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CN110104864A - A kind of processing method of the fluorine-containing ammonia-containing water of acid phosphorus acid type - Google Patents

A kind of processing method of the fluorine-containing ammonia-containing water of acid phosphorus acid type Download PDF

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Publication number
CN110104864A
CN110104864A CN201910489867.0A CN201910489867A CN110104864A CN 110104864 A CN110104864 A CN 110104864A CN 201910489867 A CN201910489867 A CN 201910489867A CN 110104864 A CN110104864 A CN 110104864A
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reactor tank
tank
cucurbit
fluorine
tetrafluoro
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CN201910489867.0A
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陈琪
方稳
钊现花
刘秋月
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Shenglong Resource Regeneration (wuxi) Co Ltd
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Shenglong Resource Regeneration (wuxi) Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34Chemical or biological purification of waste gases
    • B01D53/46Removing components of defined structure
    • B01D53/68Halogens or halogen compounds
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34Chemical or biological purification of waste gases
    • B01D53/74General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/80Semi-solid phase processes, i.e. by using slurries
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B25/00Phosphorus; Compounds thereof
    • C01B25/16Oxyacids of phosphorus; Salts thereof
    • C01B25/26Phosphates
    • C01B25/45Phosphates containing plural metal, or metal and ammonium
    • C01B25/451Phosphates containing plural metal, or metal and ammonium containing metal and ammonium
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F9/00Multistage treatment of water, waste water or sewage
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2257/00Components to be removed
    • B01D2257/20Halogens or halogen compounds
    • B01D2257/204Inorganic halogen compounds
    • B01D2257/2047Hydrofluoric acid
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/001Processes for the treatment of water whereby the filtration technique is of importance
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/02Treatment of water, waste water, or sewage by heating
    • C02F1/04Treatment of water, waste water, or sewage by heating by distillation or evaporation
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/02Treatment of water, waste water, or sewage by heating
    • C02F1/04Treatment of water, waste water, or sewage by heating by distillation or evaporation
    • C02F1/043Details
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/66Treatment of water, waste water, or sewage by neutralisation; pH adjustment
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/10Inorganic compounds
    • C02F2101/105Phosphorus compounds
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/10Inorganic compounds
    • C02F2101/12Halogens or halogen-containing compounds
    • C02F2101/14Fluorine or fluorine-containing compounds
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/10Inorganic compounds
    • C02F2101/16Nitrogen compounds, e.g. ammonia
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2209/00Controlling or monitoring parameters in water treatment
    • C02F2209/02Temperature
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2209/00Controlling or monitoring parameters in water treatment
    • C02F2209/06Controlling or monitoring parameters in water treatment pH

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Biomedical Technology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Water Supply & Treatment (AREA)
  • Inorganic Chemistry (AREA)
  • Removal Of Specific Substances (AREA)

Abstract

The present invention provides a kind of processing methods of fluorine-containing ammonia-containing water of acid phosphorus acid type, and described method includes following steps: (1) fluorine-containing ammonia-containing water being placed in home-made contrivance, heating distillation enters hydrogen fluoride in reactor tank;(2) after reaching critical setting value by detector detection hydrogen fluoride gas concentration, magnesia slurry is pumped into reactor tank, and dispersion slurries come into full contact with hydrogen fluoride gas to react;(3) it by mixed material finally formed in reactor tank, stirs and evenly mixs, filters, dries to obtain magnesium fluoride;(4) by magnesia slurry again with remain waste water in cucurbit in step (3) and stir and evenly mix, add ammonium hydroxide, filtering, dry ammonium magnesium phosphate.Integrated artistic of the present invention is simple, makes effective use of and has resource and each component performance difference in waste water, realizes the reasonable resource disposition of this waste water step by step, it can be achieved that continuity operates, and treatment effeciency is high, and generates in the process without time useless and secondary pollution.

