CN101318662A - Method for preparing liquid soluble glass with silica gel in atmosphere pressure - Google Patents
Method for preparing liquid soluble glass with silica gel in atmosphere pressure Download PDFInfo
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- CN101318662A CN101318662A CNA2008100586578A CN200810058657A CN101318662A CN 101318662 A CN101318662 A CN 101318662A CN A2008100586578 A CNA2008100586578 A CN A2008100586578A CN 200810058657 A CN200810058657 A CN 200810058657A CN 101318662 A CN101318662 A CN 101318662A
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- silica gel
- atmosphere pressure
- caustic soda
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- soluble glass
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Abstract
The invention relates to a method for preparing a liquid water glass with silica gel at the condition of normal pressure and drying, which belongs to the technical field of sodium silicate production in the inorganic chemistry industry. The method comprises the following steps: a) liquid caustic soda for industrial use is added to a reaction pot, heated and stirred, b) when the temperature of the liquid caustic soda reaches 70-80 DEG. C, wet silica gel is evenly added, c) the heating is continued and the temperature is kept at 76-112 DEG. C, the liquid caustic soda reacts with the wet silica gel, d) the reaction stops after the wet silica gel is completely dissolved and a translucent liquid substance is produced, the liquid substance is condensed and cooled to obtain the product. The method of the invention has simple process, low energy consumption and low cost; besides, the method develops a very good way for utilizing waste silica gel which is a byproduct of phosphate fertilizer plants.
Description
Technical field:
The invention belongs to the water glass production technical field in the inorganic chemistry industry, relate to a kind of method for preparing liquid soluble glass by silica gel in atmosphere pressure.
Background technology
Silica gel is the by product of phosphate fertilizer plant, and each big-and-middle-sized phosphatic fertilizer company of the whole nation is all recycled to silicofluoric acid at present, and only its silica gel does not rationally utilize basically.Because of it contains silicofluoric acid and tiny SiO
2, serious environment pollution is considered as by people in " refuse " for a long time, is among the circumstances that is difficult to handle and can not piles up.
The method of traditional mode of production water glass is divided into two kinds of dry method and wet methods.
What be used for dry production at present has yellow soda ash and quartz sand and sodium sulfate and quartz sand, i.e. two kinds of operational paths of soda ash method and mirabilite method.The soda ash method is that quartz sand powder is broken to 60-80 order fineness, mixes with light ash, by stirring feeder and lift compound is added high hopper, quantitatively adds in the reflecting kiln again, and compound carries out frit reaction under 1350 ℃ of conditions.Its chemical equation is: Na
2CO
3+ nSiO
2→ Na
2OnSiO
2+ CO
2↑, production process comprises batching, calcines, soaks 4 procedures such as molten, concentrated.The soda ash method is fully matured technically, but has shortcomings such as energy consumption height, raw material consumption height, facility investment are big, cost height.Mirabilite method is for relaxing the nervous novel method of developing, replacing soda ash with the abundant saltcake of storage of soda ash.Its chemical equation is: 2Na
2SO
4+ C+2nSiO
2→ 2Na
2OnSiO
2+ 2SO
2↑+CO
2↑, the production technique of mirabilite method and soda ash method is basic identical, but mirabilite method when saltcake reacts incomplete, has saltcake water to exist in reaction process, contacts and can blast with water, so mirabilite method is of little use in actual production.
It is to be raw material with quartz sand and industrial liquid caustic soda that conventional wet is produced, and in autoclave, is 140 ℃-160 ℃ in temperature, and pressure is 5.9 * 10
5Pa reacted 7 hours down, but this method is difficult to make the water glass of high-module.Its chemical equation is: nSiO
2+ 2NaOH → Na
2OnSiO
2+ H
2O, whole technological process can be divided into batch mixes, reacting by heating and filtering and concentrating etc.
In sum, the method for traditional mode of production water glass, complex technical process, temperature of reaction is up to 1400 ℃-1500 ℃, and reaction pressure is had relatively high expectations to equipment material up to 0.6MPa, and energy expenditure is also very high simultaneously.
Prior art has had the silica gel of phosphate fertilizer plant's by-product after treatment as the raw material of preparation water glass, its major technique means are that silica gel and industrial liquid caustic soda are carried out compressive reaction, in reaction pressure is 0.7MPa-0.8MPa, about 160 ℃ of temperature of reaction just can obtain liquid soluble glass under reaction times 6-7 hour.
Summary of the invention
The object of the present invention is to provide a kind ofly to prepare the method for liquid soluble glass, and technology is simple, a kind of method that is prepared liquid soluble glass by silica gel in atmosphere pressure that energy consumption is low by silica gel in atmosphere pressure.
