CN107500249A - The method of the comprehensive utilization of acid-etched glass slag - Google Patents
The method of the comprehensive utilization of acid-etched glass slag Download PDFInfo
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- CN107500249A CN107500249A CN201710829879.4A CN201710829879A CN107500249A CN 107500249 A CN107500249 A CN 107500249A CN 201710829879 A CN201710829879 A CN 201710829879A CN 107500249 A CN107500249 A CN 107500249A
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- Prior art keywords
- acid
- etched glass
- glass slag
- fluorine
- glass
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/19—Fluorine; Hydrogen fluoride
- C01B7/191—Hydrogen fluoride
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/08—Compounds containing halogen
- C01B33/10—Compounds containing silicon, fluorine, and other elements
- C01B33/103—Fluosilicic acid; Salts thereof
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/46—Sulfates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/68—Aluminium compounds containing sulfur
- C01F7/74—Sulfates
- C01F7/743—Preparation from silicoaluminious materials, e.g. clays or bauxite
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Dispersion Chemistry (AREA)
- Glass Compositions (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The present invention proposes a kind of method that acid-etched glass slag for comprehensive utilizes, including：(1) acid-etched glass slag is heated, the fluorine-containing acid solution on the acid-etched glass slag surface is evaporated, and fluorine-containing acid solution is absorbed as with water；(2) dried glass dregs are placed in reactor with the concentrated sulfuric acid, and using indirectly heat, gas caused by reaction obtains anhydrous hydrogen fluoride by condensation, and uncooled gas is absorbed with water；Export material residue；(3) in material residue input process water, dissolving；Solution after dissolving is aluminum sulfate solution, and aluminum sulfate solid product can be made by concentration；Undissolved solids passes through separation of solid and liquid, turns into strontium sulfate or/and calcium sulfate finished product.The present invention is reclaimed the fluorine in caused glass dregs in glass thinning technique, anhydrous hydrogen fluoride is made, fluosilicic acid, aluminium, strontium are formed with to the aluminum sulfate and strontium sulfate of economic value, not only solve process problem of the glass dregs as dangerous waste, and the higher product of economic value has been obtained, it is suitable for industrial application.
Description
Technical field
The present invention relates to caused offal treatment field during glass thinning, a kind of acid-etched glass slag is particularly related to
Comprehensive utilization.
Background technology
Electronic equipment develops towards lightening direction always, so in mobile device or the glass display screen of handheld device
In production process, there is one of glass thinning process, display screen glass is made up into technological requirement by chemical attack mode
Thickness；A certain amount of sediment will be produced in thinning process, glass thinning industry is called glass dregs.
Glass ingredient for preparing display screen all contains SiO2、Al2O3、B2O3, while addition MgO, CaO, SrO etc. are adjusted
The characteristic of whole glass.At present, glass thinning industry uses hydrofluoric acid as main thinned chemicals, caused by thinning process
Glass dregs main component is aluminum fluoride, and containing a small amount of strontium fluoride, calcirm-fluoride, (silicon and fluorine form silicate fluoride solution, boron and fluorine simultaneously
Form fluoborate solution).With the progress of thinning process, glass dregs will be stepped up, when glass dregs content reaches in reducer
It must just be filtered after certain amount, discharge the system of being thinned, otherwise will have a strong impact on the thinned efficiency and quality of glass.
Due to the feature of glass dregs, glass dregs belong to danger wastes.The typically commission of glass thinning enterprise has at dangerous waste
The unit for managing qualification carries out harmless treatment, and processing cost reaches 5500 yuan/ton；Ye You glass thinnings enterprise is by glass dregs and life
Harmless treatment is carried out with lime after waste water mixing during production, its processing cost reaches 2000 yuan/ton.No matter which kind of is used
Processing mode, the fluorine-containing material in glass dregs is changed into calcium fluoride sludge；This method waste fluorine resource in short supply and
Bauxite resource, while substantial amounts of lime is also wasted, also bring burden to environmental improvement.
In view of this, this discarded object of glass dregs is handled, obtains the higher product of economic value, such a technique
Appearance is just particularly important.
