CN102153099A - Method for preparing water glass and hydrophobic silicon dioxide by using treatment waste slag of calcined sulfate slag - Google Patents
Method for preparing water glass and hydrophobic silicon dioxide by using treatment waste slag of calcined sulfate slag Download PDFInfo
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- CN102153099A CN102153099A CN 201010588748 CN201010588748A CN102153099A CN 102153099 A CN102153099 A CN 102153099A CN 201010588748 CN201010588748 CN 201010588748 CN 201010588748 A CN201010588748 A CN 201010588748A CN 102153099 A CN102153099 A CN 102153099A
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Abstract
The invention discloses a method for preparing water glass and hydrophobic silicon dioxide by using treatment waste slag of calcined sulfate slag, which comprises the following steps of: repeatedly washing the primary discharged waste slag of the treated calcined sulfate slag for 20 to 30 minutes by using 10 to 15 percent hydrochloric acid solution, washing the filtered filter cakes for three times by using clean water, and filtering the solution to obtain pure filter cakes; mixing the pure filter cakes and liquid sodium hydroxide in a steam heated pressure reactor in a pure mass ratio of 1:1.13-1.53 to perform reaction; filtering the formed sodium silicate solution, and performing light concentration and cooling on the obtained sodium silicate liquid to obtain a water glass liquid product; and diluting and purifying the water glass liquid, performing ion exchange to remove sodium ions, adding hydrochloric acid to perform acid heat reflux concentration, adding dimethyl dichlorosilane to perform hydrophobic treatment, removing the solvent, and drying the hydrophobic product to obtain the hydrophobic silicon dioxide. Because the treatment waste slag of the calcined sulfate slag is used as a raw material for preparing the water glass and the hydrophobic silicon dioxide, the waste is changed into valuable, and considerable economic benefit is created.
Description
Technical field
The present invention relates to the technical field of the comprehensive regulation and the utilization of the inorganic industrial discharge of sulfuric acid, particularly relate to a kind of method for preparing water glass and hydrophobic silica with the improvement waste residue of sulfate cinder.
Background technology
Sulfuric acid industry is the sulfuric acid of producing for the raw material contact process with the sulfurous iron ore, mainly is made up of raw material, roasting, purification, conversion and five operations of absorption.With the purification process flow process, be divided into dry method and wet method two big classes on the general custom through gas washing in SA production.The branch that wet purification has pickling, hot concentrated acid to wash and wash again.China pyrite-based sulfuric acid production minority factory is a pickling process at present, and majority still is a washing process.
Sulfurous iron ore mainly is made up of sulphur and iron, with a spot of non-ferrous metal and rare metal.Pyrite cinder is that pyrite burning extracts the residue of discharging behind the sulphur.Except sulphur was utilized, iron and other elements were still stayed and are burnt in the slag in the sulfurous iron ore.Burning slag is the raw material that is used for smelting iron, extract non-ferrous metal and makes material of construction.
The quantity discharged of unit sulfuric acid product is relevant with the grade of sulfurous iron ore and processing condition.The high more then bed drain purge of the grade of sulfurous iron ore is just few more under identical processing condition, otherwise then high.When the sulfurous iron ore sulphur content is 25～35%, generally produce the clinker that produces 0.7～1 ton approximately per ton.The percentage composition of the various compositions of following sulfate cinder is 43.31% for Z 250 content, and aluminium sesquioxide content is 8.13%, and calcium oxide content is 1.63%, and content of magnesia is 0.46%, and silica content is 35.73%, and the content of sulphur is 0.16%.
In a series of inventions such as " prepare sulfate cinder are muriatic method with chemical method ", by having extracted Z 250, aluminium sesquioxide, calcium oxide, magnesium oxide, silicon oxide, elemental sulfur element etc. behind the salt acid purification, form that remaining acid non-soluble substance is silicon-dioxide and elemental sulfur behind the various metal-salts.The present invention utilizes the processing waste residue of sulfate cinder to prepare the method for water glass and hydrophobic silica.This method is the patented invention of typical disposal of three wastes deutero-, and its purpose is exactly will eat dry deep-frying to the various materials of three wastes the insides and element all to use only.By the decomposition residue contamination source of several levels, in the hope of the secondary of the minimizing chemical industry three wastes of maximum possible or three times exhaust emission.
