CN102515184B - Method for preparing silicon dioxide powder by hydrolyzing silicon tetrachloride - Google Patents
Method for preparing silicon dioxide powder by hydrolyzing silicon tetrachloride Download PDFInfo
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- CN102515184B CN102515184B CN 201210004573 CN201210004573A CN102515184B CN 102515184 B CN102515184 B CN 102515184B CN 201210004573 CN201210004573 CN 201210004573 CN 201210004573 A CN201210004573 A CN 201210004573A CN 102515184 B CN102515184 B CN 102515184B
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- silicon tetrachloride
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- dioxide powdery
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Abstract
The invention provides a method for preparing silicon dioxide powder by hydrolyzing silicon tetrachloride and belongs to the field of material preparation and use. The method disclosed by the invention comprises the following steps: firstly, preparing 0.1 to0.8g.L<-1> surfactant solution serving as a reaction substrate, heating the solution to 30 to 55 DEG C, adding silicon tetrachloride into the solution, stirring the solution, aging the solution for a period of time and obtaining suspension containing an ortho-silicic acid precipitate; and filtering the suspension containing the ortho-silicic acid precipitate, washing the ortho-silicic acid precipitate, obtaining an ortho-silicic acid filter cake, drying the ortho-silicic acid filter cake and obtaining silicon dioxide powder. The method prepared by the invention has the characteristics of readily available raw material, simple preparation process, low reaction temperature, short reaction time, low energy consumption, suitability for industrial production and the like.
Description
Technical field
The invention belongs to and belong to material preparation and Application Areas, it is suitable for the additive as reinforcing rubber.Relate to a kind of method for preparing silicon-dioxide powdery with silicon tetrachloride hydrolysis in surfactant soln.
Background technology
Polysilicon is the foundation stone of photovoltaic solar industry, the demand sharp increase, and along with starting of numerous domestic large polycrystalline silicon project, a large amount of savings of its downstream severe corrosive silicon tetrachloride as by-product have limited the sound development of polysilicon industrial chain.In recent years, many investigators are devoted to explore new silicon tetrachloride and consume the path, and obtain the silicon-dioxide that suitable particle size distributes by improving existing technology.
The method that with the silicon tetrachloride is the feedstock production silicon-dioxide powdery at present mainly contains vapor phase process, organic solvent method, alkaline water solution, direct hydrolysis method.Vapor phase process is that silicon tetrachloride gasification and water vapour reaction are generated silicon-dioxide, and this technology needs to carry out under High Temperature High Pressure, and equipment material requires harsh, the production cost height.Organic solvent method is that silicon tetrachloride issues the reaction of unboiled water solution at organic solvent system.The solvent that this method is used is all toxic, contaminate environment, and the tail washings difficult treatment, the process exploitation prospect is little.Prepare silicon-dioxide in basic solution, precipitation is complete, and solid-liquid separation is easy.But alkaline environment neutralized reaction product hydrogenchloride has caused the wasting of resources.It is simple that the direct hydrolysis method has technology, low cost and other advantages, and product can only generate silicic acid, rather than silicon-dioxide, and the not volatile effusion of hydrogenchloride that generates.
If the production technique that a kind of energy consumption is low, cost is low can be provided, can solve the not shortcoming of volatile effusion of hydrogenchloride, and obtain silicon-dioxide powdery.Just can obtain the cleaner production approach that a kind of new silicon tetrachloride consumes path and silicon-dioxide, have very high industrial applications to be worth.
Summary of the invention
The objective of the invention is at the problem in the present technology, provide a kind of silicon tetrachloride hydrolysis to prepare the method for silicon-dioxide powdery.It has characteristics such as raw material is easy to get, preparation process is simple, temperature of reaction is low, the reaction times is short, energy consumption is low, reaction cost is low.
Specific practice is: at first prepare certain density surfactant soln as reaction substrate, more above-mentioned reaction substrate is heated to certain temperature, silicon tetrachloride joins in the above-mentioned solution within a certain period of time.Behind reinforced the finishing, reaction suspension is stirred ageing 1h, namely obtain one and contain the suspension that positive silicic acid precipitates.Filter the above-mentioned suspension that contains positive silicic acid precipitation, and wash positive silicic acid precipitation, obtain described positive silicic acid filter cake.The positive silicic acid filter cake that final drying is above-mentioned obtains silicon-dioxide powdery.
