CN105883833A - Method for producing sodium silicate and coarse pore spherical silica gel from sulfuric acid slag - Google Patents
Method for producing sodium silicate and coarse pore spherical silica gel from sulfuric acid slag Download PDFInfo
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- CN105883833A CN105883833A CN201410499683.XA CN201410499683A CN105883833A CN 105883833 A CN105883833 A CN 105883833A CN 201410499683 A CN201410499683 A CN 201410499683A CN 105883833 A CN105883833 A CN 105883833A
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- sodium silicate
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Abstract
The invention discloses a method for producing sodium silicate and coarse pore spherical silica gel from sulfuric acid slag. The method comprises repeatedly washing primarily discharged waste slag of sulfuric acid slag treatment through a hydrochloric acid solution with a concentration of 9-16% for 21-32min, washing the filter cake through clear water three times, carrying out filtration to obtain pure filter cake, mixing the pure filter cake and liquid sodium hydroxide according to a pure mass ratio of 1: 1.08-1.58, carrying out a reaction process on the mixture in a pressure reactor subjected to steam heating to obtain a sodium silicate solution, filtering the sodium silicate solution, carrying out light concentration and cooling on the sodium silicate solution to obtain a sodium silicate solution product, diluting the sodium silicate solution through water, mixing the dilute sodium silicate solution and dilute sulphuric acid, carrying out gelatinization balling, carrying out aging for 6h, carrying out washing through warm water at a temperature of 52-68 DEG C, carrying out immersion in ammonium hydroxide with a concentration of 0.13-0.21% for 6h and carrying out drying to obtain the coarse pore spherical silica gel. The method utilizes sulfuric acid slag treatment waste slag as a raw material to prepare sodium silicate and coarse pore spherical silica gel, realizes change of waste into valuables and creates considerable economic benefits.
Description
Technical field
The present invention relates to comprehensive control and the technical field of utilization of sulphuric acid inorganic industrial discharge, particularly relate to one and utilize sulphuric acid
Slag produces waterglass and the method for gross porosity spherical silica-gel.
Background technology
Sulfuric acid industry is the sulphuric acid produced for raw material contact method with troilite, mainly by raw material roasting, purify, convert and absorption etc.
Several operations form.To purify technological process in general custom, gas washing in SA production is divided into the big class of dry and wet two.Wet cleaning
Have again that pickling, hot concentrated acid wash and wash point.Pyrite-based sulfuric acid production minority factory of China is pickling process at present, and majority is still for washing
Flow process.
Troilite is mainly made up of sulfur and ferrum, with a small amount of non-ferrous metal and rare metal.Pyrite cinder is pyrite burning
The residue discharged after extracting sulfur.In troilite in addition to sulfur is utilized, ferrum and other elements remain in slag.Slag is used to
Ironmaking, extracts non-ferrous metal and manufactures the raw material of construction material.
The slag discharge capacity of unit sulfuric acid product is relevant with the grade of troilite and process conditions.Sulfur ferrum under identical process conditions
The highest then bed drain purge of grade in ore deposit is the fewest, otherwise the highest.When troilite sulfur content is 25～35%, general production is per ton about
Produce the clinker of 0.7～1 ton.Wherein, various compositions and the percentage composition of pyrite cinder is: ferroso-ferric oxide content is 43.31
%, aluminium sesquioxide content is 8.13%, and calcium oxide content is 1.63%, and content of magnesia is 0.46%, silica content
Being 35.73%, the content of sulfur is 0.16%.
At present, the comprehensive utilization of pyrite cinder is unsatisfactory, and in addition to small part is used as ironmaking and construction material, major part uses
Landfill processes, and causes the waste of resource and the pollution of environment.
In a series of inventions such as " prepare pyrite cinder are muriatic method with chemical method ", by extracting after salt acid purification
Ferroso-ferric oxide, aluminium sesquioxide, calcium oxide, magnesium oxide, silicon oxide, elemental sulfur element etc., after forming various slaine
Remaining acid non-soluble substance is silicon dioxide and elemental sulfur.The present invention be exactly utilize the process waste residue of pyrite cinder prepare waterglass and
The method of gross porosity spherical silica-gel.The method is the patented invention that the typical disposal of three wastes is derivative, and its purpose seeks to inside a three wastes
Various materials and element eat dry deep-frying only all of.By the decomposition residue contamination source of several levels, in the hope of maximum possible
Reduce the secondary of the chemical industry three wastes or the exhaust emission of three times.