Summary of the invention
Technical problem to be solved by this invention is; improvement waste residue to sulfate cinder is handled; comprehensive utilization; preparation water glass and hydrophobic silica provide a kind of and prepare the method for water glass and hydrophobic silica with the improvement waste residue of sulfate cinder, and this method has effectively been avoided the secondary pollution of sulfuric acid industry; in primary emission, seek potentiality eat dry deep-frying clean, turn waste into wealth; become valuable silicon series product at last, create considerable economic, protected environment.
The technical solution adopted for the present invention to solve the technical problems is: the improvement waste residue of sulfate cinder prepares the method for water glass and hydrophobic silica, comprises the steps:
The hydrochloric acid soln repetitive scrubbing of primary emission waste residue (being mainly acid non-soluble substances such as silicon-dioxide and elemental sulfur) that sulfate cinder is administered 20～30 minutes with 10～15%, filter cake after the filtration washs three times with clear water, make pH value reach 6～7 and filter stand-byly again, obtain pure filter cake; Acid filtrate washing capable of circulation is used, and pollutes to save cost and to prevent; Acid clear water washing lotion can be blent the hydrochloric acid washings, and remainder reasonably discharges by basic treatment;
The pure filter cake (silicon-dioxide meter) of above-mentioned acquisition is mixed in the steam-heated pressure reactor with pure mass ratio 1:1.13～1.53 with liquid sodium hydroxide, start steam heating, stop to feed open steam after making reaction pressure reach 0.7～0.8Mpa, with the jacket steam insulation, and kept this pressure 3～8 hours; Afterwards the sodium silicate solution that forms is filtered, obtains the filter cake elemental sulfur, through washing, dry, pulverize, be packaged to be the elemental sulfur product; The sodium silicate liquid that obtains is concentrated, cools off through light again, obtain the water glass liquid product;
With the water glass liquid diluting and the purification of above-mentioned acquisition, carry out ion-exchange, remove sodium ion, adding hydrochloric acid then carries out acid heat and reflux to concentrate, add the dimethyldichlorosilane(DMCS) solvent monomer and carry out hydrophobic treatment, deviate from solvent, drying makes the hydrophobic silica product.
Its chemical equation is as follows: SiO2+2NaOH====Na2SiO3+H2O
Na2SiO3+?2HCl?====2NaCl+SiO2?+H2O
The invention has the beneficial effects as follows: one, the invention provides a kind of method for preparing water glass and hydrophobic silica with the improvement waste residue of sulfate cinder, this method has effectively utilized the material of the improvement waste residue of sulfate cinder to form, improvement waste residue to sulfate cinder is handled, water glass and hydrophobic silica are prepared in comprehensive utilization.Its two, water glass and hydrophobic silica purposes are wide, be two kinds of products that economic worth is bigger, have improved the economic benefit of the improvement waste residue of handling sulfate cinder, have created very big income repayment, are the model of the chemical industry comprehensive regulation and utilization.Its three, less investment prepares water glass and hydrophobic silica is particularly suitable to the improvement waste residue of handling sulfate cinder, we can say and has opened up a new road.Its four, the purity height of preparation, quality is guaranteed.Its five, this method has effectively been avoided the secondary pollution of sulfuric acid industry, in primary emission, seek potentiality eat dry deep-frying clean, turn waste into wealth, become valuable silicon series product at last, create considerable economic.