Of the present inventionly a kind ofly prepare the method for liquid soluble glass by silica gel in atmosphere pressure, its method is:
A. the industrial liquid caustic soda adds retort, and heating is stirred;
When treating that b. the liquid caustic soda temperature rises to 70 ℃-80 ℃, the balanced silica gel that wets that adds;
C. continue heating, temperature is remained on 76 ℃-112 ℃, liquid caustic soda and wet silica gel react;
D. react to the whole dissolvings of silica gel, get translucent fluent meterial, fluent meterial is concentrated, cooling gets product.
The additional proportion of described industrial liquid caustic soda and wet silica gel is: 1-2.5: 2.
The concentration of the described industrial liquid caustic soda of step a is 25%-30%.
The silica containing fluorine that the described wet silica gel of step b is phosphate fertilizer plant's by-product separates through press filtration, removes silicofluoric acid, forms through washing.
The pH value 3.5-4.0 of described wet silica gel, moisture 60%-70%.
The described adding of the step b silica gel that wets, the mode of its adding are balanced the adding, promptly in 30 minutes silica gel are added.
The described concentrated employing water-ring vacuum pump of steps d carries out vacuum-evaporation, when being concentrated into heat and surveying degree Beaume and reach 37 ° of B é-38 ° of B é, stops to concentrate.
A kind of method for preparing liquid soluble glass by silica gel in atmosphere pressure of the present invention, one of its raw materials for production are phosphate fertilizer plant's by product waste residue silica gel, preparation process is after quantitative industrial liquid caustic soda is added retort, heating is also stirred it, when alkali liquid temperature rises to 70 ℃-80 ℃, the balanced retort that drops into of the silica gel that will quantitatively wet remains at temperature of charge under 76 ℃-112 ℃ the condition and reacts.Treat that silica gel all dissolves, material is translucent behind the state, changes enriching stage over to.At this moment, start water-ring vacuum pump, carry out vacuum-evaporation.When heat survey degree Beaume reaches 37 ° of B é-38 ° of B é, stop to concentrate, be finished product after the cooling.The present invention need not to use high temperature, high pressure, and can directly make liquid soluble glass, and unorthodox method obtains solid water glass like that earlier, low-temp reaction becomes liquid more afterwards, technology is reduced the number of than traditional method, and technology of the present invention is simple, and energy consumption is low, cost is low, and what have more meaning is the approach that utilizes that it has opened up an extraordinary phosphate fertilizer plant by product waste residue silica gel.
Description of drawings
Fig. 1 is the inventive method schematic flow sheet.
Embodiment:
The present invention is further illustrated below in conjunction with embodiment, but be not limited to embodiment.
Embodiment 1
With 1.44kg concentration is that 25.2% industrial liquid caustic soda adds in the retort, heats and stirs it.When alkali liquid temperature rises to 70 ℃-80 ℃, the balanced wet silica gel of 2kg that drops into, its pH value is 3.6, water content is 63.16%, adds within half an hour.Remain at temperature of charge under 90 ℃-95 ℃ the condition and react, treat that silica gel all dissolves, material is translucent behind the state, changes enriching stage over to.At this moment, start water-ring vacuum pump, carry out vacuum-evaporation.When heat survey degree Beaume reaches 37 ° of B é-38 ° of B é, stop to concentrate.Entire reaction concentration time 3.5 hours obtains finished product water glass 2.65kg after the cooling, 40 ° of B é of actual measurement degree Beaume, and the actual measurement modulus is 3.0.Na
2The yield of O is 77.13%, SiO
2Yield be 86.68%.
Embodiment 2
With 1.731kg concentration is that 27.2% industrial liquid caustic soda adds in the retort, heats and stirs it.When alkali liquid temperature rises to 70 ℃-80 ℃, the balanced wet silica gel of 2kg that drops into, its pH value is 4.0, water content is 65.84%, adds within half an hour.Remain at temperature of charge under 76 ℃-81 ℃ the condition and react, treat that silica gel all dissolves, material is translucent behind the state, changes enriching stage over to.At this moment, start water-ring vacuum pump, carry out vacuum-evaporation.When heat survey degree Beaume reaches 37 ° of B é-38 ° of B é, stop to concentrate.Entire reaction concentration time 3 hours obtains finished product water glass 3.40kg after the cooling, 40 ° of B é of actual measurement degree Beaume, and the actual measurement modulus is 3.21.Na
2The yield of O is 79.13%, SiO
2Yield be 94.16%.
