CN102180471A - Method for preparing waterglass and microporous massive silica gel from treated waste residue of sulphuric acid cinder - Google Patents
Method for preparing waterglass and microporous massive silica gel from treated waste residue of sulphuric acid cinder Download PDFInfo
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- CN102180471A CN102180471A CN2010106161653A CN201010616165A CN102180471A CN 102180471 A CN102180471 A CN 102180471A CN 2010106161653 A CN2010106161653 A CN 2010106161653A CN 201010616165 A CN201010616165 A CN 201010616165A CN 102180471 A CN102180471 A CN 102180471A
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- filter cake
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Abstract
The invention relates to a method for preparing waterglass and microporous massive silica gel from treated waste residue of sulphuric acid cinder, which comprises the following steps of: repeatedly washing the treated primary discharge waste residue of the sulphuric acid cinder for 20-30 minutes by using a 10-15% hydrochloric acid solution, and washing a filtered filter cake for three times by using clean water so as to obtain a pure filter cake; mixing the pure filter cake with liquid sodium hydroxide in a pressure reactor heated by vapor in a for pure mass ratio of 1: (1.13-1.53) for reacting; filtering a formed sodium silicate solution, and lightly concentrating and cooling the sodium silicate solution to obtain the product of the waterglass liquid; and diluting the waterglass liquid with water and mixing with dilute sulphuric acid, gelling at a temperature of 20-30 DEG C, soaking in a dilute sulphuric acid solution for 3-5 hours, then taking out, washing by using warm water with a temperature of 55 DEG C, filtering gel, and drying so as to obtain the microporous massive silica gel. In the method, the waterglass and the microporous massive silica gel are prepared by using the treated waste residue of the sulphuric acid cinder as a raw material, so that 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 pore block 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 pore block 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 pore block silica gel provide a kind of and prepare the method for water glass and pore block 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 pore block 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 gel forming under 5～8 the environment at pH value, place 0.016～0.02% dilution heat of sulfuric acid to soak 3～5 hours then in 25～30 ℃ temperature, acid content reaches till 0.01～0.015 in gel, warm water with 55 ℃ after taking out washs, drags for glue, be less than or equal to 10%, screening through for the first time drying to moisture content; Dry for the second time to moisture content and be less than or equal to 2%, make the pore block silica gel.
Its chemical equation is as follows: SiO
2+ 2NaOH====Na
2SiO
3+ H
2O
Na
2SiO
3+H
2SO
4＝＝＝＝Na
2SO
4++SiO
2+H
2O
The invention has the beneficial effects as follows: one, the invention provides a kind of method for preparing water glass and pore block 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 pore block silica gel are prepared in comprehensive utilization.Its two, water glass and pore block 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 pore block 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 pore block 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 pore block 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 with liquid sodium hydroxide at 1: 1.33, 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 gel forming under 5～8 the environment at pH value, place 0.016～0.02% dilution heat of sulfuric acid to soak 3～5 hours then in 25～30 ℃ temperature, acid content reaches till 0.01～0.015 in gel, warm water with 55 ℃ after taking out washs, drags for glue, be less than or equal to 10%, screening through for the first time drying to moisture content; Dry for the second time to moisture content and be less than or equal to 2%, make 231.6 kilograms of pore block silica gels.
Embodiment 2, and present embodiment is described a kind ofly to prepare the method for water glass and pore block 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 pore block 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 with liquid sodium hydroxide at 1: 1.53, 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 gel forming under 5～8 the environment at pH value, place 0.016～0.02% dilution heat of sulfuric acid to soak 3～5 hours then in 25～30 ℃ temperature, acid content reaches till 0.01～0.015 in gel, warm water with 55 ℃ after taking out washs, drags for glue, be less than or equal to 10%, screening through for the first time drying to moisture content; Dry for the second time to moisture content and be less than or equal to 2%, make 266.5 kilograms of pore block silica gels.
Embodiment 3, and present embodiment is described a kind ofly to prepare the method for water glass and pore block 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 pore block 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 with liquid sodium hydroxide at 1: 1.13, 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 gel forming under 5～8 the environment at pH value, place 0.016～0.02% dilution heat of sulfuric acid to soak 3～5 hours then in 25～30 ℃ temperature, acid content reaches till 0.01～0.015 in gel, warm water with 55 ℃ after taking out washs, drags for glue, be less than or equal to 10%, screening through for the first time drying to moisture content; Dry for the second time to moisture content and be less than or equal to 2%, make 196.9 kilograms of pore block 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 pore block 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, 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 gel forming under 5～8 the environment at pH value, place 0.016～0.02% dilution heat of sulfuric acid to soak 3～5 hours then in 25～30 ℃ temperature, acid content reaches till 0.01～0.015 in gel, warm water with 55 ℃ after taking out washs, drags for glue, be less than or equal to 10%, screening through for the first time drying to moisture content; Dry for the second time to moisture content and be less than or equal to 2%, make the pore block silica gel.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102642848A (en) * | 2012-04-19 | 2012-08-22 | 宫毅 | Comprehensive utilization method of acid sludge generated in acid making by smelting fume |
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2010
- 2010-12-19 CN CN2010106161653A patent/CN102180471A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102642848A (en) * | 2012-04-19 | 2012-08-22 | 宫毅 | Comprehensive utilization method of acid sludge generated in acid making by smelting fume |
| CN102642848B (en) * | 2012-04-19 | 2014-03-12 | 宫毅 | Comprehensive utilization method of acid sludge generated in acid making by smelting fume |
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Application publication date: 20110914 |