Embodiment
Embodiment 1, and present embodiment is described a kind ofly to prepare the method for water glass and hydrophobic silica with the improvement waste residue of sulfate cinder, comprises the steps:
Get silica content and be primary emission waste residue 500 kilograms of preparations water glass and hydrophobic silica that 35.73% sulfate cinder is administered, the hydrochloric acid soln repetitive scrubbing of primary emission waste residue (being mainly acid non-soluble substances such as silicon-dioxide and elemental sulfur) that sulfate cinder is administered 20～30 minutes with 10～15%, filter cake after the filtration washs three times with clear water, make pH value reach 6～7 and filter stand-byly again, obtain pure filter cake; Acid filtrate washing capable of circulation is used, and pollutes to save cost and to prevent; Acid clear water washing lotion can be blent the hydrochloric acid washings, and remainder reasonably discharges by basic treatment;
The pure filter cake (silicon-dioxide meter) of above-mentioned acquisition is mixed in the steam-heated pressure reactor with pure mass ratio 1:1.33 with liquid sodium hydroxide, start steam heating, stop to feed open steam after making reaction pressure reach 0.7～0.8Mpa, with the jacket steam insulation, and kept this pressure 3～8 hours; Afterwards the sodium silicate solution that forms is filtered, obtains the filter cake elemental sulfur, through washing, dry, pulverize, be packaged to be the elemental sulfur product; The sodium silicate liquid that obtains is concentrated, cools off through light again, obtain 362.3 kg of water glass precursor solution products;
With the water glass liquid diluting and the purification of above-mentioned acquisition, carry out ion-exchange, remove sodium ion, adding hydrochloric acid then carries out acid heat and reflux to concentrate, add the dimethyldichlorosilane(DMCS) solvent monomer and carry out hydrophobic treatment, deviate from solvent, drying makes 178.2 kilograms of hydrophobic silica products.
Embodiment 2, and present embodiment is described a kind ofly to prepare the method for water glass and hydrophobic silica with the improvement waste residue of sulfate cinder, comprises the steps:
Get silica content and be primary emission waste residue 500 kilograms of preparations water glass and hydrophobic silica that 35.73% sulfate cinder is administered, the hydrochloric acid soln repetitive scrubbing of primary emission waste residue (being mainly acid non-soluble substances such as silicon-dioxide and elemental sulfur) that sulfate cinder is administered 20～30 minutes with 10～15%, filter cake after the filtration washs three times with clear water, make pH value reach 6～7 and filter stand-byly again, obtain pure filter cake; Acid filtrate washing capable of circulation is used, and pollutes to save cost and to prevent; Acid clear water washing lotion can be blent the hydrochloric acid washings, and remainder reasonably discharges by basic treatment;
The pure filter cake (silicon-dioxide meter) of above-mentioned acquisition is mixed in the steam-heated pressure reactor with pure mass ratio 1:1.53 with liquid sodium hydroxide, start steam heating, stop to feed open steam after making reaction pressure reach 0.7～0.8Mpa, with the jacket steam insulation, and kept this pressure 3～8 hours; Afterwards the sodium silicate solution that forms is filtered, obtains the filter cake elemental sulfur, through washing, dry, pulverize, be packaged to be the elemental sulfur product; The sodium silicate liquid that obtains is concentrated, cools off through light again, obtain 416.8 kg of water glass precursor solution products;
With the water glass liquid diluting and the purification of above-mentioned acquisition, carry out ion-exchange, remove sodium ion, adding hydrochloric acid then carries out acid heat and reflux to concentrate, add the dimethyldichlorosilane(DMCS) solvent monomer and carry out hydrophobic treatment, deviate from solvent, drying makes 205 kilograms of hydrophobic silica products.
Embodiment 3, and present embodiment is described a kind ofly to prepare the method for water glass and hydrophobic silica with the improvement waste residue of sulfate cinder, comprises the steps:
Get silica content and be primary emission waste residue 500 kilograms of preparations water glass and hydrophobic silica that 35.73% sulfate cinder is administered, the hydrochloric acid soln repetitive scrubbing of primary emission waste residue (being mainly acid non-soluble substances such as silicon-dioxide and elemental sulfur) that sulfate cinder is administered 20～30 minutes with 10～15%, filter cake after the filtration washs three times with clear water, make pH value reach 6～7 and filter stand-byly again, obtain pure filter cake; Acid filtrate washing capable of circulation is used, and pollutes to save cost and to prevent; Acid clear water washing lotion can be blent the hydrochloric acid washings, and remainder reasonably discharges by basic treatment;
The pure filter cake (silicon-dioxide meter) of above-mentioned acquisition is mixed in the steam-heated pressure reactor with pure mass ratio 1:1.13 with liquid sodium hydroxide, start steam heating, stop to feed open steam after making reaction pressure reach 0.7～0.8Mpa, with the jacket steam insulation, and kept this pressure 3～8 hours; Afterwards the sodium silicate solution that forms is filtered, obtains the filter cake elemental sulfur, through washing, dry, pulverize, be packaged to be the elemental sulfur product; The sodium silicate liquid that obtains is concentrated, cools off through light again, obtain 307.9 kg of water glass precursor solution products;
With the water glass liquid diluting and the purification of above-mentioned acquisition, carry out ion-exchange, remove sodium ion, adding hydrochloric acid then carries out acid heat and reflux to concentrate, add the dimethyldichlorosilane(DMCS) solvent monomer and carry out hydrophobic treatment, deviate from solvent, drying makes 151.4 kilograms of hydrophobic silica products.