Description

A kind of processing method of the fluorine-containing ammonia-containing water of acid phosphorus acid type
Technical field
This application involves industrial waste water treatment more particularly to a kind of places of the fluorine-containing ammonia-containing water of acid phosphorus acid type Reason method.
Background technique
As semiconductor industry is quickly grown, especially often used in electronics industry production process hydrofluoric acid, phosphoric acid, The a large amount of chemical agent such as ammonium hydroxide, organic solvent, consequent are that secondary waste water contains and largely toxic to surrounding enviroment has Evil ingredient, then exacerbates the severity of China's water pollution and shortage of water resources.
The above waste water is big with total amount, system complicated component, pollution is strong, biodegradability is poor, fluoride and ammonia-nitrogen content High feature.Traditional treatment method is by fluorine in wastewater, ammonia nitrogen removal or to be reduced to a certain extent rear qualified discharge.Simple contains Fluorine waste water mainly uses chemical precipitation method, absorption method, and freezing, ultrafiltration method for removing fluor, electroosmose process etc. be because of input cost height, and Low efficiency, deficiency in economic performance and less popularization.For ammonia nitrogen waste water then mainly using blow-off method, biochemical method, chemical precipitation method etc. Some more effective methods.But high-concentration fluorine-contained composite wastes containing ammonia nitrogen numerous for system ingredient as above, conventional treatment Method may be unable to reach expected removal effect in actual use.In addition, for fluorine-containing useless containing ammonia nitrogen under acid phosphatase system The treatment research of water is also relatively fewer.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of processing of fluorine-containing ammonia-containing water of acid phosphorus acid type by the application Method.Overall craft of the present invention is simple, and treatment conditions are more mild, makes full use of and has resource in waste water, under normal conditions Implementation can be operated, realize the reasonable disposition of waste water step by step, while being generated in the process without time useless and secondary waste water, dispose effect It is all good.
Technical scheme is as follows:
A kind of processing system of the fluorine-containing ammonia-containing water of acid phosphorus acid type, the processing system include cucurbit (1), reactor tank (3), elevator pump (4), pretreatment tank (5);
Cucurbit (1) bottom is furnished with electric heating cover (2), and bottleneck is furnished with motor (6) and tetrafluoro connector (7);
Equipped with detector (10), motor (12) and nozzle (13) at the top of the reactor tank (3);
It are furnished with motor (15) at the top of the pretreatment tank (5);
The cucurbit (1) is connected to by tetrafluoro connector (7) and tetrafluoro straight tube (8) with reactor tank (3);The tetrafluoro straight tube (8) fixed using fixed bracket (9);
The reactor tank (3) is connected to by elevator pump (4) with pretreatment tank (5).
The cucurbit (1), reactor tank (3) and pretreatment tank (5) capacity are 5L;The reactor tank (3) is carbon steel Fluorine-lined material, pretreatment tank (5) are stainless steel material, and tank body material thickness is 8mm.
Polypropylene plastics nozzle (13) are installed at reactor tank (3) end socket, and are equipped with detector (10), are examined Survey range is 0~100ppm.
The cucurbit (1), reactor tank (3), pretreatment tank (5) three are equipped with blender, and material is consistent with tank body, and Motor (6), (12), the revolving speed of (15) is adjustable, and 0~40 rev/min of range.
The heated hydrogen fluoride gas (11) evaporated of waste water is straight through tetrafluoro connector (7) and tetrafluoro in the cucurbit (1) It manages (8) to enter in reactor tank (3), issues response signal by detector (10), reach elevator pump (4) after setting critical value Starting will pre-process tank (5) in mixing magnesia slurry (14) is pumped into reactor tank, it is evenly dispersed through nozzle (13) and and fluorine Change hydrogen (11) to come into full contact with, stir and evenly mix, is closed lower than elevator pump (4) after critical value and stop charging.
A kind of method of the processing system processing fluorine-containing ammonia-containing water of acid phosphorus acid type, the method includes walking as follows It is rapid:
(1) it adds waste water into tetrafluoro cucurbit, the fixed tetrafluoro cucurbit is placed in above electric heating cover, uses tetrafluoro It is connected and is fixed with reactor tank by connector, straight tube;
(2) magnesia is put into pretreatment tank, adds water and stirs mixing and forms slurries;
