CN102153100A - Method for preparing water glass and electronic silicon dioxide from treatment waste residues of sulfuric acid slags - Google Patents
Method for preparing water glass and electronic silicon dioxide from treatment waste residues of sulfuric acid slags Download PDFInfo
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- CN102153100A CN102153100A CN 201010589466 CN201010589466A CN102153100A CN 102153100 A CN102153100 A CN 102153100A CN 201010589466 CN201010589466 CN 201010589466 CN 201010589466 A CN201010589466 A CN 201010589466A CN 102153100 A CN102153100 A CN 102153100A
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- water glass
- silicon dioxide
- filter cake
- washing
- sulfuric acid
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Abstract
The invention discloses a method for preparing water glass and electronic silicon dioxide from treatment waste residues of sulfuric acid slags and relates to comprehensive treatment and utilization of sulfuric acid inorganic industrial emission. The method comprises the following steps of: washing the treatment waste residues of the sulfuric acid slags by solution of hydrochloric acid, filtering to obtain a filter cake and washing the filter cake by clear water for later use; blending cleaning solution of hydrochloric acid which can be used for washing circularly by acid clear water washing liquor; mixing the obtained filter cake and liquid sodium hydroxide in a pressure reactor heated by steam to perform a reaction; then filtering formed sodium silicate solution to obtain a filter cake elemental sulfur product; carrying out light concentration, cooling and packaging on the obtained sodium silicate liquid to obtain a liquid product of a water glass adhesive; then performing a reaction of the water glass solution and nitric acid to generate silicon dioxide; and carrying out poaching, pickling, deionized water washing and dehydration on the silicon dioxide to obtain the electronic silicon dioxide product. With the adoption of the method, after the treatment waste residues of the sulfuric acid slags are firstly processed, higher economic benefits are generated.
Description
Technical field
The invention belongs to the technical field of the comprehensive regulation and the utilization of the inorganic industrial discharge of sulfuric acid, especially a kind of processing waste residue of sulfate cinder prepares the method for water glass and electronic grade silicon dioxide.
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 several operations such as raw material roasting, purification, conversion and absorptions.With the purification process flow process, gas washing in SA production is divided into dry method and wet method two big classes on the general custom.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 to be used for ironmaking, extracts the raw material of non-ferrous metal and manufacturing material of construction.
The burning slag quantity discharged of unit sulfuric acid product is relevant with the grade and the processing condition of sulfurous iron ore.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 the 0.7-1 ton approximately per ton.Wherein the various compositions of sulfate cinder and percentage composition are: Z 250 content is 43.31%, 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%.
Sulfate cinder has extracted Z 250, aluminium sesquioxide, calcium oxide, magnesium oxide, silicon oxide, elemental sulfur element etc. after by the salt acid purification, forms that remaining acid non-soluble substance is silicon-dioxide and elemental sulfur behind the various metal-salts.
Secondary residue after one, sulfate cinder are administered does not only effectively utilize, and can cause secondary pollution.
Two, water glass can be used for being coated with brush material, can improve the weathering resistance ability; Also can be used for reinforcing soil, preparation rapid hardening water-resisting agent, prepare fields such as acidproof gelling, acid resisting mortar and acid resisting concrete and antiseptic project application; Electronic grade silicon dioxide can be used as the strengthening agent of rubber, the anti-sedimentation agent that prevents the agent of plastics film agglutinating opening, pigment, coating matting agent, viscosity-controlling agent, medicine vehicle, support of the catalyst and be used for makeup etc.
Summary of the invention
The utilization once more of the waste residue after the present invention is intended to administer for the first time at sulfate cinder and meeting the need of market provides a kind of improvement waste residue of sulfate cinder to prepare the method for water glass and electronic grade silicon dioxide.
For achieving the above object, a kind of to prepare sulfate cinder with chemical method be that the technical scheme of phosphatic method is as follows in the present invention:
The improvement waste residue of sulfate cinder prepares the method for water glass and electronic grade silicon dioxide, will administer waste residue the first time of sulfate cinder by pickling, conversion, purifying process, makes water glass and electronic grade silicon dioxide product:
Described acid cleaning process is: waste residue silicon-dioxide that sulfate cinder is discharged after treatment and elemental sulfur be with the hydrochloric acid soln repetitive scrubbing of 10-15% 20-30 minute, and the filter cake after the filtration makes pH value reach 6-7 three times with the clear water washing to filter stand-by again; Acid clear water washing lotion is blent the hydrochloric acid washings, and washing capable of circulation is used, and remainder discharges by basic treatment;
Described conversion process is: the above-mentioned pure filter cake that obtains is mixed in the steam-heated pressure reactor with pure mass ratio 1:1.13-1.53 by silicon-dioxide and liquid sodium hydroxide, start after steam heating makes reaction pressure reach 0.7-0.8Mpa, stop to feed open steam, with jacket steam insulation and kept this pressure 3-8 hour; Afterwards the sodium silicate solution that forms is filtered obtain the filter cake elemental sulfur through wash drying, crushing packing obtains the elemental sulfur product; The sodium silicate liquid that obtains is again through gently concentrating, cool off, be packaged to be the liquid product of water glass adhesive;
Described purifying process is: above-mentioned water glass solution and nitric acid are generated silicon-dioxide with pure mass ratio 1:0.83-1.23 reaction, make the electronic grade silicon dioxide product through rinsing, pickling, deionized water washing, dehydration.
