions of enter
Line replacement 5 hours, forms wet gel, and the displacement liquid is glycerine and polyethylene glycol oxide；
(2) wet gel is dried, dry temperature is subzero 5 DEG C, the vacuum of freeze-drying is 30000Pa, cold
The lyophilized dry time is 12 hours, obtains aeroge.
Embodiment 4
A kind of preparation method of aeroge, following steps are used during its modification processing：
(1) organic silicon solution for preparing aluminium hydroxide and isopropanol are with 1：After 1.5 ratio mixing, PH is adjusted with acetic acid
It is worth for 3.5, obtains gel prepad fluid；Gel prepad fluid and displacement liquid are sequentially placed into displacement slot, temperature is in displacement slot
Enter line replacement under conditions of 75 DEG C 5.5 hours, form wet gel, the displacement liquid is glycerine and polyethylene glycol oxide；
(2) wet gel is dried, dry temperature is subzero 15 DEG C, the vacuum of freeze-drying is 10000Pa, cold
The lyophilized dry time is 24 hours, obtains aeroge.
Embodiment 5
A kind of preparation method of aeroge, following steps are used during its modification processing：
(1) the gel prepad fluid and displacement liquid prepared silicate are sequentially placed into displacement slot, glycerine and polyethylene glycol oxide
Mass ratio be 45：65, temperature forms wet gel to enter line replacement 4.5 hours under conditions of 75 DEG C in displacement slot, described to put
Liquid is changed for glycerine and polyethylene glycol oxide；
(2) wet gel is dried, dry temperature is subzero 15 DEG C, the vacuum of freeze-drying is 30000Pa, cold
The lyophilized dry time is 24 hours, obtains aeroge.
Embodiment 6
A kind of preparation method of aeroge, following steps are used during its modification processing：
(1) the gel prepad fluid and displacement liquid of the preparations such as titanium oxide are sequentially placed into displacement slot, glycerine and polyoxyethylene
The mass ratio of alkene is 35：65, temperature forms wet gel to enter line replacement 5.5 hours under conditions of 75 DEG C in displacement slot, described
Displacement liquid is glycerine and polyethylene glycol oxide；
(2) wet gel is dried, dry temperature is subzero 15 DEG C, the vacuum of freeze-drying is 10000Pa, cold
The lyophilized dry time is 24 hours, obtains aeroge.
Embodiment 7
A kind of preparation method of aeroge, following steps are used during its modification processing：
(1) the gel prepad fluid and displacement liquid of the preparations such as aluminium hydroxide are sequentially placed into displacement slot, glycerine and polyoxygenated
The mass ratio of ethene is 45：55, temperature forms wet gel, institute to enter line replacement 5.5 hours under conditions of 75 DEG C in displacement slot
Displacement liquid is stated for glycerine and polyethylene glycol oxide；
(2) wet gel is dried, dry temperature is subzero 25 DEG C, the vacuum of freeze-drying is 20000Pa, cold
The lyophilized dry time is 24 hours.Obtain aeroge.
Embodiment 8
A kind of preparation method of aeroge, following steps are used during its modification processing：
(1) will with silicate etc. be raw material prepare gel prepad fluid and displacement liquid be sequentially placed into displacement slot, glycerine and
The mass ratio of polyethylene glycol oxide is 42:58, temperature is formed wet to enter line replacement 5.5 hours under conditions of 75 DEG C in displacement slot
Gel, the displacement liquid is glycerine and polyethylene glycol oxide；
(2) wet gel is subjected to vacuum freeze drying, the temperature of freeze-drying is subzero 25 DEG C, the vacuum of freeze-drying
For 50000Pa, the time of freeze-drying is 2 hours, obtains aeroge.
The technical parameter of aeroge is made from embodiment 1-8：Specific surface area：1500m2/ g, bulk density：80-
120kg/m3, porosity：97-99%, aperture：Less than 40nm, particle size range：0.1-2mm.
The foregoing is only a specific embodiment of the invention, but protection scope of the present invention is not limited thereto, any
Those familiar with the art the invention discloses technical scope in, change or replacement can be readily occurred in, should all be contained
Cover within protection scope of the present invention.Therefore, protection scope of the present invention should be based on the protection scope of the described claims.