(3) electric heating cover is opened, waste water in cucurbit is heated, the volatilization of fluorine in wastewater hydrogen enters reactor tank by straight tube In, it is detected using detector, after hydrogen fluoride gas concentration reaches critical setting value, promotes pump startup and by step (2) Prepared magnesia slurry is pumped into reactor tank, controls its flow velocity, keeps slurries abundant using the nozzle being arranged inside reactor tank Hydrogen fluoride gas is contacted and absorbs, until gas detection closes elevator pump after being lower than critical setting value;
(4) by finally formed mixed material in step (3) described reactor tank, continue to stir and evenly mix, blowing filtering is dried It does to get magnesium fluoride;
(5) magnesia slurry prepared by step (2) is pumped into step (3) to distill in resulting mother liquor, is stirred and evenly mixed, and Ammonium hydroxide is added and adjusts pH, filtering, drying are to get ammonium magnesium phosphate.
The fluorine in wastewater content is 8~9g/L, and ammonia-nitrogen content is 5~6g/L, 40~50wt% of phosphoric acid quality concentration;Step Suddenly it is 1:1.5~2 that (2) described magnesia, which mixes solid-liquid mass ratio with water, and stirring and evenly mixing the time is 1~2h.
Electric heating cover set temperature described in step (3) is 30~40 DEG C;The critical setting value of hydrogen fluoride gas be 0.5~ 1ppm;Magnesia mixed liquor feed flow rate is 20~30L/h;When mixed material stirs and evenly mixs in reactor tank described in step (4) Between be 1~2h, solid drying temperature be 60~70 DEG C, drying time be 3~5h.
The ammoniacal liquor mass concentration used described in step (5) is 30~40wt%, and pH is adjusted to 5~6, is persistently stirred to react 2~3h of time, solid drying temperature are 80~90 DEG C, and drying time is 6~8h.
The present invention is beneficial to be had the technical effect that
The present invention handles this fluorine-containing ammonia-containing water of acid phosphorus acid type using homemade device.As shown in Fig. 1, firstly, it is sharp With each component boiling point difference in waste water, by distilling, by fluorine in wastewater component, evaporation divides from system in the form of hydrogen fluoride gas From then using detector offer signal, foundation and the long-range interlocking between elevator pump, i.e., when detection hydrogen fluoride gas concentration After reaching critical setting value, elevator pump voluntarily starts and injects magnesia slurry in time, until gas concentrations are lower than setting value After be automatically stopped, while using nozzle it is evenly dispersed to slurries, to the abundant spray-absorption of hydrogen fluoride gas react.Pass through as a result, This design device, can not only realize that fluorination reaction is automatically continuously run, but also reacted in the way of this spray, it is possible to increase object Phase-contact surface and improve reaction rate and conversion ratio, and then magnesium fluoride superfine powder is obtained by gas-liquid-solid reaction. Finally, in waste water remaining ingredient phosphorus, ammonia can again in conjunction with magnesia slurry, finally can isochronous resources obtain ammonium phosphate magnesium powder End.
Overall craft of the present invention is simple, and treatment conditions are more mild, makes full use of and has resource in waste water, in normal condition Under implementation can be operated, realize the reasonable disposition of waste water step by step, while generating in the process without time useless with secondary waste water, disposition effect Fruit is all good.
Detailed description of the invention
Fig. 1 is self-control processing unit schematic diagram provided by the invention;
In figure, 1, cucurbit, 2, electric heating cover, 3, reactor, 4, elevator pump, 5, pretreatment tank, 6/12/15, motor, 7, Tetrafluoro connector, 8, tetrafluoro straight tube, 9, fixed bracket, 10, detector, 11, hydrogen fluoride gas, 13, nozzle, 14/16, oxidation Magnesium slurries.
Fig. 2 is the schematic diagram of products obtained therefrom magnesium fluoride, ammonium magnesium phosphate in embodiment 1
Specific embodiment
With reference to the accompanying drawings and examples, the present invention is specifically described.
Referring to Fig.1, processing unit, i.e., a kind of processing system of the fluorine-containing ammonia-containing water of acid phosphorus acid type, the processing are made by oneself System includes cucurbit 1, reactor tank 3, elevator pump 4, pretreatment tank 5;
1 bottom of cucurbit is furnished with electric heating cover 2, and bottleneck is furnished with motor 6 and tetrafluoro connector 7;
It is furnished with detector 10, motor 12 and nozzle 13 at the top of the reactor tank 3;
It is furnished with motor 15 at the top of the pretreatment tank 5;
The cucurbit 1 is connected to by tetrafluoro connector 7 and tetrafluoro straight tube 8 with reactor tank 3;The tetrafluoro straight tube 8 is using solid Fixed rack 9 is fixed;
The reactor tank 3 is connected to by elevator pump 4 with pretreatment tank 5.
The cucurbit 1, reactor tank 3 and pretreatment 5 capacity of tank are 5L;The reactor tank 3 is carbon steel Fluorine-lined material, Pretreatment tank 5 is stainless steel material, and tank body material thickness is 8mm.
