CN110092401A - A method of calcirm-fluoride and ammonium sulfate are prepared using fluorine-containing nitrogen-containing wastewater - Google Patents
A method of calcirm-fluoride and ammonium sulfate are prepared using fluorine-containing nitrogen-containing wastewater Download PDFInfo
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- CN110092401A CN110092401A CN201910489821.9A CN201910489821A CN110092401A CN 110092401 A CN110092401 A CN 110092401A CN 201910489821 A CN201910489821 A CN 201910489821A CN 110092401 A CN110092401 A CN 110092401A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/24—Sulfates of ammonium
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- 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
- C01F11/20—Halides
- C01F11/22—Fluorides
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- 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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- 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
- C01P2006/82—Compositional purity water content
Abstract
The invention discloses a kind of methods for preparing calcirm-fluoride and ammonium sulfate using fluorine-containing nitrogen-containing wastewater, the described method comprises the following steps: (1) removing the COD in waste water, obtain solution A；(2) calcium salt mashing is added in step (1) acquired solution A, calcirm-fluoride and solution B is obtained by filtration；(3) pH of regulating step (2) acquired solution B, obtains solution C；(4) solution C obtains ammonium sulfate crystallization using drying equipment after concentration and cooling.The method of the present invention is simple, easy to operate, and the maximization for realizing fluorine nitrogen resource recycles, and realizes economic benefit and environmental benefit perfect unity.
Description
Technical field
The present invention relates to waste water recycling device technical fields, prepare fluorine by fluorine-containing nitrogen-containing wastewater more particularly, to one kind
Change the method for calcium and ammonium sulfate.
Background technique
Electronics industry usually will use a large amount of acid in production process, alkali and organic matter etc., wherein hydrofluoric acid, ammonium hydroxide, have
The a large amount of chemical agent such as solvent is using more and more extensive, so that the fluorine-containing waste water containing ammonia nitrogen of discharge is more and more, aggravation
China's water pollution and shortage of water resources situation sternly complete degree, so the processing method of the fluorine-containing nitrogen-containing wastewater of electronics industry is urgently
Wait need to study.
CN102126806 A discloses a kind of method of fluorine-containing nitrogen-containing wastewater fully recovering of electronics industry, in this method
By the mineralized nitrogen of system it is that nitrogen removes using oxidizer containing chlorine, leads to nitrogen resource direct losses, and remaining solution passes through
Addition soluble calcium salt reacts in neutral conditions generates calcirm-fluoride, and remaining chloride ion is directly entered water process system in system
System, causes the waste of vast resources.CN201309866Y discloses a kind of using " disk filtering-ultra-filtration membrane device-centre water
The waste water recycling processing unit of case-security personnel filtering-reverse osmosis " technique, but cartridge filter blocking is frequently, needs to be replaced frequently,
Increase production cost, in addition, reverse osmosis membrane cleaning effect is bad, service life is shorter.
In order to realize the recycling of resource, and process conditions are simple, realize the maximization recycling of fluorine nitrogen resource
It utilizes, reduces the processing cost of waste liquid, designing a kind of for fluorine-containing is very necessary containing ammonia nitrogen recycling calcirm-fluoride and ammonium sulfate
's.
Summary of the invention
In view of the above-mentioned problems existing in the prior art, the present invention provides it is a kind of using it is fluorine-containing containing ammonia nitrogen prepare calcirm-fluoride and
The method of ammonium sulfate.The method of the present invention is simple, easy to operate, realize fluorine nitrogen resource maximization recycle, realize through
Benefit of helping and environmental benefit perfect unity.
Technical scheme is as follows:
A method of calcirm-fluoride and ammonium sulfate being prepared using fluorine-containing nitrogen-containing wastewater, the described method comprises the following steps:
(1) COD in waste water is removed, solution A is obtained；
The method of COD uses peroxide passivation in the removal waste water, and the pH of waste water specific steps: is adjusted to 7 with ammonium hydroxide
Hydrogen peroxide is slowly added in~9, Xiang Suoshu waste water, reaction to solution bubble-free generates, and obtains solution A；Reaction temperature be 60~
80 DEG C, the hydrogen peroxide mass fraction is 20~30%, and hydrogen peroxide additional amount is the 0.3~0.5% of wastewater volume, reaction time
For 1~2h.
(2) calcium salt mashing is added in step (1) acquired solution A, calcirm-fluoride and solution B is obtained by filtration；The calcium salt is sulphur
Sour calcium or lime；The dosage of the calcium salt is calcium fluorine 1.1~1.5:2 of molar ratio, and beating time is 1~3h, washs function using band
Can filter press filtration washing obtain solid fluorinated calcium, the washing water reuse generated in the process is to being beaten link.
