CN110104842A - A kind of processing method of the fluorine-containing etching waste water containing ammonium - Google Patents
A kind of processing method of the fluorine-containing etching waste water containing ammonium Download PDFInfo
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- CN110104842A CN110104842A CN201910489844.XA CN201910489844A CN110104842A CN 110104842 A CN110104842 A CN 110104842A CN 201910489844 A CN201910489844 A CN 201910489844A CN 110104842 A CN110104842 A CN 110104842A
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Abstract
The invention discloses a kind of processing methods of fluorine-containing etching waste water containing ammonium, and described method includes following steps: (1) ammonium bicarbonate being added into waste water, is separated by solid-liquid separation after reaction, tail gas is absorbed by water；(2) filtrate being separated by solid-liquid separation in step (1) and the aqueous for absorbing tail gas are concentrated by counter-infiltration system, fresh water and concentrated water is made；(3) fresh water of step (2) is washed to obtained solid is separated by solid-liquid separation in step (1), obtains white carbon black after dry, wash water is recycled to reverse osmosis treatment；(4) white carbon black of step (3) is added in the concentrated water of step (2), adds boric acid and stirs and evenly mixs, insulation reaction is then filtered, dried；(5) obtained solid after step (4) drying is roasted, obtains boracic hetero-atom molecular-sieve.The present invention, which merges fluorine in wastewater, ammonium and organic matter etc., is converted into resource product, to realize reasonable effective disposition of such waste water, and occurs in the process without time useless with secondary pollution.
Description
Technical field
This application involves industrial waste water treatments, more particularly, to a kind of processing side of fluorine-containing etching waste water containing ammonium
Method.
Background technique
In semiconductor manufacturing industry, the formulation of fine dimension pattern is the device by etching technique to form integrated circuit
Framework, and the wet etching in etching technique is to be decomposed film portion to be etched using some specified chemical reagents, is converted into
Soluble compound enters water phase and reaches etching purpose.As being main etching solution, selective corrosion silicon wafer using hydrofluoric acid
Upper film, ammonium fluoride keep rate of etch to be used in mixed way to scale with hydrofluoric acid, while also adding to improve wetability as buffer
Some organic additives or surfactant are entered.A large amount of etching waste water are had after the completion of to be etched to generate, and are contained in this waste water
There are fluosilicic acid, ammonium fluoride and organic matter etc., if unprocessed direct emission, water body environment can be damaged, even be endangered
Evil underground water and drinking water source, and then influence human health.
It is similar with the disposition of other fluoride wastes, fluorine in water phase is fixed with sediment generally by the precipitation method, but
What is faced therewith is that sludge quantity is huge, and secondary cost of disposal is higher.In particular, the etching waste water of such complicated component, how
Realize that rationally and effectively disposition is the emphasis that the moment is paid close attention in industry.As passed through removal of impurities in 106517244 A of patent publication No. CN
Fluorine containing etchant waste liquid is prepared into ammonium acid fluoride, but it directly uses in ammonium hydroxide and cleans, in the process it is possible that ammonia taste is overflowed
Uncontrollable situation；For another example a kind of chelating resin adsorption-defluorination, but resin are used in 104843818 A of patent publication No. CN
It is expensive, and regeneration treatment is also needed after use, economically generally it is only applicable to low fluorine wastewater treatment.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of processing methods of fluorine-containing etching waste water containing ammonium by the application.
The present invention first separates silicon in etching waste water from system, obtains white carbon black finished product, while as product, can also function as
Fluorine in wastewater, ammonium and organic matter etc. are merged and are converted into resource product, to realize by the supplementary material of the subsequent disposition of waste water
Reasonable effective disposition of such waste water, and occur in the process without time useless and secondary pollution.
Technical scheme is as follows:
A kind of processing method of the fluorine-containing etching waste water containing ammonium, the treating method comprises following steps:
(1) ammonium bicarbonate is added into waste water under heating stirring, is separated by solid-liquid separation after mixing reaction, the tail gas volatilized in the process
It is absorbed by water；
(2) it is dense together with absorbing the aqueous of tail gas by counter-infiltration system and carrying out that gained filtrate will be separated by solid-liquid separation in step (1)
Fresh water and concentrated water is made in contracting；
(3) it is washed using fresh water obtained by step (2) to obtained solid is separated by solid-liquid separation in step (1), washes rear solid warp
White carbon black, wash water recirculation to reverse osmosis treatment are obtained after drying；
(4) white carbon black obtained in step (3) is added in step (2) resulting concentrated water, it is mixed adds boric acid stirring
It is even, it is placed in insulation reaction under isoperibol, then filters, dry；
(5) obtained solid after step (4) drying is roasted to get boracic hetero-atom molecular-sieve.