The content of the invention
The present invention proposes a kind of method that acid-etched glass slag for comprehensive utilizes, and solves the glass in glass thinning in the prior art
The problem of glass Slag treatment cost is high, fluorine aluminium resource waste.
The technical proposal of the invention is realized in this way：
A kind of method that acid-etched glass slag for comprehensive utilizes, including：
(1) glass dregs are dried：Acid-etched glass slag is heated, the fluorine-containing acid solution on the acid-etched glass slag surface is evaporated, and is used
Water is absorbed as fluorine-containing acid solution；
(2) sulfuric acid reaction：Step (1) dried glass dregs and the concentrated sulfuric acid are placed in reactor, using indirectly heat,
120 DEG C~600 DEG C of controlling reaction temperature, gas caused by reaction obtain anhydrous hydrogen fluoride by condensation, and uncooled gas is used
Water is absorbed as fluosilicic acid；Fully after reaction, material residue is exported in reactor；
(3) water dissolves：By in the material residue input process water of step (2), dissolved under agitation；It is molten after dissolving
Liquid is aluminum sulfate solution, and aluminum sulfate solid product can be made by concentration；Undissolved solids passes through separation of solid and liquid, turns into sulphur
Sour strontium or/and calcium sulfate finished product.
As preferable technical scheme, the process conditions that step (1) glass dregs are dried are：Hot blast indirectly heat, adds
Hot temperature is 100 DEG C~500 DEG C, is absorbed caused by evaporation containing acid vapor in spray absorber with water, tail gas during spray
Cooled, gas temperature when control is discharged into air is less than 50 DEG C；Fluorine-containing acid concentration in spray liquid reaches process value heel row
Go out, as fluorine-containing acid solution；The fluoric-containing acid is returned in glass thinning technological process.It is furthermore preferred that the heating-up temperature is 350
~450 DEG C；Initial spray liquid is process water, and fluorine-containing acid concentration recycles before being not up to technique concentration.
As preferable technical scheme, the concentrated sulfuric acid in the step (2) includes 92~98% sulfuric acid, 105% sulfuric acid, dense
One or more of combinations in Waste Sulfuric Acid of the degree more than or equal to 90%.
As preferable technical scheme, step (2) reaction temperature is 250~400 DEG C, and reaction time control exists
20 minutes~600 minutes.It is furthermore preferred that reaction time controls 180 minutes~420 minutes
As preferable technical scheme, the reaction gas in the step (2) uses concentrated sulfuric acid spraying cooling, then condensation,
Rectifying, anhydrous hydrogen fluoride product is obtained, fixed gas is absorbed with water in reaction gas, obtains silicate fluoride solution.
As preferable technical scheme, the temperature control of step (3) the water dissolving is in room temperature~120 DEG C.
As preferable technical scheme, the acid-etched glass slag in the step (1) is after glass material reacts with hydrofluoric acid
Solid waste.
As preferable technical scheme, the acid-etched glass slag in the step (1) derives from display glass panel thinning
Technique；Described acid-etched glass slag at least containing aluminium, strontium, calcium fluorine-containing hydrochlorate.
Beneficial effect
(1) present invention is reclaimed the fluorine in caused glass dregs in glass thinning technique, and anhydrous hydrogen fluoride, fluorine is made
Silicic acid, aluminium, strontium are formed with to the aluminum sulfate and strontium sulfate of economic value, the processing for not only solving glass dregs as dangerous waste is asked
Topic, and the higher product of economic value has been obtained, it is suitable for industrial application.
(2) processing technological flow of the invention is short, and condition is simple, high without complex device, small investment, return rate.
Embodiment
The technical scheme in the embodiment of the present invention will be clearly and completely described below, it is clear that described implementation
Example only part of the embodiment of the present invention, rather than whole embodiments.It is common based on the embodiment in the present invention, this area
The every other embodiment that technical staff is obtained under the premise of creative work is not made, belong to the model that the present invention protects
Enclose.
The material used in following embodiments is commercially available, in that context it may be convenient to is bought from market.
The method that a kind of acid-etched glass slag for comprehensive in following embodiments utilizes, step (1) heating-up temperature are 100~500
DEG C, 120~600 DEG C of controlling reaction temperature in step (2), reaction time is controlled at 20 minutes~600 minutes.These values
The object of the invention can be realized.Do not repeat.