(3) pH of regulating step (2) acquired solution B, obtains solution C；With sulfuric acid, ammonium hydrogen carbonate, ammonium carbonate or ammonium hydroxide tune
Save pH to 5~7
(4) solution C obtains ammonium sulfate crystallization using drying equipment after concentration and cooling.The concentration condition is 90
~110 DEG C, vacuum degree is 0.04~0.08MPa, and being concentrated into liquid specific gravity is 1.32~1.34g/mL, and cooling temperature is 20~30
DEG C, drying equipment selects Vibratingfluidbeddrier.
Preferred embodiment, the method that COD in waste water is removed described in step (1) use burgy method, the specific steps are as follows:
(1) 10g active carbon is added to 80mL nitric acid solution, heating reaction is dried after reaction, obtains modified powder
Charcoal；The nitric acid solution concentration is 4~5mol/L, and reaction temperature is 50~60 DEG C, and drying temperature is 110~120 DEG C, when dry
Between be 2~3 hours.
(2) pH of waste water sulfuric acid or ammonium hydroxide are adjusted in 3~6, Xiang Suoshu waste water to be added described in step (1) and are modified
Burgy stirs 1~3h, and the ie in solution that filters to get filtrate A, filtered time useless burgy can be reused by electrolytic regeneration；Institute
Stating sulfuric acid mass fraction is 10%~30%, and ammonium hydroxide mass fraction is 10%~30%, and the modified burgy mass fraction is 0.1
~0.2wt%.
The present invention is beneficial to be had the technical effect that
In order to realize the abundant recycling of resource, the applicant is by a large amount of experiment, a kind of utilization for designing
The fluorine-containing method for preparing calcirm-fluoride and ammonium sulfate containing ammonia nitrogen.The fairly simple method of this technology utilization carries out, first with burgy
Or the method for hydrogen peroxide removes organic matter, adds the sl. sol. calcium salt reaction such as lime or calcium sulfate, generates the fluorination of indissoluble
Calcium, can be obtained the higher calcirm-fluoride of purity, cleaning solution reuse after washing, the solution after separating fluorine is added acid or alkali, uses bicarbonate
Ammonia or ammonium carbonate adjust pH, obtain corresponding ammonium salt, and method is simple, easy to operate, realize the maximization recycling of fluorine nitrogen resource
It utilizes, realizes economic benefit and environmental benefit perfect unity.
Detailed description of the invention
Fig. 1 is present invention process flow diagram.
Specific embodiment
With reference to the accompanying drawings and examples, the present invention is specifically described.
Embodiment 1
The fluorine-containing nitrogen-containing wastewater 200mL (fluorine content 16g/L, ammonia-nitrogen content 22g/L) of certain electronics producer production line is taken, is used
0.1% burgy is added in sulfuric acid regulation solution pH=3, stirs 1.5h, filtering, and secondary useless send to electrolytic tank electrolysis regenerates, and filtrate is added
The mashing of 12.6g calcium sulfate, additional amount is that calcium fluorine ratio is 1.1:2, after stirring 1h, after filters pressing, after filter cake is washed using filter press
6.61g fluorination calcium product is obtained, filtrate is after ammonium hydroxide adjusts pH=5, at 90 DEG C of temperature and vacuum degree 0.04MPa, evaporation
It is 1.32g/mL to concentrate specific gravity, is cooled to 20 DEG C, centrifugation obtains 16.12g ammonium sulfate crystallization, and filter press cleaning solution is for beating
Starch link.The present embodiment burgy passes through modification, i.e., 10g active carbon is added to 80mL nitric acid solution, heating reaction, reaction
After it is dry, obtain modified burgy.
Embodiment 2
The fluorine-containing nitrogen-containing wastewater 200mL (fluorine content 15g/L, ammonia-nitrogen content 20g/L) of certain electronics producer production line is taken, is used
Ammonium hydroxide adjusts pH value of solution=5, and 0.2% burgy is added, and stirs 2.5h, filtering, and secondary useless send to electrolytic tank electrolysis regenerates, and filtrate is added
The mashing of 7.59g lime, additional amount is that calcium fluorine ratio is 1.3:2, and after stirring 2h, after filters pressing, filter cake obtains after washing using filter press
It is fluorinated calcium product to 6.18g, filtrate at 100 DEG C of temperature and vacuum degree 0.06MPa, is evaporated to after persulfuric acid adjusts pH=6
Concentrate specific gravity is 1.33g/mL, is cooled to 25 DEG C, centrifugation obtains 14.18g ammonium sulfate crystallization, and filter press cleaning solution is for being beaten
Link.The present embodiment burgy passes through modification, i.e., 10g active carbon is added to 80mL nitric acid solution, heating reaction, reaction knot
It is dry after beam, obtain modified burgy.