Summary of the invention
The technical problem to be solved is, processes the improvement waste residue of pyrite cinder, comprehensive utilization, prepares water glass
Glass and gross porosity spherical silica-gel, it is provided that a kind of utilize pyrite cinder to produce waterglass and the method for gross porosity spherical silica-gel, the method is effective
The secondary pollution avoiding sulfuric acid industry, primary emission is found potentiality and eats that dry deep-frying is clean, turns waste into wealth, eventually become
The silicon series of products being worth, create considerable economic benefit, protect environment.
The technical solution adopted for the present invention to solve the technical problems is: one utilizes pyrite cinder to produce waterglass and gross porosity is spherical
The method of silica gel, comprises the steps:
The primary emission waste residue (the predominantly acid non-soluble substance such as silicon dioxide and elemental sulfur) administered by pyrite cinder is with 9～the salt of 16%
Acid solution cyclic washing 21～32 minutes, the clear water of the filter cake after filtration washs three times, make pH value reach 6～7 filter again stand-by,
Obtain pure filter cake；Acid filtrate capable of circulation washing use, with cost-effective and prevent pollute；Acid clear water washing liquid can blend salt
Acid elution liquid, 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 pure mass ratio 1: 1.08～1.58
In steam-heated pressure reactor, start steam heating, after making reaction pressure reach 0.7～0.8Mpa, stop being passed through directly steaming
Vapour, is incubated with jacket steam, and maintains this pressure 4～9 hours；Afterwards the sodium silicate solution formed is filtered, obtain filter cake list
Matter sulfur, scrubbed, be dried, pulverize, be packaged to be elemental sulfur product；By the sodium silicate liquid obtained again through gently concentrating, cooling down,
Obtain waterglass fluid product；
The waterglass liquid dilute with water of above-mentioned acquisition is mixed with dilute sulfuric acid, in the environment of pH value is 5～8 in temperature be 21～
Carry out the ball that is gelled when 33 DEG C, aging 6 hours, with the warm water of 52～68 DEG C washing, then with 0.13～0.21% ammonia immersion at
Manage 6 hours, to expand glueballs aperture, dry to moisture less than or equal to 10% through for the first time after immersion, after screening second
Secondary drying less than or equal to 2%, prepares gross porosity spherical silica-gel to moisture.
The chemical equation of the present invention is as follows:
SiO2+ 2NaOH=Na2SiO3+H2O
Na2SiO3+H2SO4=Na2SO4+SiO2+H2O
The invention has the beneficial effects as follows: one, the invention provides one one and utilize pyrite cinder to produce waterglass and gross porosity
The method of spherical silica-gel, the method effectively make use of the material composition administering waste residue of pyrite cinder, the improvement to pyrite cinder
Waste residue processes, comprehensive utilization, prepares waterglass and gross porosity spherical silica-gel.Its two, waterglass and gross porosity spherical silica-gel are used
Way is wide, is the product that two kinds of economic worths are bigger, improves the economic benefit administering waste residue processing pyrite cinder, creates very
Big profit return, is the model of chemical industry comprehensive control and utilization.Its three, small investment, to process pyrite cinder improvement
Waterglass prepared by waste residue and gross porosity spherical silica-gel is especially suitable, it may be said that opens a Tiao Xin road.Its four, the purity of preparation is high,
Quality is guaranteed.Its five, the method effectively avoids the secondary pollution of sulfuric acid industry, in primary emission find potentiality eat
Dry deep-frying is clean, turn waste into wealth, and eventually becomes valuable silicon series of products, creates considerable economic benefit.
