CN105197942A - Cyclic utilization method for residual heat in silicon dioxide aerogel production - Google Patents
Cyclic utilization method for residual heat in silicon dioxide aerogel production Download PDFInfo
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- CN105197942A CN105197942A CN201510574541.XA CN201510574541A CN105197942A CN 105197942 A CN105197942 A CN 105197942A CN 201510574541 A CN201510574541 A CN 201510574541A CN 105197942 A CN105197942 A CN 105197942A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The invention provides a cyclic utilization method for residual heat in silicon dioxide aerogel production. The method comprises the steps of putting 50 parts (by volume) of dilute sulfuric acid solution in a vessel, dropwise adding a water glass solution into the vessel under the condition of magnetic stirring until the pH of a solution system reaches 4.5, dropwise adding 2 parts (by volume) of dryness control chemical additive DCCA and 2 parts (by volume) of anhydrous ethanol into the solution system, carrying out uniformly stirring, carrying out gelatinizing at normal temperature, carrying out aging for 2 hours, adding 50 parts (by volume) of anhydrous ethanol into the aged gel, carrying out soaking for 10 hours, then, adding 50 parts (by volume) of hexane into the gel, carrying out soaking for 11 hours, smashing the wet gel, carrying out suction filtration, carrying out washing repeatedly, then, putting the wet gel into a distillation vessel containing 150 parts (by volume) of azeotropic distillation medium, carrying out uniformly stirring, carrying out heating to carry out azeotropic distillation until the gel is evaporated to dryness, and then, drying the evaporated gel in an airblast drying oven for 2 hours at the temperature of 105 DEG C, thereby obtaining SiO2 aerogel powder. According to the method, a sol-gel/azeotropic distillation method is adopted, the flocculation process is fast, the flocculation effect is good, the uniformity of a gel structure is good, the structure of the silicon dioxide aerogel can be kept unatrophied and uncracked, and the produced product is large in pore volume and high in specific surface area.
Description
Technical field
The present invention relates to aerosil production technical field, particularly relate to the method for recycling residual heat in the production of a kind of aerosil.
Background technology
Aerosil is a kind of novel light nano-porous materials grown up this year, and it has translucent and that density is ultralight characteristic.Structurally have that voidage is high, density is low, primary particle is little and the feature such as specific surface area is large, be all used widely in all many-sides such as mechanics, acoustics, calorifics, optics and electricity.
The raw material of synthetic silica aerogel mainly adopts expensive tetraethoxy both at home and abroad at present, dry by adopting supercritical technology.Although adopt Supercritical Drying Technology to reduce surface tension; avoid the micropore atrophy of dried aerogel and dry and cracked; then supercritical process requires harsh to drying conditions; equipment is complicated; obvious burden is all caused to cost and safety; can not continuity and large-scale production, thus limit the application of this drying means.Therefore explore and how to maintain aerosil structure the study hotspot that atrophy and other cracked drying process become domestic and international scientific worker does not occur.
Summary of the invention
A kind of method of recycling residual heat in the object of the present invention is to provide aerosil to produce, to solve the problems of the technologies described above.
Technical problem to be solved by this invention realizes by the following technical solutions:
A kind of method of recycling residual heat in aerosil production, it is characterized in that: get 50 parts of (volume) dilution heat of sulfuric acid in container, under magnetic stirring, adopt mode first quick and back slow to drip the water glass solution diluted, until the pH of solution system reaches 4.5, then drip 2 parts of (volume) drying control chemical additive DCCA and 2 part of (volume) dehydrated alcohols, after stirring, be placed in gel under normal temperature, after aging 2 hours, obtain SiO
2wet gel;
50 parts of (volume) dehydrated alcohols are added in the wet gel after aging, soak 10 hours, then add 50 parts of (volume) hexanes, soak 11 hours, wet gel is smashed to pieces, suction filtration also washs for several times, then this wet gel is put into the distil container that 150 parts of (volume) component distillation media are housed, stirs, component distillation is carried out in heating, until evaporate to dryness, then remaining sample is placed in air dry oven in 105 DEG C of dryings 2 hours, obtains SiO
2aerogel powder; Described distil container is connected with holding tank by pipeline, and described install pipeline has interlayer, is provided with prolong in interlayer, and the heat that the cooling fluid in prolong is taken away is for the blast pipe preheating by air dry oven.