Embodiment 3
The fluorine-containing nitrogen-containing wastewater 200mL (fluorine content 18g/L, ammonia-nitrogen content 25g/L) of certain electronics producer production line is taken, is surveyed
Determine stoste pH=8,0.4% hydrogen peroxide is added, after the water-bath that temperature is 70 DEG C stirs 1.5h, 10.52g lime is added and beats
Slurry, additional amount is that calcium fluorine ratio is 1.5:2, and after stirring 3h, after filters pressing, filter cake obtains 7.44g fluorination after washing using filter press
Calcium product, filtrate at 110 DEG C of temperature and vacuum degree 0.08MPa, are evaporated to concentrate ratio after ammonium carbonate adjusts pH=7
Weight is 1.34g/mL, is cooled to 30 DEG C, centrifugation obtains 18.39g ammonium sulfate crystallization, and filter press cleaning solution is for being beaten link.
Each raw material cited by the present invention can realize that the bound value of the present invention and each raw material, interval value can
It realizes the present invention, embodiment is just not listed one by one herein.The bound of technological parameter (such as temperature, time) of the invention takes
Value, interval value can realize the present invention, embodiment numerous to list herein.
Detect example:
The indexs of correlation such as calcirm-fluoride that Examples 1 to 3 recycles and ammonium sulfate purity are as shown in table 1.Purity in table 1
It is mass fraction.
Table 1
It can see from the data of table 1, for the calcirm-fluoride purity that the present invention recycles all 98% or more, other indexs are full
Sufficient national standard GB/T 27804-2011 requirement, total sulfur content is 0.5% or so, and for ammonium sulfate purity 98% or more, index meets state
Mark GB 535-1995 requirement.
Claims (9)
1. a kind of method for preparing calcirm-fluoride and ammonium sulfate using fluorine-containing nitrogen-containing wastewater, which is characterized in that the method includes
Following steps:
(1) COD in waste water is removed, solution A is obtained；
(2) calcium salt mashing is added in step (1) acquired solution A, calcirm-fluoride and solution B is obtained by filtration；
(3) pH of regulating step (2) acquired solution B, obtains solution C；
(4) solution C obtains ammonium sulfate crystallization using drying equipment after concentration and cooling.
2. the method according to claim 1, wherein the method for COD uses in removal waste water described in step (1)
Burgy method, the specific steps are as follows:
(1) 10g active carbon is added to 80mL nitric acid solution, heating reaction is dried after reaction, obtains modified burgy；
(2) pH of waste water sulfuric acid or ammonium hydroxide are adjusted in 3~6, Xiang Suoshu waste water and modified powder described in step (1) is added
Charcoal stirs 1~3h, and the ie in solution that filters to get filtrate A, filtered time useless burgy can be reused by electrolytic regeneration.
3. according to the method described in claim 2, it is characterized in that, nitric acid solution concentration described in step (1) is 4~5mol/
L, reaction temperature are 50~60 DEG C, and drying temperature is 110~120 DEG C, and drying time is 2~3 hours.
4. according to the method described in claim 2, it is characterized in that, sulfuric acid mass fraction described in step (2) be 10%~
30%, ammonium hydroxide mass fraction is 10%~30%, and the modified burgy mass fraction is 0.1~0.2wt%.
5. the method according to claim 1, wherein the method for COD uses in removal waste water described in step (1)
Peroxide passivation, specific steps: the pH of waste water being adjusted in 7~9, Xiang Suoshu waste water with ammonium hydroxide and is slowly added to hydrogen peroxide, reaction
It is generated to solution bubble-free, obtains solution A.
6. according to the method described in claim 5, it is characterized in that, the reaction temperature be 60~80 DEG C, the dioxygen water quality
Measuring score is 20%~30%, and hydrogen peroxide additional amount is the 0.3~0.5% of wastewater volume, and the reaction time is 1~2h.
7. the method according to claim 1, wherein calcium salt described in step (2) is calcium sulfate or lime；It is described
The dosage of calcium salt is calcium fluorine 1.1~1.5:2 of molar ratio, and beating time is 1~3h, crosses diafiltration using filter press with washing function
Wash to obtain solid fluorinated calcium, the washing water reuse generated in the process is to being beaten link.
8. the method according to claim 1, wherein the middle sulfuric acid of step (3), ammonium hydrogen carbonate, ammonium carbonate or ammonia
Water adjusts pH to 5~7.
9. the method according to claim 1, wherein concentration condition described in step (4) is 90~110 DEG C, very
Reciprocal of duty cycle is 0.04~0.08MPa, and being concentrated into liquid specific gravity is 1.32~1.34g/mL, and cooling temperature is 20~30 DEG C, and drying is set
Alternatively use Vibratingfluidbeddrier.
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| CN201910489821.9A CN110092401A (en) | 2019-06-06 | 2019-06-06 | A method of calcirm-fluoride and ammonium sulfate are prepared using fluorine-containing nitrogen-containing wastewater |
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Cited By (1)
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