CN105439157A - Method for producing water glass and fine-pore massive silica gel by using pyrite cinders - Google Patents

Method for producing water glass and fine-pore massive silica gel by using pyrite cinders Download PDF

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Publication number
CN105439157A
CN105439157A CN201410538195.5A CN201410538195A CN105439157A CN 105439157 A CN105439157 A CN 105439157A CN 201410538195 A CN201410538195 A CN 201410538195A CN 105439157 A CN105439157 A CN 105439157A
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water glass
gel
filter cake
silica gel
acid
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CN201410538195.5A
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徐联菊
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CHANGDE XIANGDA ENVIRONMENTAL PROTECTION AND TECHNOLOGY Co Ltd
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CHANGDE XIANGDA ENVIRONMENTAL PROTECTION AND TECHNOLOGY Co Ltd
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Abstract

The invention provides a method for producing water glass and a fine-pore massive silica gel by using pyrite cinders. The method comprises the following steps of: repeatedly washing primarily discharged residues in pyrite cinder treatment with a 9-16% hydrochloric acid solution for 19-32 minutes, filtering to obtain a filter cake; washing the filter cake with clean water for three times; filtering to obtian a pure filter cake; mixing the pure filter cake with liquid sodium hydroxide in a pure mass ratio of 1: (1.12-1.55) in a steam heated pressure reactor for reaction; filtering the formed sodium silicate solution, and lightly condensing and cooling the sodium silicate solution to obtain a water glass liquid product; and diluting the water glass liquid with water and mixing the water glass liquid with dilute sulphuric acid, performing gel formation at 21-32 DEG C, soaking the gel in a dilute sulphuric acid solution for 3-5 hours, taking out the gel, and washing the gel by 55 DEG C warm water, fishing the gel, and drying the gel to obtain the fine-pore massive silica gel. The method, which prepares the water glass and fine-pore massive silica gel by taking treatment residues of pyrite cinders as raw materials, turns waste into wealth, thereby creating a considerable economic benefit.