Claims (10)
1. a kind of preparation method of aeroge, it is characterised in that comprise the following steps：
(1) gel prepad fluid and displacement liquid are sequentially placed into displacement slot and enter line replacement, form wet gel, the displacement liquid is sweet
Oil and polyethylene glycol oxide；
(2) wet gel is dried, obtains aeroge.
2. the preparation method of aeroge according to claim 1, it is characterised in that the time replaced described in step (1)
For 4.5-5.5 hours, the temperature of the displacement was 65-80 DEG C.
3. the preparation method of aeroge according to claim 2, it is characterised in that the time replaced described in step (1)
For 5 hours, the temperature of the displacement was 75 DEG C.
4. the preparation method of aeroge according to claim 1, it is characterised in that glycerine and polyoxy described in step (1)
The mass ratio for changing ethene is (35-45)：(65-55).
5. the preparation method of aeroge according to claim 4, it is characterised in that the matter of the glycerine and polyethylene glycol oxide
Amount is than being 42:58.
6. the preparation method of aeroge according to claim 1, it is characterised in that the gel prepad fluid be silicate,
The gel prepad fluid that aluminium hydroxide and titanium oxide are prepared.
7. the preparation method of aeroge according to claim 1, it is characterised in that the drying is freeze-drying.
8. the preparation method of aeroge according to claim 7, it is characterised in that the freeze-drying is dry for vacuum refrigeration
It is dry.
9. the preparation method of aeroge according to claim 8, it is characterised in that the temperature of the vacuum freeze drying is
Subzero 5 DEG C-subzero 25 DEG C, the vacuum of the vacuum freeze drying is 100-50000Pa, the time of the vacuum freeze drying
For 2-48 hours.
10. the preparation method of aeroge according to claim 9, it is characterised in that the temperature of the vacuum freeze drying
For subzero 15 DEG C, the vacuum of the vacuum freeze drying is 10000Pa, and the time of the vacuum freeze drying is 24 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710395598.2A CN107151019A (en) | 2017-05-27 | 2017-05-27 | A kind of preparation method of aeroge |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710395598.2A CN107151019A (en) | 2017-05-27 | 2017-05-27 | A kind of preparation method of aeroge |
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| CN107151019A true CN107151019A (en) | 2017-09-12 |
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| CN201710395598.2A Pending CN107151019A (en) | 2017-05-27 | 2017-05-27 | A kind of preparation method of aeroge |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109734101A (en) * | 2019-03-12 | 2019-05-10 | 江苏脒诺甫纳米材料有限公司 | A kind of high temperature resistant silicon substrate aerogel powder and preparation method thereof |
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| CN105142598A (en) * | 2013-02-25 | 2015-12-09 | 欧莱雅 | Gel-type cosmetic composition |
| CN106565198A (en) * | 2016-10-19 | 2017-04-19 | 成都新柯力化工科技有限公司 | A method of preparing flexible aerosil through atmospheric-pressure drying |
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2017
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|---|---|---|---|---|
| CN105142598A (en) * | 2013-02-25 | 2015-12-09 | 欧莱雅 | Gel-type cosmetic composition |
| CN106565224A (en) * | 2016-10-18 | 2017-04-19 | 成都新柯力化工科技有限公司 | Method for improving silica aerogel by using mullite fibers |
| CN106565198A (en) * | 2016-10-19 | 2017-04-19 | 成都新柯力化工科技有限公司 | A method of preparing flexible aerosil through atmospheric-pressure drying |
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| 严瑞瑄 主编: "《水溶性高分子》", 30 June 1998, 北京：化学工业出版社 * |
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| 杨亚玲 等主编: "《大学物理》", 30 June 2015, 北京：中国农业出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109734101A (en) * | 2019-03-12 | 2019-05-10 | 江苏脒诺甫纳米材料有限公司 | A kind of high temperature resistant silicon substrate aerogel powder and preparation method thereof |
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Application publication date: 20170912 |