CN102153098A - Method for preparing water glass and macroporous spherical silica gel from treatment waste residues of sulfuric acid cinder - Google Patents
Method for preparing water glass and macroporous spherical silica gel from treatment waste residues of sulfuric acid cinder Download PDFInfo
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- CN102153098A CN102153098A CN 201010588718 CN201010588718A CN102153098A CN 102153098 A CN102153098 A CN 102153098A CN 201010588718 CN201010588718 CN 201010588718 CN 201010588718 A CN201010588718 A CN 201010588718A CN 102153098 A CN102153098 A CN 102153098A
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Abstract
The invention relates to a method for preparing water glass and macroporous spherical silica gel from treatment waste residues of sulfuric acid cinder, which comprises the following steps of: repeatedly washing primary discharge waste residues of sulfuric acid cinder treatment for 20-30 min by using a 10-15% hydrochloric acid solution, washing filter cakes after filtration by using clean water three times, and filtering the filter cakes to obtain clean filter cakes; mixing the clean filter cakes and liquid sodium hydroxide according to the mass ratio of 1:(1.13-1.53) in a steam-heated pressure reactor to react; filtering a formed sodium silicate solution, and lightly concentrating and cooling the sodium silicate liquid to obtain a water glass liquid product; and diluting the water glass liquid, mixing the diluted water glass liquid with dilute sulphuric acid, gelatinizing into spheres, aging for 6 h, washing the spheres by using 50-65 DEG C warm water, immersing the spheres in 0.15-0.2% ammonia water for 6 h, and drying to obtain the macroporous spherical silica gel. In the invention, the water glass and the macroporous spherical silica gel are prepared by using the treatment waste residues of sulfuric acid cinder as raw materials, the waste is changed into the valuable, and a significant 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 gross porosity spherical silica-gel 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 gross porosity spherical silica-gel.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 gross porosity spherical silica-gel provide a kind of and prepare the method for water glass and gross porosity spherical silica-gel 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 gross porosity spherical silica-gel, 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;
The water glass liquid dilute with water of above-mentioned acquisition is mixed with dilute sulphuric acid, be when temperature is 20～30 ℃, to carry out the gelling ball under 5～8 the environment at pH value, aging 6 hours, warm water washing with 50～65 ℃, used 0.15～0.2% ammoniacal liquor immersion treatment again 6 hours, and, soaked after dry for the first time to moisture content and be less than or equal to 10% to enlarge the glueballs aperture, screening back is dried to moisture content and be less than or equal to 2% for the second time, makes the gross porosity spherical silica-gel.
Its chemical equation is as follows: SiO2+2NaOH====Na2SiO3+H2O
Na2SiO3+?H2SO4====Na2SO4+?+SiO2+?H2O
The invention has the beneficial effects as follows: one, the invention provides a kind of method for preparing water glass and gross porosity spherical silica-gel 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 gross porosity spherical silica-gel are prepared in comprehensive utilization.Its two, water glass and gross porosity spherical silica-gel 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 the gross porosity spherical silica-gel 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 gross porosity spherical silica-gel 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 gross porosity spherical silica-gel 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;
The water glass liquid dilute with water of above-mentioned acquisition is mixed with dilute sulphuric acid, be when temperature is 20～30 ℃, to carry out the gelling ball under 5～8 the environment at pH value, aging 6 hours, warm water washing with 50～65 ℃, used 0.15～0.2% ammoniacal liquor immersion treatment again 6 hours, and, soaked after dry for the first time to moisture content and be less than or equal to 10% to enlarge the glueballs aperture, screening back is dried to moisture content and be less than or equal to 2% for the second time, makes 231.6 kilograms of gross porosity spherical silica-gels.
Embodiment 2, and present embodiment is described a kind ofly to prepare the method for water glass and gross porosity spherical silica-gel 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 gross porosity spherical silica-gel 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;
The water glass liquid dilute with water of above-mentioned acquisition is mixed with dilute sulphuric acid, be when temperature is 20～30 ℃, to carry out the gelling ball under 5～8 the environment at pH value, aging 6 hours, warm water washing with 50～65 ℃, used 0.15～0.2% ammoniacal liquor immersion treatment again 6 hours, and, soaked after dry for the first time to moisture content and be less than or equal to 10% to enlarge the glueballs aperture, screening back is dried to moisture content and be less than or equal to 2% for the second time, makes 266.5 kilograms of gross porosity spherical silica-gels.
Embodiment 3, and present embodiment is described a kind ofly to prepare the method for water glass and gross porosity spherical silica-gel 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 gross porosity spherical silica-gel 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;
The water glass liquid dilute with water of above-mentioned acquisition is mixed with dilute sulphuric acid, be when temperature is 20～30 ℃, to carry out the gelling ball under 5～8 the environment at pH value, aging 6 hours, warm water washing with 50～65 ℃, used 0.15～0.2% ammoniacal liquor immersion treatment again 6 hours, and, soaked after dry for the first time to moisture content and be less than or equal to 10% to enlarge the glueballs aperture, screening back is dried to moisture content and be less than or equal to 2% for the second time, makes 196.9 kilograms of gross porosity spherical silica-gels.
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 gross porosity spherical silica-gel, 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;
The water glass liquid dilute with water of above-mentioned acquisition is mixed with dilute sulphuric acid, be when temperature is 20～30 ℃, to carry out the gelling ball under 5～8 the environment at pH value, aging 6 hours, warm water washing with 50～65 ℃, used 0.15～0.2% ammoniacal liquor immersion treatment again 6 hours, and, soaked after dry for the first time to moisture content and be less than or equal to 10% to enlarge the glueballs aperture, screening back is dried to moisture content and be less than or equal to 2% for the second time, makes the gross porosity spherical silica-gel.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090022646A1 (en) * | 2007-07-20 | 2009-01-22 | The Titanium Dioxide Co. Ltd. (Cristal) | Process for hydrothermal production of sodium silicate solutions and precipitated silicas |
| CN101654737A (en) * | 2008-12-19 | 2010-02-24 | 河南德海源诚矿业有限公司 | Compound iron ore pellet of molybdenum tailings and sulfate slags and preparation method thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090022646A1 (en) * | 2007-07-20 | 2009-01-22 | The Titanium Dioxide Co. Ltd. (Cristal) | Process for hydrothermal production of sodium silicate solutions and precipitated silicas |
| CN101654737A (en) * | 2008-12-19 | 2010-02-24 | 河南德海源诚矿业有限公司 | Compound iron ore pellet of molybdenum tailings and sulfate slags and preparation method thereof |
Non-Patent Citations (3)
| Title |
|---|
| 《天津化工》 20070531 朱红，等 硫铁矿烧渣在环境治理中的应用 第24-26页 1 第21卷, 第3期 * |
| 《有色矿冶》 20080831 富维俊，等 硫酸烧渣再回收铁试验研究 第24-27页 1 第24卷, 第4期 * |
| 《有色矿冶》 20100227 马涌，等 硫酸烧渣的综合利用研究 第24-27页 1 第26卷, 第1期 * |
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Application publication date: 20110817 |