The above only is three preferred embodiments of the present invention, is not to be used for limiting the present invention, and all its similar embodiment should be covered by the protection domain of patent of the present invention.
Claims (1)
1. the improvement waste residue of sulfate cinder prepares the method for water glass and hydrophobic silica, it is characterized in that comprising the steps:
The primary emission waste residue that sulfate cinder is administered was with 10～15% hydrochloric acid soln repetitive scrubbing 20～30 minutes, and the filter cake after the filtration washs three times with clear water, made pH value reach 6～7 and filtered stand-byly again, obtained pure filter cake; Acid filtrate washing capable of circulation is used, and pollutes to save cost and to prevent; Acid clear water washing lotion can be blent the hydrochloric acid washings, and remainder reasonably discharges by basic treatment;
The pure filter cake and the liquid sodium hydroxide of above-mentioned acquisition are mixed in the steam-heated pressure reactor with pure mass ratio 1:1.13～1.53, start steam heating, stop to feed open steam after making reaction pressure reach 0.7～0.8Mpa,, and kept this pressure 3～8 hours with the jacket steam insulation; Afterwards the sodium silicate solution that forms is filtered, obtains the filter cake elemental sulfur, through washing, dry, pulverize, be packaged to be the elemental sulfur product; The sodium silicate liquid that obtains is concentrated, cools off through light again, obtain the water glass liquid product;
With the water glass liquid diluting and the purification of above-mentioned acquisition, carry out ion-exchange, remove sodium ion, adding hydrochloric acid then carries out acid heat and reflux to concentrate, add the dimethyldichlorosilane(DMCS) solvent monomer and carry out hydrophobic treatment, deviate from solvent, drying makes the hydrophobic silica product.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59121116A (en) * | 1982-12-27 | 1984-07-13 | Tokuyama Soda Co Ltd | Production of sodium silicate |
| CN101214963A (en) * | 2008-01-02 | 2008-07-09 | 吉林大学 | Method for preparing high pure nano silicon dioxide from oil shale slag |
| CN101234763A (en) * | 2008-02-18 | 2008-08-06 | 周华明 | Method for preparing sodium silicate and sodium metasilicate from white residue |
| CN101279738A (en) * | 2008-05-12 | 2008-10-08 | 崔国强 | Method for preparing liquid sodium silicate by one-step liquid phase reaction |
| CN101538046A (en) * | 2009-03-10 | 2009-09-23 | 大连工业大学 | Method for simultaneously preparing SiO2 aerogel and zeolite by utilizing fly ash |
-
2010
- 2010-12-15 CN CN 201010588748 patent/CN102153099A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59121116A (en) * | 1982-12-27 | 1984-07-13 | Tokuyama Soda Co Ltd | Production of sodium silicate |
| CN101214963A (en) * | 2008-01-02 | 2008-07-09 | 吉林大学 | Method for preparing high pure nano silicon dioxide from oil shale slag |
| CN101234763A (en) * | 2008-02-18 | 2008-08-06 | 周华明 | Method for preparing sodium silicate and sodium metasilicate from white residue |
| CN101279738A (en) * | 2008-05-12 | 2008-10-08 | 崔国强 | Method for preparing liquid sodium silicate by one-step liquid phase reaction |
| CN101538046A (en) * | 2009-03-10 | 2009-09-23 | 大连工业大学 | Method for simultaneously preparing SiO2 aerogel and zeolite by utilizing fly ash |
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Application publication date: 20110817 |