Embodiment 1
Glass dregs used in the embodiment：The glass dregs of certain glass thinning workshop discharge, igloss 56.50%, solid content are
43.50% (wherein aluminum fluoride 28.00%, magnesium fluoride 0.17%, calcirm-fluoride 5.71%, strontium fluoride 9.09%, other 0.53%)；
The composition of glass dregs filter process mother liquor is：HF -10%, H2SiF6- 10%, HCl -5%, soluble-salt -0.93%, its
Remaining is process water.
A kind of method that acid-etched glass slag for comprehensive utilizes, comprises the following steps：
Step S1：Dry glass slag
Start rotary kiln exhaust gas absorption system and heating system, control rotary kiln rotating speed 1rpm, take fluorgypsum 500kg, use
Spiral puts into fluorgypsum in rotary kiln, then clear with fluorgypsum 500kg with glass dregs wet product 2000kg is sent into rotary kiln
Wash spiral, 500 DEG C of control rotary kiln hot blast temperature, mixed material exports from stove tail, Temperature fall, is packaged into jumbo bag, standby.Stove
Head is dried tail gas and absorbed with running water, obtain 2000kg recovery fluoric-containing acid (HF --- 5.6%, H2SiF6--- 5.65%,
HCl --- 2.8%).
Step S2：Clear up glass dregs
Start rotary kiln exhaust gas absorption system and heating system, control rotary kiln rotating speed 1.5rpm, take fluorgypsum
1000kg, fluorgypsum is put into rotary kiln with spiral, with the glass dregs that will be dried/fluorgypsum compound and 1275kg
(the nitration mixture of 98% sulfuric acid and oleum：Here it is the sulfuric acid for being made into 100% of 98% sulfuric acid and oleum) it is sent into revolution
In kiln, then with fluorgypsum 500kg clean spiral, 500 DEG C of control rotary kiln hot blast temperature, reaction material residue exports from stove tail, natural
Cooling, sampling analysis (calcium sulphate content 65.61%, sulfuric acid aluminium content 27.72%, sulfuric acid content of strontium 6.46%).Burner reacts
Gas is absorbed with running water, obtain 2520kg hydrofluoric acid (HF --- 10.20%, H2SO4--- 0.09%).
Step S3：Processing reaction material residue
To 0.5M3Running water 350kg is put into stirred autoclave, takes stove end reaction material residue 100Kg, starts stirring, will
React in material residue input reactor, after feeding intake, open chuck electric heater, when suspension temperature reaches 110 DEG C, start
Timing is simultaneously incubated 2h, filtering, obtains mother liquor 269kg (sulfuric acid aluminum concentration is 7.33%)；Filter cake originally water washing 5 times, sampling
Analysis, filter cake composition are following (butt)：Calcium sulfate --- 89.98%, strontium sulfate --- 9.04%.
Note：Addition fluorgypsum is to react rotary furnace for protection, the startup of normal fluorite-Production By Sulfuric Acid Process hydrofluoric acid, is adopted
Reaction rotary furnace is protected with this method.
Embodiment 2
Glass dregs used in the embodiment：The glass dregs of certain glass thinning workshop discharge, igloss 56.50%, solid content are
43.50% (wherein aluminum fluoride 28.00%, magnesium fluoride 0.17%, calcirm-fluoride 5.71%, strontium fluoride 9.09%, other 0.53%)；
The composition of glass dregs filter process mother liquor is：HF -10%, H2SiF6- 10%, HCl -5%, soluble-salt -0.93%, its
Remaining is process water.
A kind of method that acid-etched glass slag for comprehensive utilizes, comprises the following steps：
Step S1：Dry glass slag
Start rotary kiln exhaust gas absorption system and heating system, control rotary kiln rotating speed 1rpm, take fluorgypsum 500kg, use
Spiral puts into fluorgypsum in rotary kiln, then clear with fluorgypsum 500kg with glass dregs wet product 2000kg is sent into rotary kiln
Spiral is washed, using hot blast indirectly heat, 150 DEG C of control rotary kiln hot blast temperature, mixed material exports from stove tail, Temperature fall,
It is packaged into jumbo bag, standby.Burner is dried tail gas and absorbed with spray column absorption tower, and spray liquid is running water, and stone is used during spray
Black heat exchanger cools to spray liquid, and control spray liquid temperature is less than 50 DEG C, obtain 2050kg recovery fluoric-containing acid (HF ---
5.35%th, H2SiF6 --- 5.45%, HCl --- is 2.84%).