Embodiment 3
With 1.731kg concentration is that 28.3% industrial liquid caustic soda adds in the retort, heats and stirs it.When alkali liquid temperature rises to 70 ℃-80 ℃, the balanced wet silica gel of 2kg that drops into, its pH value is 3.5, water content is 62.87%, adds within half an hour.Remain at temperature of charge under 82 ℃-89 ℃ the condition and react, treat that silica gel all dissolves, material is translucent behind the state, changes enriching stage over to.At this moment, start water-ring vacuum pump, carry out vacuum-evaporation.When heat survey degree Beaume reaches 37 ° of B é-38 ° of B é, stop to concentrate.Entire reaction concentration time 3 hours obtains finished product water glass 3.25kg after the cooling, 42 ° of B é of actual measurement degree Beaume, and the actual measurement modulus is 3.11.Na
2The yield of O is 77.37%, SiO
2Yield be 89.16%.
Embodiment 4
With 1.935kg concentration is that 29.4% industrial liquid caustic soda adds in the retort, heats and stirs it.When alkali liquid temperature rises to 70 ℃-80 ℃, the balanced wet silica gel of 2kg that drops into, its pH value is 3.8, water content is 68.25%, adds within half an hour.Remain at temperature of charge under 96 ℃-103 ℃ the condition and react, treat that silica gel all dissolves, material is translucent behind the state, changes enriching stage over to.At this moment, start water-ring vacuum pump, carry out vacuum-evaporation.When heat survey degree Beaume reaches 37 ° of B é-38 ° of B é, stop to concentrate.Entire reaction concentration time 4.5 hours obtains finished product water glass 3.25kg after the cooling, 40 ° of B é of actual measurement degree Beaume, and the actual measurement modulus is 3.04.Na
2The yield of O is 77.93%, SiO
2Yield be 91.19%.
Embodiment 5
With 1.935kg concentration is that 26.8% industrial liquid caustic soda adds in the retort, heats and stirs it.When alkali liquid temperature rises to 70 ℃-80 ℃, the balanced wet silica gel of 2kg that drops into, its pH value is 3.7, water content is 61.85%, adds within half an hour.Remain at temperature of charge under 103 ℃-112 ℃ the condition and react, treat that silica gel all dissolves, material is translucent behind the state, changes enriching stage over to.At this moment, start water-ring vacuum pump, carry out vacuum-evaporation.When heat survey degree Beaume reaches 37 ° of B é-38 ° of B é, stop to concentrate.Entire reaction concentration time 4.5 hours obtains finished product water glass 3.25kg after the cooling, 42 ° of B é of actual measurement degree Beaume, and the actual measurement modulus is 2.97.Na
2The yield of O is 81.01%, SiO
2Yield be 92.66%.
Embodiment 6
With 1.42kg concentration is that 26.5% industrial liquid caustic soda adds in the retort, heats and stirs it.When alkali liquid temperature rises to 70 ℃-80 ℃, the balanced wet silica gel of 2kg that drops into, its pH value is 3.9, water content is 64.57%, adds within half an hour.Remain at temperature of charge under 93 ℃-100 ℃ the condition and react, treat that silica gel all dissolves, material is translucent behind the state, changes enriching stage over to.At this moment, start water-ring vacuum pump, carry out vacuum-evaporation.When heat survey degree Beaume reaches 37 ° of B é-38 ° of B é, stop to concentrate.Entire reaction concentration time 3.2 hours obtains finished product water glass 2.6kg after the cooling, 38 ° of B é of actual measurement degree Beaume, and the actual measurement modulus is 2.26.Na
2The yield of O is 71.2%, SiO
2Yield be 86.22%.
Claims (8)
1, a kind ofly prepare the method for liquid soluble glass, it is characterized in that described method is by silica gel in atmosphere pressure:
A. the industrial liquid caustic soda adds retort, and heating is stirred;
When treating that b. the liquid caustic soda temperature rises to 70 ℃-80 ℃, the balanced silica gel that wets that adds;
C. continue heating, temperature is remained on 76 ℃-112 ℃, liquid caustic soda and wet silica gel react;
D. react to the whole dissolvings of silica gel, get translucent fluent meterial, fluent meterial is concentrated, cooling gets product.
2, according to claim 1ly a kind ofly prepare the method for liquid soluble glass, it is characterized in that the additional proportion of described industrial liquid caustic soda and wet silica gel is: 1-2.5: 2 by silica gel in atmosphere pressure.
3, according to claim 1 and 2ly a kind ofly prepare the method for liquid soluble glass, it is characterized in that the concentration of the described industrial liquid caustic soda of step a is 25%-30% by silica gel in atmosphere pressure.
4, according to claim 1 and 2ly a kind ofly prepare the method for liquid soluble glass, it is characterized in that the silica containing fluorine that the described wet silica gel of step b is phosphate fertilizer plant's by-product separates through press filtration, removes silicofluoric acid, forms through washing by silica gel in atmosphere pressure.
5, according to claim 4ly a kind ofly prepare the method for liquid soluble glass, it is characterized in that the pH value 3.5-4.0 of described wet silica gel, moisture 60%-70% by silica gel in atmosphere pressure.