Further, described sulfate cinder contains Z 250, aluminium sesquioxide, calcium oxide, magnesium oxide, silicon oxide and sulphur in its component.
Main chemical reactions formula of the present invention is:
SiO
2+2NaOH====Na
2SiO
3+H
2O
Na
2SiO
3+?2HNO
3====2NaNO
3+H
2SiO
3
H
2SiO
3====?SiO
2+H
2O
Beneficial effect of the present invention is: one, and provide a kind of improvement waste residue of sulfate cinder to prepare the method for water glass and electronic grade silicon dioxide, can avoid the secondary pollution of sulfuric acid industry; Its two, the silicon series product of producing serve many purposes, economic benefit is considerable; Its three, the acid filtrate that produces in process washing capable of circulation is used to save cost and to prevent and is polluted.
Embodiment
Embodiment one
The improvement waste residue of sulfate cinder prepares the method for water glass and electronic grade silicon dioxide, to administer waste residue the first time of sulfate cinder by pickling, conversion, purifying process, make water glass and electronic grade silicon dioxide product, the various compositions of used sulfate cinder and percentage composition are 43.31% for Z 250 content, aluminium sesquioxide content is 8.13%, and calcium oxide content is 1.63%, and content of magnesia is 0.46%, silica content is 35.73%, and the content of sulphur is 0.16%.
Described acid cleaning process is: 500Kg waste residue silicon-dioxide that sulfate cinder is discharged after treatment and elemental sulfur be with the hydrochloric acid soln repetitive scrubbing of 10-15% 20-30 minute, and the filter cake after the filtration makes pH value reach 6-7 three times with the clear water washing to filter stand-by again; Acid clear water washing lotion is blent the hydrochloric acid washings, and washing capable of circulation is used, and remainder discharges by basic treatment;
Described conversion process is: the above-mentioned pure filter cake that obtains is mixed in the steam-heated pressure reactor with pure mass ratio 1:1.13 by silicon-dioxide and liquid sodium hydroxide, start after steam heating makes reaction pressure reach 0.7-0.8Mpa, stop to feed open steam, with jacket steam insulation and kept this pressure 3-8 hour; Afterwards the sodium silicate solution that forms is filtered obtain the filter cake elemental sulfur through wash drying, crushing packing obtains the elemental sulfur product; The sodium silicate liquid that obtains is again through gently concentrating, cool off, be packaged to be the liquid product of 858Kg water glass adhesive;
Described purifying process is: above-mentioned water glass solution and nitric acid are generated silicon-dioxide with pure mass ratio 1:0.83 reaction, make 340Kg electronic grade silicon dioxide product through rinsing, pickling, deionized water washing, dehydration.
Embodiment two
The improvement waste residue of sulfate cinder prepares the method for water glass and electronic grade silicon dioxide, to administer waste residue the first time of sulfate cinder by pickling, conversion, purifying process, make water glass and electronic grade silicon dioxide product, the various compositions of used sulfate cinder and percentage composition are 43.31% for Z 250 content, aluminium sesquioxide content is 8.13%, and calcium oxide content is 1.63%, and content of magnesia is 0.46%, silica content is 35.73%, and the content of sulphur is 0.16%.
Described acid cleaning process is: 500Kg waste residue silicon-dioxide that sulfate cinder is discharged after treatment and elemental sulfur be with the hydrochloric acid soln repetitive scrubbing of 10-15% 20-30 minute, and the filter cake after the filtration makes pH value reach 6-7 three times with the clear water washing to filter stand-by again; Acid clear water washing lotion is blent the hydrochloric acid washings, and washing capable of circulation is used, and remainder discharges by basic treatment;
Described conversion process is: the above-mentioned pure filter cake that obtains is mixed in the steam-heated pressure reactor with pure mass ratio 1:1.33 by silicon-dioxide and liquid sodium hydroxide, start after steam heating makes reaction pressure reach 0.7-0.8Mpa, stop to feed open steam, with jacket steam insulation and kept this pressure 3-8 hour; Afterwards the sodium silicate solution that forms is filtered obtain the filter cake elemental sulfur through wash drying, crushing packing obtains the elemental sulfur product; The sodium silicate liquid that obtains is again through gently concentrating, cool off, be packaged to be the liquid product of 1009Kg water glass adhesive;
Described purifying process is: above-mentioned water glass solution and nitric acid are generated silicon-dioxide with pure mass ratio 1:1.03 reaction, make 495Kg electronic grade silicon dioxide product through rinsing, pickling, deionized water washing, dehydration.