Step S2：Clear up glass dregs
Start rotary kiln exhaust gas absorption system and heating system, control rotary kiln rotating speed 1.5rpm, take fluorgypsum
1000kg, fluorgypsum is put into rotary kiln with spiral, (used with the glass dregs that will be dried/fluorgypsum compound and 1285kg
90% spent acid and the nitration mixture of oleum) it is sent into rotary kiln, then clean spiral, control rotary kiln heat with fluorgypsum 500Kg
600 DEG C of air temperature, reaction response material residue export from stove tail, Temperature fall, sampling analysis (calcium sulphate content 65.63%, aluminum sulfate
Content 27.71%, sulfuric acid content of strontium 6.45%).Burner reaction gas carries out spraying cooling with the concentrated sulfuric acid, and condensation, rectifying, are obtained afterwards
To 2512kg hydrogen fluoride (HF --- 10.14%, H2SO4--- 0.08%).
Step S3：Processing reaction material residue
To 0.5M3Running water 350kg is put into stirred autoclave, takes stove end reaction material residue 100Kg, starts stirring, will
React in material residue input reactor, after feeding intake, open chuck electric heater, when suspension temperature reaches 110 DEG C, start
Timing is simultaneously incubated 2h, filtering, obtains mother liquor 267kg (sulfuric acid aluminum concentration is 7.32%)；Filter cake originally water washing 5 times, sampling
Analysis, filter cake composition are following (butt)：Calcium sulfate --- 89.96%, strontium sulfate --- 9.03%.
Note：Addition fluorgypsum is to react rotary furnace for protection, the startup of normal fluorite-Production By Sulfuric Acid Process hydrofluoric acid, is adopted
Reaction rotary furnace is protected with this method.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
God any modification, equivalent substitution and improvements made etc., should be included in the scope of the protection with principle.
Claims (9)
1. a kind of method that acid-etched glass slag for comprehensive utilizes, including：
(1) glass dregs are dried：Acid-etched glass slag is heated, the fluorine-containing acid solution on the acid-etched glass slag surface is evaporated, inhaled with water
Receive as fluorine-containing acid solution；
(2) sulfuric acid reaction：Step (1) dried glass dregs and the concentrated sulfuric acid are placed in reactor, using indirectly heat, control
120 DEG C~600 DEG C of reaction temperature, gas caused by reaction obtains anhydrous hydrogen fluoride by condensation, and uncooled gas is inhaled with water
Receive as fluosilicic acid；Fully after reaction, material residue is exported in reactor；
(3) water dissolves：By in the material residue input process water of step (2), dissolved under agitation；Solution after dissolving is
Aluminum sulfate solution, aluminum sulfate solid product can be made by concentration；Undissolved solids passes through separation of solid and liquid, turns into strontium sulfate
Or/and calcium sulfate finished product.
2. the method that a kind of acid-etched glass slag for comprehensive according to claim 1 utilizes, it is characterised in that the step (1)
Glass dregs dry process conditions be：Hot blast indirectly heat, heating-up temperature are 100 DEG C~500 DEG C, contain acid vapor caused by evaporation
Absorbed in spray absorber with water, tail gas is cooled during spray, and gas temperature when control is discharged into air is less than 50
℃；Fluorine-containing acid concentration in spray liquid is discharged after reaching process value, as fluorine-containing acid solution；The fluoric-containing acid returns to glass thinning
In technological process.
3. the method that a kind of acid-etched glass slag for comprehensive according to claim 2 utilizes, it is characterised in that the heating-up temperature
For 350~450 DEG C；Initial spray liquid is process water, and fluorine-containing acid concentration recycles before being not up to technique concentration.
4. the method that a kind of acid-etched glass slag for comprehensive according to claim 1 utilizes, it is characterised in that the step (2)
In the concentrated sulfuric acid include 92~98% sulfuric acid, 105% sulfuric acid, concentration more than or equal to 90% Waste Sulfuric Acid in it is one or more of
Combination.