Description

A kind of method utilizing sulfate cinder to produce water glass and pore block silica gel
Technical field
The present invention relates to the comprehensive regulation of sulfuric acid inorganic industrial discharge and the technical field of utilization, particularly relate to a kind of method utilizing sulfate cinder to produce water glass and pore block silica gel.
Background technology
Sulfuric acid industry take sulfurous iron ore as the sulfuric acid that contact raw method is produced, primarily of raw material, roasting, purification, conversion and absorption five operation compositions.With purification process flow process in general custom, be divided into dry method and the large class of wet method two through gas washing in SA production.Wet purification has again pickling, hot concentrated acid is washed and washed point.Pyrite-based sulfuric acid production minority factory of current China is pickling process, and majority is still washing process.
Sulfurous iron ore forms, with a small amount of non-ferrous metal and rare metal primarily of sulphur and iron.Pyrite cinder is the residue of discharging after pyrite burning extracts sulphur.In sulfurous iron ore except sulphur is utilized, iron and other elements are still stayed in slag.Slag is used to the raw material smelting iron, extract non-ferrous metal and manufacture material of construction.
The quantity discharged of unit sulfuric acid product is relevant with the grade of sulfurous iron ore and processing condition.Under identical processing condition, the higher then bed drain purge of the grade of sulfurous iron ore is fewer, otherwise then high.When sulfurous iron ore sulphur content is 25 ~ 35%, the general production clinker about producing 0.7 ~ 1 ton per ton.The percentage composition of the various compositions of sulfate cinder is Z 250 content is below 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%.
In a series of inventions such as " prepare sulfate cinder are muriatic method with chemical method ", by being extracted Z 250, aluminium sesquioxide, calcium oxide, magnesium oxide, silicon oxide, elemental sulfur element etc. after salt acid purification, acid non-soluble substance remaining after forming various metal-salt is silicon-dioxide and elemental sulfur.The present invention is exactly the method utilizing the process waste residue of sulfate cinder to prepare water glass and pore block silica gel.This method is the patented invention that the typical disposal of three wastes derives, and its object is exactly the various material inside the three wastes and element will be eaten dry deep-frying only all to use.By the decomposition residue contamination source of several level, in the hope of the secondary of the minimizing chemical industry three wastes or the exhaust emission of three times of maximum possible.
Summary of the invention
Technical problem to be solved by this invention is; the improvement waste residue of sulfate cinder is processed; comprehensive utilization; prepare water glass and pore block silica gel, provide a kind of method utilizing sulfate cinder to produce water glass and pore block silica gel, the method effectively avoids the secondary pollution of sulfuric acid industry; find in primary emission potentiality to eat dry deep-frying clean, turn waste into wealth; finally become valuable silicon series product, create considerable economic benefit, protect environment.
The technical solution adopted for the present invention to solve the technical problems is: a kind of method utilizing sulfate cinder to produce water glass and pore block silica gel, comprises the steps:
The primary emission waste residue (being mainly the acid non-soluble substance such as silicon-dioxide and elemental sulfur) that sulfate cinder is administered with 9 ~ 16% hydrochloric acid soln repetitive scrubbing 19 ~ 32 minutes, filter cake clear water after filtration washs three times, making pH value reach 6 ~ 7 filters stand-by again, obtains pure filter cake; Acid filtrate washing capable of circulation uses, to save cost and preventing pollution; Acid clear water washing lotion can blend hydrochloric acid washings, and remainder is reasonably discharged by basic treatment;
The pure filter cake (silicon-dioxide meter) of above-mentioned acquisition and liquid sodium hydroxide are mixed in steam-heated pressure reactor with pure mass ratio 1: 1.12 ~ 1.55, start steam heating, stop after making reaction pressure reach 0.6 ~ 0.9Mpa passing into open steam, with jacket steam insulation, and maintain this pressure 4 ~ 9 hours; The sodium silicate solution that will be formed afterwards filters, and obtains filter cake elemental sulfur, through washing, dry, pulverize, be packaged to be elemental sulfur product; By the sodium silicate liquid obtained again through gently concentrating, cooling, obtain 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 21 ~ 32 DEG C, carry out gel forming under the environment of 5 ~ 8 at pH value, then the dilution heat of sulfuric acid being placed in 0.017 ~ 0.021% soaks 3 ~ 5 hours in the temperature of 26 ~ 32 DEG C, in gel, acid content reaches till 0.011 ~ 0.016, wash with the warm water of 55 DEG C, drag for glue after taking out, dry through first time and be less than or equal to 10% to moisture content, screen; Second time is dried and is less than or equal to 2% to moisture content, obtains pore block silica gel.
Main chemical reactions equation of the present invention 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 utilizing sulfate cinder to produce water glass and pore block silica gel, the method effectively make use of the material composition of the improvement waste residue of sulfate cinder, the improvement waste residue of sulfate cinder is processed, comprehensive utilization, prepares water glass and pore block silica gel.Its two, water glass and pore block silica gel purposes are wide, are the products that two kinds of economic worths are larger, and improve the economic benefit of the improvement waste residue of process sulfate cinder, creating very large profit return, is the model of the chemical industry comprehensive regulation and utilization.Its three, less investment, prepares water glass and pore block silica gel is particularly applicable to the improvement waste residue of process sulfate cinder, opens a Tiao Xin road.Its four, the purity of preparation is high, and quality is guaranteed.Its five, the method effectively avoids the secondary pollution of sulfuric acid industry, find in primary emission potentiality to eat dry deep-frying clean, turn waste into wealth, finally become valuable silicon series product, create considerable economic benefit.