The fluorine in wastewater content is 7~8g/L, and ammonia-nitrogen content is 3~4g/L.
The additional amount of ammonium bicarbonate described in step (1) is 1.5~2:1 calculating by with fluorine in wastewater mass concentration ratio；Reaction temperature
Degree is 65~80 DEG C, and the reaction time is 1~2h.
Counter-infiltration system operating pressure described in step (2) is 0.8~1.0MPa, and cycles of concentration is 2~3 times.
Washing solid-liquid mass ratio described in step (3) is 1:1.5~2, and washing time is 1~2h, and solid drying temperature is
50~60 DEG C, drying time is 4~6h.
The mixing mass ratio of white carbon black, concentrated water and boric acid described in step (4) is 1.5~2:1.2:1, and reaction temperature is
120~180 DEG C, soaking time be 16~for 24 hours, solid drying temperature be 80~90 DEG C.
Maturing temperature described in step (5) is 500~600 DEG C, 5~7h of calcination time.
Beneficial effects of the present invention:
The invention proposes the processing methods for the fluorine-containing etching waste water containing ammonium.Overall craft of the present invention is simple, handles ring
Border is more mild, makes full use of and has resource in waste water, realizes the disposal of resources of this etching waste water.
Firstly, separate silicon in fluosilicic acid from system with precipitated form silica with the precipitation method, it is related
Technological reaction is NH4HCO3+H2SiF6→SiO2↓+NH4F+CO2↑+H2O, reaction normal reaction heat are 79.638KJ/mol, are
The endothermic reaction, and the free enthalpy difference of standard is -1171913KJ/mol, therefore the reaction spontaneous can carry out to the right.Thus, it is risen in heating
It will increase reaction rate under temperature, while the reaction is gas-liquid-solid reaction, can constantly have CO in treatment process2Gas with
SiO2Precipitating generates, and reaction constantly carries out to the right for irreversible reaction, and as gas continuous bubbling is emerged, and reaction interface is continuous
Update has further speeded up reaction speed.The application will can quickly and efficiently etch fluorine in wastewater silicon by above-mentioned technique as a result,
Acid is converted into white carbon black, and reaction rate is fast, high conversion rate.
Then, in the case that room temperature without phase-change using high pressure counter-infiltration system to waste water carry out desalination, purifying, concentration, with
This reduces subsequent disposition amount.
Finally, the white carbon black of conversion is continued as subsequent technique raw material, and other components ammonium fluoride, organic matter in waste water
Then serve as template and mineralizer, addition boric acid auxiliary collaboration and other components in waste water are changed into together directly and has height and urges
Change the boracic hetero-atom molecular-sieve of performance, what the application was used is high-temperature solvent thermal method, is given up using during confined reaction
Water organic component has assembling ability to nano particle, then after being fired template agent removing, as shown in Figure 3, point of preparation
Son sieve object phase, granular size, in terms of can obtain Effective Regulation.
It is strong that the above process can operate implementation, generates in the process without time useless with secondary waste water, practical function is all good, has good
Good economic benefit and environmental benefit.
Detailed description of the invention
Fig. 1 is process flow chart provided by the invention；
Fig. 2 is that the embodiment of the present invention 1 obtains the schematic diagram of product white carbon black, molecular sieve；
Fig. 3 is high power scanning electron microscope (SEM) photograph of the 1 gained molecular sieve of the embodiment of the present invention under 1 μm.
Specific embodiment
With reference to the accompanying drawings and examples, the present invention is specifically described.
Embodiment 1
A kind of processing method of the fluorine-containing etching waste water containing ammonium, the treating method comprises following steps:
(1) 1 ton of fluorine-containing etching containing ammonium waste water (fluorine content 7.2g/L, ammonia-nitrogen content 3.5g/L) is taken, is stirred at 65 DEG C
Under, by being 1.5:1 to waste water addition ammonium bicarbonate with fluorine in wastewater mass concentration ratio, solid and ammonium fluoride filtrate are obtained after stirring 1h,
The tail gas volatilized in the process is absorbed by aqueous；
(2) ammonium fluoride filtrate is concentrated with tail gas absorption aqueous by counter-infiltration system, system running pressure
0.8Mpa, output fresh water (fluorine content 0.145ppm, ammonia-nitrogen content 0.106ppm) and concentrated water after stoste is concentrated into 2 times；
It (3) is 1:1.5 by solid-liquid mass ratio, step (1) obtained solid is beaten washing 1h by the fresh water obtained by step (2),
The fluorine and ammonium root plasma that solid surface-attached is washed away with this, are then separated by filtration, at wash water recirculation to counter-infiltration system
Reason, solid obtain white carbon black, purity 95.8% after dry 4h at 50 DEG C；
(4) it using white carbon black as silicon source, is added in reverse osmosis output concentrated water ammonium fluoride solution, then boron is added thereto
Acid, three are that 1.5:1.2:1 is stirred and evenly mixed and is placed on 120 DEG C of heat preservation 16h in insulating box in mass ratio, are then filtered, washed,
Molecular sieve crude product is dried to obtain at 80 DEG C；Crude product is roasted to 5h at 500 DEG C up to boracic hetero-atom molecular-sieve B-ZSM-5, purity
98.6%.