Detailed description of the invention
Embodiment one, a kind of described in the present embodiment utilizes pyrite cinder to produce waterglass and the method for gross porosity spherical silica-gel, including
Following steps:
Take 500 kilograms of the primary emission waste residue that pyrite cinder that silica content is 35.73% administers and prepare waterglass and gross porosity is spherical
Silica gel, the primary emission waste residue (the predominantly acid non-soluble substance such as silicon dioxide and elemental sulfur) administered by pyrite cinder is with 9～16%
Hydrochloric acid solution cyclic washing 21～32 minutes, the clear water of the filter cake after filtration washs three times, make pH value reach 6～7 filter again stand-by,
Obtain pure filter cake；Acid filtrate capable of circulation washing use, with cost-effective and prevent pollute；Acid clear water washing liquid can blend salt
Acid elution liquid, remainder is reasonably discharged by basic treatment；
With pure mass ratio 1: 1.33, the pure filter cake (silicon dioxide meter) of above-mentioned acquisition and liquid sodium hydroxide are mixed in steam add
In the pressure reactor of heat, start steam heating, stop after making reaction pressure reach 0.7～0.8Mpa being passed through live (open) steam, use
Jacket steam is incubated, and maintains this pressure 4～9 hours；Afterwards the sodium silicate solution formed is filtered, obtains filter cake elemental sulfur,
Scrubbed, be dried, pulverize, be packaged to be elemental sulfur product；By the sodium silicate liquid obtained again through gently concentrating, cooling down, it is thus achieved that
362.3 kg of water glass precursor solution product；
The waterglass liquid dilute with water of above-mentioned acquisition is mixed with dilute sulfuric acid, in the environment of pH value is 5～8 in temperature be 21～
Carry out the ball that is gelled when 33 DEG C, aging 6 hours, with the warm water of 52～68 DEG C washing, then with 0.13～0.21% ammonia immersion at
Manage 6 hours, to expand glueballs aperture, dry to moisture less than or equal to 10% through for the first time after immersion, after screening second
Secondary drying less than or equal to 2%, prepares 231.6 kilograms of gross porosity spherical silica-gels to moisture.
Embodiment two, a kind of described in the present embodiment utilizes pyrite cinder to produce waterglass and the method for gross porosity spherical silica-gel, including
Following steps:
Take 500 kilograms of the primary emission waste residue that pyrite cinder that silica content is 35.73% administers and prepare waterglass and gross porosity is spherical
Silica gel, the primary emission waste residue (the predominantly acid non-soluble substance such as silicon dioxide and elemental sulfur) administered by pyrite cinder is with 9～16%
Hydrochloric acid solution cyclic washing 21～32 minutes, the clear water of the filter cake after filtration washs three times, make pH value reach 6～7 filter again stand-by,
Obtain pure filter cake；Acid filtrate capable of circulation washing use, with cost-effective and prevent pollute；Acid clear water washing liquid can blend salt
Acid elution liquid, remainder is reasonably discharged by basic treatment；
With pure mass ratio 1: 1.53, the pure filter cake (silicon dioxide meter) of above-mentioned acquisition and liquid sodium hydroxide are mixed in steam add
In the pressure reactor of heat, start steam heating, stop after making reaction pressure reach 0.7～0.8Mpa being passed through live (open) steam, use
Jacket steam is incubated, and maintains this pressure 4～9 hours；Afterwards the sodium silicate solution formed is filtered, obtains filter cake elemental sulfur,
Scrubbed, be dried, pulverize, be packaged to be elemental sulfur product；By the sodium silicate liquid obtained again through gently concentrating, cooling down, it is thus achieved that
416.8 kg of water glass precursor solution product；
The waterglass liquid dilute with water of above-mentioned acquisition is mixed with dilute sulfuric acid, in the environment of pH value is 5～8 in temperature be 21～
Carry out the ball that is gelled when 33 DEG C, aging 6 hours, with the warm water of 52～68 DEG C washing, then with 0.13～0.21% ammonia immersion at
Manage 6 hours, to expand glueballs aperture, dry to moisture less than or equal to 10% through for the first time after immersion, after screening second
Secondary drying less than or equal to 2%, prepares 266.5 kilograms of gross porosity spherical silica-gels to moisture.