Embodiment
Embodiment one, a kind of method utilizing sulfate cinder to produce water glass and pore block silica gel described in the present embodiment, comprises the steps:
Get silica content be 35.73% sulfate cinder administer 500 kilograms, primary emission waste residue prepare water glass and pore block silica gel, the primary emission waste residue (being mainly the acid non-soluble substance such as silicon-dioxide and elemental sulfur) that sulfate cinder is administered with 9 ~ 16% hydrochloric acid soln repetitive scrubbing 19 ~ 32 minutes, filter cake clear water after filtration washs three times, making pH value reach 6 ~ 7 filters stand-by again, obtains pure filter cake; Acid filtrate washing capable of circulation uses, to save cost and preventing pollution; Acid clear water washing lotion can blend hydrochloric acid washings, and remainder is reasonably discharged by basic treatment;
The pure filter cake (silicon-dioxide meter) of above-mentioned acquisition and liquid sodium hydroxide are mixed in steam-heated pressure reactor with pure mass ratio 1: 1.33, start steam heating, stop after making reaction pressure reach 0.6 ~ 0.9Mpa passing into open steam, with jacket steam insulation, and maintain this pressure 4 ~ 9 hours; The sodium silicate solution that will be formed afterwards filters, and obtains filter cake elemental sulfur, through washing, dry, pulverize, be packaged to be elemental sulfur product; By the sodium silicate liquid obtained again through gently concentrating, cooling, 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 21 ~ 32 DEG C, carry out gel forming under the environment of 5 ~ 8 at pH value, then the dilution heat of sulfuric acid being placed in 0.017 ~ 0.021% soaks 3 ~ 5 hours in the temperature of 26 ~ 32 DEG C, in gel, acid content reaches till 0.011 ~ 0.016, wash with the warm water of 55 DEG C, drag for glue after taking out, dry through first time and be less than or equal to 10% to moisture content, screen; Second time is dried and is less than or equal to 2% to moisture content, obtains 231.6 kilograms of pore block silica gels.
Embodiment two, a kind of method utilizing sulfate cinder to produce water glass and pore block silica gel described in the present embodiment, comprises the steps:
Get silica content be 35.73% sulfate cinder administer 500 kilograms, primary emission waste residue prepare water glass and pore block silica gel, the primary emission waste residue (being mainly the acid non-soluble substance such as silicon-dioxide and elemental sulfur) that sulfate cinder is administered with 9 ~ 16% hydrochloric acid soln repetitive scrubbing 19 ~ 32 minutes, filter cake clear water after filtration washs three times, making pH value reach 6 ~ 7 filters stand-by again, obtains pure filter cake; Acid filtrate washing capable of circulation uses, to save cost and preventing pollution; Acid clear water method liquid can blend hydrochloric acid washings, and remainder is reasonably discharged by basic treatment;
The pure filter cake (silicon-dioxide meter) of above-mentioned acquisition and liquid sodium hydroxide are mixed in steam-heated pressure reactor with pure mass ratio 1: 1.53, start steam heating, stop after making reaction pressure reach 0.6 ~ 0.9Mpa passing into open steam, with jacket steam insulation, and maintain this pressure 4 ~ 9 hours; The sodium silicate solution that will be formed afterwards filters, and obtains filter cake elemental sulfur, through washing, dry, pulverize, be packaged to be elemental sulfur product; By the sodium silicate liquid obtained again through gently concentrating, cooling, 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 21 ~ 32 DEG C, carry out gel forming under the environment of 5 ~ 8 at pH value, then the dilution heat of sulfuric acid being placed in 0.017 ~ 0.021% soaks 3 ~ 5 hours in the temperature of 26 ~ 32 DEG C, in gel, acid content reaches till 0.011 ~ 0.016, wash with the warm water of 55 DEG C, drag for glue after taking out, dry through first time and be less than or equal to 10% to moisture content, screen; Second time is dried and is less than or equal to 2% to moisture content, obtains 266.5 kilograms of pore block silica gels.
Embodiment three, a kind of method utilizing sulfate cinder to produce water glass and pore block silica gel described in the present embodiment, comprises the steps:
Get silica content be 35.73% sulfate cinder administer 500 kilograms, primary emission waste residue prepare water glass and pore block silica gel, the primary emission waste residue (being mainly the acid non-soluble substance such as silicon-dioxide and elemental sulfur) that sulfate cinder is administered with 9 ~ 16% hydrochloric acid soln repetitive scrubbing 19 ~ 32 minutes, filter cake clear water after filtration washs three times, making pH value reach 6 ~ 7 filters stand-by again, obtains pure filter cake; Acid filtrate washing capable of circulation uses, to save cost and preventing pollution; Acid clear water washing lotion can blend hydrochloric acid washings, and remainder is reasonably discharged by basic treatment;
The pure filter cake (silicon-dioxide meter) of above-mentioned acquisition and liquid sodium hydroxide are mixed in steam-heated pressure reactor with pure mass ratio 1: 1.13, start steam heating, stop after making reaction pressure reach 0.6 ~ 0.9Mpa passing into open steam, with jacket steam insulation, and maintain this pressure 4 ~ 9 hours; The sodium silicate solution that will be formed afterwards filters, and obtains filter cake elemental sulfur, through washing, dry, pulverize, be packaged to be elemental sulfur product; By the sodium silicate liquid obtained again through gently concentrating, cooling, 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 21 ~ 32 DEG C, carry out gel forming under the environment of 5 ~ 8 at pH value, then 0 is placed in, the dilution heat of sulfuric acid of 017 ~ 0.021% soaks 3 ~ 5 hours in the temperature of 26 ~ 32 DEG C, in gel, acid content reaches till 0.011 ~ 0.016, wash with the warm water of 55 DEG C, drag for glue after taking out, through first time, oven dry is less than or equal to 10% to moisture content, screening; Second time is dried and is less than or equal to 2% to moisture content, obtains 196.9 kilograms of pore block silica gels.
The above is only three preferred embodiments of the present invention, is not used for limiting the present invention, and its similar embodiments all, all should be covered by the protection domain of patent of the present invention.