Described dilute sulphuric acid is that 98% vitriol oil and water are formulated by the volume ratio of 1:30, and described water glass solution is that industrial waterglass and water are formulated by the volume ratio of 1:2.
Gelation process comprises centrifugal solidifying wadding and leaves standstill solidifying two stages of wadding, centrifugal solidifying wadding 1.5 hours, leave standstill solidifying wadding 0.5 hour, centrifugal solidifying wadding to make container rotation centered by its central shaft, makes the fast rapid hardening wadding of container contents, in container rotation process, rotational velocity adopts the mode hocketed of accelerating and slow down, the maximum value of rotational velocity is 120r/min, and the minimum value of rotational velocity is 25r/min, accelerates to be 5s with the time of moderating process.
This solidifying wadding method, solidifying wadding efficiency can be improved and optimize solidifying wadding effect, under the mating reaction accelerated and be rotated in deceleration, impel gel structure homogenizing, prevent stress during drying cause shrink and dry and cracked, the time that traditional natural coagulates wadding is longer, is unfavorable for enhancing productivity, this solidifying wadding method substantially reduces the solidifying wadding time, improves production efficiency.
The invention has the beneficial effects as follows:
The present invention adopts the method for sol-gel/component distillation, and solidifying wadding process is fast, and solidifying wadding is effective, gel structure good evenness, and can maintain aerosil structure and atrophy and cracked does not occur, the product pore volume prepared is large, specific surface area is high.
Embodiment
The technique means realized to make the present invention, creation characteristic, reaching object and effect is easy to understand, below in conjunction with specific embodiment, set forth the present invention further, but following embodiment being only the preferred embodiments of the present invention, and not all.Based on the embodiment in embodiment, those skilled in the art under the prerequisite not making creative work obtain other embodiment, all belong to protection scope of the present invention.
A kind of method of recycling residual heat in aerosil production, get 50 parts of (volume) dilution heat of sulfuric acid in container, under magnetic stirring, adopt mode first quick and back slow to drip the water glass solution diluted, until the pH of solution system reaches 4.5, then drip 2 parts of (volume) drying control chemical additive DCCA and 2 part of (volume) dehydrated alcohols, after stirring, be placed in gel under normal temperature, after aging 2 hours, obtain SiO
2wet gel;
50 parts of (volume) dehydrated alcohols are added in the wet gel after aging, soak 10 hours, then add 50 parts of (volume) hexanes, soak 11 hours, wet gel is smashed to pieces, suction filtration also washs for several times, then this wet gel is put into the distil container that 150 parts of (volume) component distillation media are housed, stirs, component distillation is carried out in heating, until evaporate to dryness, then remaining sample is placed in air dry oven in 105 DEG C of dryings 2 hours, obtains SiO
2aerogel powder;
Gelation process comprises centrifugal solidifying wadding and leaves standstill solidifying two stages of wadding, centrifugal solidifying wadding 1.5 hours, leave standstill solidifying wadding 0.5 hour, centrifugal solidifying wadding to make container rotation centered by its central shaft, makes the fast rapid hardening wadding of container contents, in container rotation process, rotational velocity adopts the mode hocketed of accelerating and slow down, the maximum value of rotational velocity is 120r/min, and the minimum value of rotational velocity is 25r/min, accelerates to be 5s with the time of moderating process;
Above-mentioned dilute sulphuric acid is that 98% vitriol oil and water are formulated by the volume ratio of 1:30, and above-mentioned water glass solution is that industrial waterglass and water are formulated by the volume ratio of 1:2.
More than show and describe ultimate principle of the present invention, principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and specification sheets is only preference of the present invention; be not used for limiting the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.Application claims protection domain is defined by appending claims and equivalent thereof.