6, according to claim 1 and 2ly a kind ofly prepare the method for liquid soluble glass, it is characterized in that by silica gel in atmosphere pressure, the described adding of the step b silica gel that wets, the mode of its adding is balanced adding the in 30 minutes.
7, according to claim 1 and 2ly a kind ofly prepare the method for liquid soluble glass, it is characterized in that the described concentrated employing water-ring vacuum pump of steps d carries out vacuum-evaporation by silica gel in atmosphere pressure.
8, according to claim 1 and 2ly a kind ofly prepare the method for liquid soluble glass, it is characterized in that, when being concentrated into heat and surveying degree Beaume and reach 37 ° of B é-38 ° of B é, stop to concentrate by silica gel in atmosphere pressure.
Priority Applications (1)
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|---|---|---|---|
| CN2008100586578A CN101318662B (en) | 2008-07-10 | 2008-07-10 | Method for preparing liquid soluble glass with silica gel in atmosphere pressure |
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|---|---|---|---|
| CN2008100586578A CN101318662B (en) | 2008-07-10 | 2008-07-10 | Method for preparing liquid soluble glass with silica gel in atmosphere pressure |
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| Publication Number | Publication Date |
|---|---|
| CN101318662A true CN101318662A (en) | 2008-12-10 |
| CN101318662B CN101318662B (en) | 2010-12-29 |
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|---|---|---|---|
| CN2008100586578A Expired - Fee Related CN101318662B (en) | 2008-07-10 | 2008-07-10 | Method for preparing liquid soluble glass with silica gel in atmosphere pressure |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103030153A (en) * | 2013-01-18 | 2013-04-10 | 昆明道尔森科技有限公司 | Method for preparing potash water glass |
| CN103030152A (en) * | 2013-01-18 | 2013-04-10 | 昆明道尔森科技有限公司 | Method for preparing electronic potassium silicate solution |
| CN103359750A (en) * | 2013-06-25 | 2013-10-23 | 叶卫斌 | Preparation method and application of artificial water-soluble silicon |
| CN103506213A (en) * | 2013-08-29 | 2014-01-15 | 紫金矿业集团股份有限公司 | Method for preparing liquid sodium silicate through copper and sulfide tailings |
| CN108117085A (en) * | 2018-03-21 | 2018-06-05 | 新乡市星汉化工有限公司 | Wet production potassium-sodium water glass |
| CN110127707A (en) * | 2019-06-12 | 2019-08-16 | 云南凯威特新材料股份有限公司 | A method of high hydrophobicity aerosil is prepared with product silica gel in phosphate fertilizer industry |
| TWI741683B (en) * | 2020-07-16 | 2021-10-01 | 國立臺灣大學 | Method of manufacturing high modulus water glass deposit by use of silicon kerf waste |
-
2008
- 2008-07-10 CN CN2008100586578A patent/CN101318662B/en not_active Expired - Fee Related
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103030153A (en) * | 2013-01-18 | 2013-04-10 | 昆明道尔森科技有限公司 | Method for preparing potash water glass |
| CN103030152A (en) * | 2013-01-18 | 2013-04-10 | 昆明道尔森科技有限公司 | Method for preparing electronic potassium silicate solution |
| CN103030153B (en) * | 2013-01-18 | 2014-09-24 | 昆明道尔森科技有限公司 | Method for preparing potash water glass |
| CN103030152B (en) * | 2013-01-18 | 2015-01-21 | 昆明道尔森科技有限公司 | Method for preparing electronic potassium silicate solution |
| CN103359750A (en) * | 2013-06-25 | 2013-10-23 | 叶卫斌 | Preparation method and application of artificial water-soluble silicon |
| CN103506213A (en) * | 2013-08-29 | 2014-01-15 | 紫金矿业集团股份有限公司 | Method for preparing liquid sodium silicate through copper and sulfide tailings |
| CN103506213B (en) * | 2013-08-29 | 2015-06-17 | 紫金矿业集团股份有限公司 | Method for preparing liquid sodium silicate through copper and sulfide tailings |
| CN108117085A (en) * | 2018-03-21 | 2018-06-05 | 新乡市星汉化工有限公司 | Wet production potassium-sodium water glass |
| CN110127707A (en) * | 2019-06-12 | 2019-08-16 | 云南凯威特新材料股份有限公司 | A method of high hydrophobicity aerosil is prepared with product silica gel in phosphate fertilizer industry |
| TWI741683B (en) * | 2020-07-16 | 2021-10-01 | 國立臺灣大學 | Method of manufacturing high modulus water glass deposit by use of silicon kerf waste |
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|---|---|
| CN101318662B (en) | 2010-12-29 |
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