Claims (1)

1. the method utilizing sulfate cinder to produce water glass and pore block silica gel, it is characterized in that comprising the steps: primary emission waste residue that sulfate cinder is administered with 9 ~ 16% hydrochloric acid soln repetitive scrubbing 19 ~ 32 minutes, filter cake clear water after filtration washs three times, making pH value reach 6 ~ 7 filters stand-by again, obtains pure filter cake; Acid filtrate washing capable of circulation uses, to save cost and preventing pollution; Acid clear water washing lotion can blend hydrochloric acid washings, and remainder is reasonably deposited by basic treatment; The pure filter cake of above-mentioned acquisition and liquid sodium hydroxide are mixed in steam-heated pressure reactor with pure mass ratio 1: 1.12 ~ 1.55, start steam heating, stop after making reaction pressure reach 0.6 ~ 0.9Mpa passing into open steam, with jacket steam insulation, and maintain this pressure 4 ~ 9 hours; The sodium silicate solution that will be formed afterwards filters, and obtains filter cake elemental sulfur, through Xian Di, drying, pulverizes, is packaged to be elemental sulfur product; By the sodium silicate liquid obtained again through gently concentrating, cooling, obtain 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 21 ~ 32 DEG C, carry out gel forming under the environment of 5 ~ 8 at pH value, then the dilution heat of sulfuric acid being placed in 0.017 ~ 0.021% soaks 3 ~ 5 hours in the temperature of 25 ~ 32 DEG C, in gel, acid content reaches till 0.011 ~ 0.016, wash with the warm water of 55 DEG C, drag for glue after taking out, dry through first time and be less than or equal to 10% to moisture content, screen; Second time is dried and is less than or equal to 2% to moisture content, obtains pore block silica gel.
CN201410538195.5A 2014-09-24 2014-09-24 Method for producing water glass and fine-pore massive silica gel by using pyrite cinders Pending CN105439157A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109735010A (en) * 2016-10-09 2019-05-10 芜湖瑞德机械科技有限公司 A kind of automobile engine hollow tube and preparation method thereof modified based on graphene

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109735010A (en) * 2016-10-09 2019-05-10 芜湖瑞德机械科技有限公司 A kind of automobile engine hollow tube and preparation method thereof modified based on graphene

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Application publication date: 20160330