5. the method that a kind of acid-etched glass slag for comprehensive according to claim 1 utilizes, it is characterised in that the step (2)
Reaction temperature is 250~400 DEG C, and reaction time is controlled at 20 minutes~600 minutes.
6. the method that a kind of acid-etched glass slag for comprehensive according to claim 1 utilizes, it is characterised in that the step (2)
In reaction gas use concentrated sulfuric acid spraying cooling, then condensation, rectifying, obtain anhydrous hydrogen fluoride product, fixed gas in reaction gas
Absorbed with water, obtain silicate fluoride solution.
7. the method that a kind of acid-etched glass slag for comprehensive according to claim 1 utilizes, it is characterised in that the step (3)
The temperature control of water dissolving is in room temperature~120 DEG C.
8. the method that a kind of acid-etched glass slag for comprehensive according to claim 1 utilizes, it is characterised in that the step (1)
In acid-etched glass slag be glass material and the reacted solid waste of hydrofluoric acid.
9. the method that a kind of acid-etched glass slag for comprehensive according to claim 1 or 8 utilizes, it is characterised in that the step
(1) the acid-etched glass slag in derives from display glass panel thinning technique；Described acid-etched glass slag at least containing aluminium, strontium,
The fluorine-containing hydrochlorate of calcium.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710829879.4A CN107500249B (en) | 2017-09-15 | 2017-09-15 | Comprehensive utilization method of acid-etched glass slag |
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| CN201710829879.4A CN107500249B (en) | 2017-09-15 | 2017-09-15 | Comprehensive utilization method of acid-etched glass slag |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112357943A (en) * | 2020-11-10 | 2021-02-12 | 湖北省宏源药业科技股份有限公司 | Method for recovering cryolite from acid pickling residues of silicon-aluminum glass |
| CN113860257A (en) * | 2021-11-04 | 2021-12-31 | 浙江容跃环保科技有限公司 | Method and system for regenerating and recycling glass thinning waste acid liquor |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102249279A (en) * | 2010-12-21 | 2011-11-23 | 王莉 | Method for using vitriol sludge hydrolyzed filter cake to prepare aluminum sulfate and byproduct calcium sulfate |
| CN102502502A (en) * | 2011-11-08 | 2012-06-20 | 湖南有色郴州氟化学有限公司 | Method for preparing hydrogen fluoride gas from 98% sulphuric acid |
| CN103539127A (en) * | 2013-10-31 | 2014-01-29 | 洛阳氟钾科技有限公司 | Process for decomposing potash feldspars |
| CN104341111A (en) * | 2013-07-26 | 2015-02-11 | 睿志达光电(深圳)有限公司 | Glass etching solution regeneration method and glass etching method |
-
2017
- 2017-09-15 CN CN201710829879.4A patent/CN107500249B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102249279A (en) * | 2010-12-21 | 2011-11-23 | 王莉 | Method for using vitriol sludge hydrolyzed filter cake to prepare aluminum sulfate and byproduct calcium sulfate |
| CN102502502A (en) * | 2011-11-08 | 2012-06-20 | 湖南有色郴州氟化学有限公司 | Method for preparing hydrogen fluoride gas from 98% sulphuric acid |
| CN104341111A (en) * | 2013-07-26 | 2015-02-11 | 睿志达光电(深圳)有限公司 | Glass etching solution regeneration method and glass etching method |
| CN103539127A (en) * | 2013-10-31 | 2014-01-29 | 洛阳氟钾科技有限公司 | Process for decomposing potash feldspars |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112357943A (en) * | 2020-11-10 | 2021-02-12 | 湖北省宏源药业科技股份有限公司 | Method for recovering cryolite from acid pickling residues of silicon-aluminum glass |
| CN113860257A (en) * | 2021-11-04 | 2021-12-31 | 浙江容跃环保科技有限公司 | Method and system for regenerating and recycling glass thinning waste acid liquor |
| CN113860257B (en) * | 2021-11-04 | 2022-04-22 | 浙江容跃环保科技有限公司 | Method and system for regenerating and recycling glass thinning waste acid liquor |
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