Fig. 2 is the schematic diagram of the resulting white carbon black (a) of the present embodiment, molecular sieve (b), it can be seen from the figure that white carbon black
White in appearance superfines, integral particle size distribution is uniform, and by 2404 standard detection of HG/T, its specific surface area be can reach
195m2/ g, tensile strength can reach 24.8MPa, can be used as rubber product and catalyst support material, and the molecule of modified synthesis
It is also white powdered to sieve appearance, powder is fine and smooth loose.
High power scanning electron microscope (SEM) photograph of the 1 gained molecular sieve of Fig. 3 embodiment of the present invention under 1 μm, as seen from Figure 3, molecule
It is in cube shaped for sieving, and surface is relatively smooth, measures correlated performance such as micropore specific surface (439.8m2/ g), bulk density (1.23g/
cm3) etc. be substantially better than irregular serial powder (the micropore specific surface 341.6m of monomer ZSM-5 or some2/g；Bulk density
0.68g/cm3), more excellent catalytic performance can be shown in organic catalytic reaction.
Embodiment 2
A kind of processing method of the fluorine-containing etching waste water containing ammonium, the treating method comprises following steps:
(1) 1.5 tons of fluorine-containing etchings containing ammonium waste water (fluorine content 7.5g/L, ammonia-nitrogen content 3g/L) are taken, are stirred at 75 DEG C
Under, by being 1.8:1 to waste water addition ammonium bicarbonate with fluorine in wastewater mass concentration ratio, solid is obtained after stirring 1.5h and ammonium fluoride is filtered
Liquid, the tail gas volatilized in the process are absorbed by aqueous；
(2) ammonium fluoride filtrate is concentrated with tail gas absorption aqueous by counter-infiltration system, system running pressure
0.95Mpa, output fresh water (fluorine content 0.098ppm, ammonia-nitrogen content 0.36ppm) and concentrated water after stoste is concentrated into 2.5 times；
It (3) is 1:1.8 by solid-liquid mass ratio, step (1) obtained solid is beaten and washes by the fresh water obtained by step (2)
1.5h is washed away the fluorine and ammonium root plasma of solid surface-attached with this, is then separated by filtration, wash water recirculation to reverse osmosis system
System processing, solid obtain white carbon black, purity 97.4% after dry 5h at 56 DEG C；
(4) it using white carbon black as silicon source, is added in reverse osmosis output concentrated water ammonium fluoride solution, then boron is added thereto
Acid, three are that 1.7:1.2:1 is stirred and evenly mixed and is placed on 160 DEG C of heat preservation 20h in insulating box in mass ratio, are then filtered, washed,
Molecular sieve crude product is dried to obtain at 85 DEG C.Crude product is roasted to 6h at 550 DEG C up to boracic hetero-atom molecular-sieve B-ZSM-5, purity
97.9%.
Gained white carbon black white in appearance superfines, integral particle size distribution is uniform, by 2404 standard detection of HG/T
Its specific surface area can reach 206m2/ g, tensile strength can reach 26.1MPa, can be used as rubber product and catalyst support material.
And the molecular sieve appearance of modified synthesis is also white powdered, powder is fine and smooth loose, after measured correlated performance such as micropore specific surface
(429.7m2/ g), bulk density (1.16g/cm3) etc. be substantially better than the irregular serial powder (micropore of monomer ZSM-5 or some
Specific surface 340.8m2/g；Bulk density 0.62g/cm3), more excellent catalytic can be shown in organic catalytic reaction
Energy.