The present invention is achieved by the following technical programs:
A kind of silicon tetrachloride hydrolysis of the present invention prepares the method for silicon-dioxide powdery, and it may further comprise the steps:
At first compound concentration is 0.1～0.8gL
-1Surfactant soln as reaction substrate, again described reaction substrate is heated to 30～55 ℃, then silicon tetrachloride is joined in the time in the above-mentioned solution at 0.5～1h, behind reinforced the finishing, reaction suspension is stirred ageing 1h, namely obtain containing the suspension of positive silicic acid precipitation, filter the described suspension that contains positive silicic acid precipitation, and wash positive silicic acid precipitation, obtain described positive silicic acid filter cake, the described positive silicic acid filter cake of final drying obtains silicon-dioxide powdery.
The add-on of described silicon tetrachloride is 1～1.8mol/ (L substrate).
Preferably, described silicon tetrachloride hydrolysis prepares the method for silicon-dioxide powdery, it is characterized in that, described tensio-active agent is a kind of in sodium lauryl sulphate, Sodium dodecylbenzene sulfonate, OP-10 or the tween-80.
Preferably, described silicon tetrachloride hydrolysis prepares the method for silicon-dioxide powdery, it is characterized in that, the add-on of its silicon tetrachloride is 1.5mol/ (L substrate).
Preferably, described silicon tetrachloride hydrolysis prepares the method for silicon-dioxide powdery, it is characterized in that, described surfactant soln concentration is 0.3gL
-1
Preferably, described silicon tetrachloride hydrolysis prepares the method for silicon-dioxide powdery, it is characterized in that, the reinforced time of its silicon tetrachloride is 1h.
The present invention compared with prior art has the following advantages:
1. to select the silicon tetrachloride as by-product of polysilicon for use be reaction raw materials to this method, and the cost of preparation silicon-dioxide is lower.
2. selected tensio-active agent and water effect slackened the generation that silica dioxide granule is reunited, and improves the strainability of reaction mixture, makes this method be easier to industrialization.
3. originally be reflected in the bubbling reactor and carry out, less investment, preparation process is simple.
In a word, the present invention has characteristics such as raw material is easy to get, preparation process is simple, temperature of reaction is low, the reaction times is short, energy consumption is low, reaction cost is low, is fit to suitability for industrialized production.
Embodiment
The present invention is further illustrated below by specific embodiment:
Embodiment 1
Compound concentration is 0.3gL
-1Sodium dodecylbenzene sulfonate solution is as reaction substrate, and is heated to 45 ℃, begins to add silicon tetrachloride, and the add-on of silicon tetrachloride is 1mol/ (L substrate), and the reinforced time is 1h.Behind reinforced the finishing, reaction suspension is stirred ageing 1h, namely obtain one and contain the suspension that positive silicic acid precipitates.Filter the above-mentioned suspension that contains positive silicic acid precipitation, and wash positive silicic acid precipitation, obtain described positive silicic acid filter cake.The positive silicic acid filter cake that final drying is above-mentioned obtains silicon-dioxide powdery.The median size that records above-mentioned powder is 41nm, and recording silica product DBP adsorptive value is 2cm
3G
-1
Embodiment 2
Compound concentration is 0.3gL
-1OP-10 solution is as reaction substrate, and is heated to 40 ℃, begins to add silicon tetrachloride, and the add-on of silicon tetrachloride is 1.5mol/ (L substrate), and the reinforced time is 0.5h.Behind reinforced the finishing, reaction suspension is stirred ageing 1h, namely obtain one and contain the suspension that positive silicic acid precipitates.Filter the above-mentioned suspension that contains positive silicic acid precipitation, and wash positive silicic acid precipitation, obtain described positive silicic acid filter cake.The positive silicic acid filter cake that final drying is above-mentioned obtains silicon-dioxide powdery.The median size that records above-mentioned powder is 31nm, and recording silica product DBP adsorptive value is 1.9cm
3G
-1
Embodiment 3
Compound concentration is 0.3gL
-1Sodium dodecyl sulfate solution is as reaction substrate, and is heated to 40 ℃, begins to add silicon tetrachloride, and the add-on of silicon tetrachloride is 1mol/ (L substrate), and the reinforced time is 0.5h.Behind reinforced the finishing, reaction suspension is stirred ageing 1h, namely obtain one and contain the suspension that positive silicic acid precipitates.Filter the above-mentioned suspension that contains positive silicic acid precipitation, and wash positive silicic acid precipitation, obtain described positive silicic acid filter cake.The positive silicic acid filter cake that final drying is above-mentioned obtains silicon-dioxide powdery.The median size that records above-mentioned powder is 52nm, and recording silica product DBP adsorptive value is 2.2cm
3G
-1
Embodiment 4
Compound concentration is 0.3gL
-1Tween-80 solution is as reaction substrate, and is heated to 35 ℃, begins to add silicon tetrachloride, and the add-on of silicon tetrachloride is 1.5mol/ (L substrate), and the reinforced time is 1h.Behind reinforced the finishing, reaction suspension is stirred ageing 1h, namely obtain one and contain the suspension that positive silicic acid precipitates.Filter the above-mentioned suspension that contains positive silicic acid precipitation, and wash positive silicic acid precipitation, obtain described positive silicic acid filter cake.The positive silicic acid filter cake that final drying is above-mentioned obtains silicon-dioxide powdery.The median size that records above-mentioned powder is 74nm, and recording silica product DBP adsorptive value is 2.8cm
3G
-1
The positive silicic acid precipitation that technical solution of the present invention obtains is filtered easily, obtains positive silicic acid filter cake; Behind described positive silicic acid filter cake heating, drying, namely obtain silicon-dioxide powdery.The median size of described silicon-dioxide powdery is between 20～100nm, and recording silicon-dioxide powdery DBP adsorptive value is 1.8～2.8cm
3G
-1, be suitable for as rubber reinforced additive etc.