Claims (3)
1. an aerosil produce in the method for recycling residual heat, it is characterized in that: get 50 parts of (volume) dilution heat of sulfuric acid in container, under magnetic stirring, mode is first quick and back slow adopted to drip the water glass solution diluted, until the pH of solution system reaches 4.5, then 2 parts of (volume) drying control chemical additive DCCA and 2 part of (volume) dehydrated alcohols are dripped, after stirring, be placed in gel under normal temperature, after aging 2 hours, obtain SiO
2wet gel;
50 parts of (volume) dehydrated alcohols are added in the wet gel after aging, soak 10 hours, then add 50 parts of (volume) hexanes, soak 11 hours, wet gel is smashed to pieces, suction filtration also washs for several times, then this wet gel is put into the distil container that 150 parts of (volume) component distillation media are housed, stirs, component distillation is carried out in heating, until evaporate to dryness, then remaining sample is placed in air dry oven in 105 DEG C of dryings 2 hours, obtains SiO
2aerogel powder; Described distil container is connected with holding tank by pipeline, and described install pipeline has interlayer, is provided with prolong in interlayer, and the heat that the cooling fluid in prolong is taken away is for the blast pipe preheating by air dry oven.
2. aerosil according to claim 1 produce in the method for recycling residual heat, it is characterized in that: described dilute sulphuric acid is that 98% vitriol oil and water are formulated by the volume ratio of 1:30, described water glass solution is that industrial waterglass and water are formulated by the volume ratio of 1:2.
3. aerosil according to claim 1 produce in the method for recycling residual heat, it is characterized in that: gelation process comprises centrifugal solidifying wadding and leaves standstill solidifying two stages of wadding, centrifugal solidifying wadding 1.5 hours, leave standstill solidifying wadding 0.5 hour, centrifugal solidifying wadding to make container rotation centered by its central shaft, make the fast rapid hardening wadding of container contents, in container rotation process, rotational velocity adopts the mode hocketed of accelerating and slow down, the maximum value of rotational velocity is 120r/min, the minimum value of rotational velocity is 25r/min, accelerates to be 5s with the time of moderating process.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510574541.XA CN105197942A (en) | 2015-09-10 | 2015-09-10 | Cyclic utilization method for residual heat in silicon dioxide aerogel production |
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| CN201510574541.XA CN105197942A (en) | 2015-09-10 | 2015-09-10 | Cyclic utilization method for residual heat in silicon dioxide aerogel production |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112777601A (en) * | 2020-12-31 | 2021-05-11 | 新疆永安硅材料有限公司 | Environment-friendly special silicon dioxide and production method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009038393A2 (en) * | 2007-09-19 | 2009-03-26 | Neb, Co., Ltd. | Method for preparing surface-modified transparent bead type aerogel and aerogel prepared therefrom |
| CN101837982A (en) * | 2010-03-19 | 2010-09-22 | 福建师范大学 | Method for preparing silicon dioxide aerogel powder |
| CN103073008A (en) * | 2013-01-31 | 2013-05-01 | 中国科学技术大学 | Preparation method of silicon dioxide aerogel |
| CN104760964A (en) * | 2015-04-29 | 2015-07-08 | 江西安德力高新科技有限公司 | Silicon dioxide aerogel preparation method |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009038393A2 (en) * | 2007-09-19 | 2009-03-26 | Neb, Co., Ltd. | Method for preparing surface-modified transparent bead type aerogel and aerogel prepared therefrom |
| CN101837982A (en) * | 2010-03-19 | 2010-09-22 | 福建师范大学 | Method for preparing silicon dioxide aerogel powder |
| CN103073008A (en) * | 2013-01-31 | 2013-05-01 | 中国科学技术大学 | Preparation method of silicon dioxide aerogel |
| CN104760964A (en) * | 2015-04-29 | 2015-07-08 | 江西安德力高新科技有限公司 | Silicon dioxide aerogel preparation method |
Non-Patent Citations (1)
| Title |
|---|
| 岳瑞丽等: "Si02气凝胶的溶胶-凝胶／共沸蒸馏法制备及表征", 《福建师范大学学报》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112777601A (en) * | 2020-12-31 | 2021-05-11 | 新疆永安硅材料有限公司 | Environment-friendly special silicon dioxide and production method thereof |
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Application publication date: 20151230 |