Embodiment 3
A kind of processing method of the fluorine-containing etching waste water containing ammonium, the treating method comprises following steps:
(1) 2 tons of fluorine-containing etchings containing ammonium waste water (fluorine content 7.8g/L, ammonia-nitrogen content 3.75g/L) are taken, are stirred at 80 DEG C
Under, by being 2:1 to waste water addition ammonium bicarbonate with fluorine in wastewater mass concentration ratio, solid and ammonium fluoride filtrate, mistake are obtained after stirring 2h
The tail gas volatilized in journey is absorbed by aqueous；
(2) ammonium fluoride filtrate is concentrated with tail gas absorption aqueous by counter-infiltration system, system running pressure
1.0Mpa, output fresh water (fluorine content 0.216ppm, ammonia-nitrogen content 0.028ppm) and concentrated water after stoste is concentrated into 3 times；
(3) it is 1:2 by solid-liquid mass ratio, above-mentioned solid is beaten washing 2h using this fresh water, the surface of solids is washed away with this
The fluorine and ammonium root plasma of attachment, are then separated by filtration, and wash water recirculation to counter-infiltration system processing, solid is done at 60 DEG C
White carbon black, purity 98.5% are obtained after dry 6h；
(4) it using white carbon black as silicon source, is added in reverse osmosis output concentrated water ammonium fluoride solution, then boron is added thereto
Acid, three are that 2:1.2:1 is stirred and evenly mixed and is placed in insulating box 180 DEG C of heat preservations for 24 hours in mass ratio, are then filtered, washed, 90
Molecular sieve crude product is dried to obtain at DEG C.Crude product is roasted to 7h at 600 DEG C up to boracic hetero-atom molecular-sieve B-ZSM-5, purity
99.2%.
Gained white carbon black white in appearance superfines, integral particle size distribution is uniform, by 2404 standard detection of HG/T
Its specific surface area can reach 199.8m2/ g, tensile strength can reach 25.7MPa, can be used as rubber product and catalyst carrier is former
Material.And the molecular sieve appearance of modified synthesis is also white powdered, powder is fine and smooth loose, and correlated performance such as micropore compares table after measured
Face (437.8m2/ g), bulk density (1.287g/cm3) etc. to be substantially better than the irregular serial powder of monomer ZSM-5 or some (micro-
Hole specific surface 342m2/g；Bulk density 0.637g/cm3), more excellent catalytic can be shown in organic catalytic reaction
Energy.
Claims (7)
1. a kind of processing method of the fluorine-containing etching waste water containing ammonium, which is characterized in that the treating method comprises following steps:
(1) ammonium bicarbonate is added into waste water under heating stirring, is separated by solid-liquid separation after mixing reaction, the tail gas volatilized in the process passes through
Water absorbs；
(2) it will be separated by solid-liquid separation gained filtrate in step (1) to be concentrated together with the aqueous for absorbing tail gas by counter-infiltration system, makes
Obtain fresh water and concentrated water；
(3) it is washed to obtained solid is separated by solid-liquid separation in step (1) using fresh water obtained by step (2), washes rear solid through drying
After obtain white carbon black, wash water recirculation to reverse osmosis treatment；
(4) white carbon black obtained in step (3) is added in step (2) resulting concentrated water, adds boric acid and stir and evenly mix, sets
The insulation reaction under isoperibol is then filtered, is dried；
(5) obtained solid after step (4) drying is roasted to get boracic hetero-atom molecular-sieve.
2. processing method according to claim 1, which is characterized in that the fluorine in wastewater content is 7~8g/L, and ammonia nitrogen contains
Amount is 3~4g/L.
3. processing method according to claim 1, which is characterized in that the additional amount of ammonium bicarbonate described in step (1) presses and gives up
Fluorine mass concentration ratio is 1.5~2:1 calculating in water；Reaction temperature is 65~80 DEG C, and the reaction time is 1~2h.
4. processing method according to claim 1, which is characterized in that counter-infiltration system operating pressure described in step (2)
For 0.8~1.0MPa, cycles of concentration is 2~3 times.
5. processing method according to claim 1, which is characterized in that washing solid-liquid mass ratio described in step (3) is 1:
1.5~2, washing time is 1~2h, and solid drying temperature is 50~60 DEG C, and drying time is 4~6h.
6. processing method according to claim 1, which is characterized in that white carbon black described in step (4), concentrated water and boric acid
Mixing mass ratio be 1.5~2:1.2:1, reaction temperature be 120~180 DEG C, soaking time be 16~for 24 hours, solid drying temperature
It is 80~90 DEG C.
7. processing method according to claim 1, which is characterized in that maturing temperature described in step (5) is 500~600
DEG C, 5~7h of calcination time.
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|---|---|---|---|---|
| CN110745832A (en) * | 2019-11-29 | 2020-02-04 | 河南骏化发展股份有限公司 | Water-saving device and process for producing white carbon black by precipitation method |
| CN113023749A (en) * | 2021-03-15 | 2021-06-25 | 盛隆资源再生（无锡）有限公司 | Method for resource utilization of etching process waste |
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