Claims (5)
1. a silicon tetrachloride hydrolysis prepares the method for silicon-dioxide powdery, it is characterized in that it may further comprise the steps:
At first compound concentration is 0.1～0.8gL
-1Surfactant soln as reaction substrate, again described reaction substrate is heated to 30～55 ℃, then silicon tetrachloride is joined in the time in the above-mentioned solution at 0.5～1h, behind reinforced the finishing, reaction suspension is stirred ageing 1h, namely obtain containing the suspension of positive silicic acid precipitation, filter the described suspension that contains positive silicic acid precipitation, and wash positive silicic acid precipitation, obtain described positive silicic acid filter cake, the described positive silicic acid filter cake of final drying obtains silicon-dioxide powdery;
The add-on of described silicon tetrachloride is 1～1.8mol/ (L substrate).
2. silicon tetrachloride hydrolysis as claimed in claim 1 prepares the method for silicon-dioxide powdery, it is characterized in that, described tensio-active agent is a kind of in sodium lauryl sulphate, Sodium dodecylbenzene sulfonate, OP-10 or the tween-80.
3. silicon tetrachloride hydrolysis as claimed in claim 1 prepares the method for silicon-dioxide powdery, it is characterized in that, the add-on of its silicon tetrachloride is 1.5mol/ (L substrate).
4. silicon tetrachloride hydrolysis as claimed in claim 1 prepares the method for silicon-dioxide powdery, it is characterized in that, described surfactant soln concentration is 0.3gL
-1
5. silicon tetrachloride hydrolysis as claimed in claim 1 prepares the method for silicon-dioxide powdery, it is characterized in that, the reinforced time of its silicon tetrachloride is 1h.
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| CN103803566B (en) * | 2014-03-10 | 2015-09-30 | 福建正盛无机材料股份有限公司 | The preparation method of transparent rubber strengthening agent precipitated silica |
| CN105859919B (en) * | 2016-04-17 | 2019-01-29 | 北京化工大学 | Complex carrier type catalyst and preparation method and application |
| CN108059168B (en) * | 2018-01-19 | 2019-09-24 | 四川广阳环保科技有限公司 | A kind of method, product and purposes preparing improved silica adsorbent using chlorosilane raffinate |
| CN107970880B (en) * | 2018-01-19 | 2019-09-03 | 四川广阳环保科技有限公司 | A kind of preparation method of improved silica adsorbent |
| CN108176366B (en) * | 2018-01-19 | 2019-09-24 | 四川广阳环保科技有限公司 | A kind of method, product and purposes preparing compound adsorbent using chlorosilane raffinate and chitosan |
| CN111943215B (en) * | 2019-05-14 | 2022-02-22 | 中天科技精密材料有限公司 | Preparation method of quartz powder |
| CN111717922A (en) * | 2020-07-01 | 2020-09-29 | 石河子大学 | Preparation method of spherical silicon dioxide |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1524785A (en) * | 2003-02-28 | 2004-09-01 | 中国石油天然气股份有限公司 | Process for preparing nm silicon dioxide from alkali metal silicate |
| CN101798088A (en) * | 2009-12-25 | 2010-08-11 | 河南科技大学 | Method for preparing white carbon black by utilizing silicon tetrachloride |
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| EP0372251B1 (en) * | 1988-11-22 | 1992-03-11 | Degussa Aktiengesellschaft | Method for the preparation of silicas |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1524785A (en) * | 2003-02-28 | 2004-09-01 | 中国石油天然气股份有限公司 | Process for preparing nm silicon dioxide from alkali metal silicate |
| CN101798088A (en) * | 2009-12-25 | 2010-08-11 | 河南科技大学 | Method for preparing white carbon black by utilizing silicon tetrachloride |
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| JP平2-180711A 1990.07.13 |
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