Embodiment three, a kind of described in the present embodiment utilizes pyrite cinder to produce waterglass and the method for gross porosity spherical silica-gel, including
Following steps:
Take 500 kilograms of the primary emission waste residue that pyrite cinder that silica content is 35.73% administers and prepare waterglass and gross porosity is spherical
Silica gel, the primary emission waste residue (the predominantly acid non-soluble substance such as silicon dioxide and elemental sulfur) administered by pyrite cinder is with 9～16%
Hydrochloric acid solution cyclic washing 21～32 minutes, the clear water of the filter cake after filtration washs three times, make pH value reach 6～7 filter again stand-by,
Obtain pure filter cake；Acid filtrate capable of circulation washing use, with cost-effective and prevent pollute；Acid clear water washing liquid can blend salt
Acid elution liquid, remainder is reasonably discharged by basic treatment；
With pure mass ratio 1: 1.13, the pure filter cake (silicon dioxide meter) of above-mentioned acquisition and liquid sodium hydroxide are mixed in steam add
In the pressure reactor of heat, start steam heating, stop after making reaction pressure reach 0.7～0.8Mpa being passed through live (open) steam, use
Jacket steam is incubated, and maintains this pressure 4～9 hours；Afterwards the sodium silicate solution formed is filtered, obtains filter cake elemental sulfur,
Scrubbed, be dried, pulverize, be packaged to be elemental sulfur product；By the sodium silicate liquid obtained again through gently concentrating, cooling down, it is thus achieved that
307.9 kg of water glass precursor solution product；
The waterglass liquid dilute with water of above-mentioned acquisition is mixed with dilute sulfuric acid, in the environment of pH value is 5～8 in temperature be 21～
Carry out the ball that is gelled when 33 DEG C, aging 6 hours, with the warm water of 52～68 DEG C washing, then with 0.13～0.21% ammonia immersion at
Manage 6 hours, to expand glueballs aperture, dry to moisture less than or equal to 10% through for the first time after immersion, after screening second
Secondary drying less than or equal to 2%, prepares 196.9 kilograms of gross porosity spherical silica-gels to moisture.
The above is only three preferred embodiments of the present invention, not for limiting the present invention, and its similar embodiments all, all
The protection domain of patent of the present invention should be covered by.
Claims (1)
1. utilize pyrite cinder to produce waterglass and a method for gross porosity spherical silica-gel, it is characterized in that comprising the steps: sulfur
The primary emission waste residue that acid slag is administered is with 9～the hydrochloric acid solution cyclic washing 21 of 16%～32 minutes, and the filter cake after filtration is with clearly
Water wash three times, make pH value reach 6～7 filter again stand-by, it is thus achieved that pure filter cake；Acid filtrate washing capable of circulation uses, with joint
Cost-saving and prevent pollute；Acid clear water washing liquid can blend hydrochloric acid cleaning mixture, and remainder is reasonably discharged by basic treatment；
The pure filter cake of above-mentioned acquisition and liquid sodium hydroxide are mixed in steam-heated pressure with pure mass ratio 1: 1.08～1.58 anti-
Answer in device, start steam heating, stop after making reaction pressure reach 0.7～0.8Mpa being passed through live (open) steam, protect with jacket steam
Temperature, and maintain this pressure 4～9 hours；Afterwards the sodium silicate solution formed is filtered, obtain filter cake elemental sulfur, scrubbed, dry
Dry, pulverize, be packaged to be elemental sulfur product；By the sodium silicate liquid obtained again through gently concentrating, cooling down, it is thus achieved that waterglass liquid
Product；The waterglass liquid dilute with water of above-mentioned acquisition is mixed with dilute sulfuric acid, in the environment of pH value is 5～8 in temperature is
Carry out the ball that is gelled when 21～33 DEG C, aging 6 hours, wash with the warm water of 52～68 DEG C, then soak with the ammonia of 0.13～0.21%
Bubble processes 6 hours, to expand glueballs aperture, dries to moisture less than or equal to 10% through for the first time, after screening after immersion
Second time is dried to moisture less than or equal to 2%, prepares gross porosity spherical silica-gel.
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| CN201410499683.XA CN105883833A (en) | 2014-09-18 | 2014-09-18 | Method for producing sodium silicate and coarse pore spherical silica gel from sulfuric acid slag |
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| CN201410499683.XA CN105883833A (en) | 2014-09-18 | 2014-09-18 | Method for producing sodium silicate and coarse pore spherical silica gel from sulfuric acid slag |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115676841A (en) * | 2022-10-27 | 2023-02-03 | 金三江(肇庆)硅材料股份有限公司 | Beer silica gel and preparation method thereof |
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- 2014-09-18 CN CN201410499683.XA patent/CN105883833A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115676841A (en) * | 2022-10-27 | 2023-02-03 | 金三江(肇庆)硅材料股份有限公司 | Beer silica gel and preparation method thereof |
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Application publication date: 20160824 |