Embodiment three
The improvement waste residue of sulfate cinder prepares the method for water glass and electronic grade silicon dioxide, to administer waste residue the first time of sulfate cinder by pickling, conversion, purifying process, make water glass and electronic grade silicon dioxide product, the various compositions of used sulfate cinder and percentage composition are 43.31% for Z 250 content, aluminium sesquioxide content is 8.13%, and calcium oxide content is 1.63%, and content of magnesia is 0.46%, silica content is 35.73%, and the content of sulphur is 0.16%.
Described acid cleaning process is: 500Kg waste residue silicon-dioxide that sulfate cinder is discharged after treatment and elemental sulfur be with the hydrochloric acid soln repetitive scrubbing of 10-15% 20-30 minute, and the filter cake after the filtration makes pH value reach 6-7 three times with the clear water washing to filter stand-by again; Acid clear water washing lotion is blent the hydrochloric acid washings, and washing capable of circulation is used, and remainder discharges by basic treatment;
Described conversion process is: the above-mentioned pure filter cake that obtains is mixed in the steam-heated pressure reactor with pure mass ratio 1:1.53 by silicon-dioxide and liquid sodium hydroxide, start after steam heating makes reaction pressure reach 0.7-0.8Mpa, stop to feed open steam, with jacket steam insulation and kept this pressure 3-8 hour; Afterwards the sodium silicate solution that forms is filtered obtain the filter cake elemental sulfur through wash drying, crushing packing obtains the elemental sulfur product; The sodium silicate liquid that obtains is again through gently concentrating, cool off, be packaged to be the liquid product of 1161Kg water glass adhesive;
Described purifying process is: above-mentioned water glass solution and nitric acid are generated silicon-dioxide with pure mass ratio 1:1.23 reaction, make 680Kg electronic grade silicon dioxide product through rinsing, pickling, deionized water washing, dehydration.
Claims (2)
1. the improvement waste residue of sulfate cinder prepares the method for water glass and electronic grade silicon dioxide, it is characterized in that: administer waste residue the first time of sulfate cinder by pickling, conversion, purifying process, make water glass and electronic grade silicon dioxide product:
Described acid cleaning process is: waste residue silicon-dioxide that sulfate cinder is discharged after treatment and elemental sulfur be with the hydrochloric acid soln repetitive scrubbing of 10-15% 20-30 minute, and the filter cake after the filtration makes pH value reach 6-7 three times with the clear water washing to filter stand-by again; Acid clear water washing lotion is blent the hydrochloric acid washings, and washing capable of circulation is used, and remainder discharges by basic treatment;
Described conversion process is: the above-mentioned pure filter cake that obtains is mixed in the steam-heated pressure reactor with pure mass ratio 1:1.13-1.53 by silicon-dioxide and liquid sodium hydroxide, start after steam heating makes reaction pressure reach 0.7-0.8Mpa, stop to feed open steam, with jacket steam insulation and kept this pressure 3-8 hour; Afterwards the sodium silicate solution that forms is filtered obtain the filter cake elemental sulfur through wash drying, crushing packing obtains the elemental sulfur product; The sodium silicate liquid that obtains is again through gently concentrating, cool off, be packaged to be the liquid product of water glass adhesive;
Described purifying process is: above-mentioned water glass solution and nitric acid are generated silicon-dioxide with pure mass ratio 1:0.83-1.23 reaction, make the electronic grade silicon dioxide product through rinsing, pickling, deionized water washing, dehydration.
2. the improvement waste residue of sulfate cinder according to claim 1 prepares the method for water glass and electronic grade silicon dioxide, it is characterized in that: described sulfate cinder, contain Z 250, aluminium sesquioxide, calcium oxide, magnesium oxide, silicon oxide and sulphur in its component.
Priority Applications (1)
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|---|---|---|---|
| CN 201010589466 CN102153100A (en) | 2010-12-15 | 2010-12-15 | Method for preparing water glass and electronic silicon dioxide from treatment waste residues of sulfuric acid slags |
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| CN 201010589466 CN102153100A (en) | 2010-12-15 | 2010-12-15 | Method for preparing water glass and electronic silicon dioxide from treatment waste residues of sulfuric acid slags |
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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 201010589466 patent/CN102153100A/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 |