Polypropylene plastics nozzle 13 is installed at 3 end socket of reactor tank, and is equipped with detector 10, detection range For 0~100ppm.
The cucurbit 1, reactor tank 3, pretreatment 5 three of tank are equipped with blender, and material is consistent with tank body, and motor 6, 12,15 revolving speed is adjustable, and 0~40 rev/min of range.
The heated hydrogen fluoride gas 11 evaporated of waste water enters through tetrafluoro connector 7 and tetrafluoro straight tube 8 in the cucurbit 1 In reactor tank 3, response signal is issued by detector 10, the starting of elevator pump 4 will pre-process tank 5 after reaching setting critical value The magnesia slurry 14 of middle mixing is pumped into reactor tank, evenly dispersed through nozzle 13 and come into full contact with, stir with hydrogen fluoride gas 11 Mixing is mixed, is closed lower than elevator pump 4 after critical value and stops charging.
Embodiment 1
A kind of processing method of the fluorine-containing ammonia-containing water of acid phosphorus acid type, the treating method comprises following steps:
(1) in home-made contrivance, 1L waste water (fluorine content 8.5g/L, ammonia-nitrogen content 5.6g/L, phosphoric acid quality concentration are taken It 40.5wt%) puts into tetrafluoro cucurbit, while magnesia and water being added in pretreatment tank for 1:1.5 by solid-liquid mass ratio, It stirs and evenly mixs 1h and obtains magnesia slurry 1L;
(2) 30 DEG C of jacket temperature are set, cucurbit is heated, makes fluorine in wastewater component in the form of hydrogen fluoride gas through tetrafluoro Connector, straight tube enter in reactor tank;
(3) it after the detector detection hydrogen fluoride concentration that reactor tank is equipped with reaches critical setting value 0.5ppm, is promoted Magnesia slurry is pumped into reactor tank by pump startup, and controlling its feed flow rate is 20L/h, utilizes the nozzle being arranged inside reactor tank It is set to come into full contact with absorption hydrogen fluoride gas, until gas concentration is then reacted lower than heating and slurry feed is stopped after critical value In-tank mixing material continues to stir and evenly mix 1h, and then blowing is filtered, washed, and obtains magnesium fluoride, purity after 3h is dried at 60 DEG C 98.9%.As shown in attached drawing 2 (a), gained magnesium fluoride is pure white superfine powder, is detected granularity and reaches 280 mesh, product is fine and smooth Without obvious impurity, it can be used for the reagents raw material such as ceramics, metal smelt;
(4) starting elevator pump is pumped into magnesia slurry, under stiring mixes well it with distillation tail water, uses in the process Mass concentration is that 30wt% ammonium hydroxide adjusts pH to 5, then continues to be stirred to react 2h, then be filtered, washed, dries 6h at 80 DEG C Ammonium magnesium phosphate, purity 94.6% are obtained afterwards.As shown in attached drawing 2 (b), gained ammonium magnesium phosphate is white particle, through object phase, structural characterization Analysis, product composition composition is single, and no other objects mutually mix, and crystalline structure is good, and integral particle size distribution is uniform, can be used for Fertilizer and water process reagent.
Embodiment 2
A kind of processing method of the fluorine-containing ammonia-containing water of acid phosphorus acid type, the treating method comprises following steps:
(1) in home-made contrivance, 1.5L waste water (fluorine content 8g/L, ammonia-nitrogen content 6g/L, phosphoric acid quality concentration are taken It 45wt%) puts into tetrafluoro cucurbit, while being 1:1.8 by magnesia and water addition pretreatment tank by solid-liquid mass ratio, stir It mixes mixing 1.5h and obtains magnesia slurry 1.5L;
(2) 35 DEG C of jacket temperature are set, cucurbit is heated, makes fluorine in wastewater component in the form of hydrogen fluoride gas through tetrafluoro Connector, straight tube enter in reactor tank;
(3) it after the detector detection hydrogen fluoride concentration that reactor tank is equipped with reaches critical setting value 0.6ppm, is promoted Magnesia slurry is pumped into reactor tank by pump startup, and controlling its feed flow rate is 24L/h, utilizes the nozzle being arranged inside reactor tank It is set to come into full contact with absorption hydrogen fluoride gas, until gas concentration is then reacted lower than heating and slurry feed is stopped after critical value In-tank mixing material continues to stir and evenly mix 1.5h, and then blowing is filtered, washed, and obtains magnesium fluoride, purity after 4h is dried at 65 DEG C 99.1%.Gained magnesium fluoride is pure white superfine powder, is detected granularity and reaches 320 mesh, product exquisiteness can be used without obvious impurity In the reagents raw material such as ceramics, metal smelt;
(4) starting elevator pump is pumped into magnesia slurry, under stiring mixes well it with distillation tail water, uses in the process Mass concentration is that 35wt% ammonium hydroxide adjusts pH to 5.6, then continues to be stirred to react 2.5h, then be filtered, washed, dries at 85 DEG C Ammonium magnesium phosphate, purity 95.3% are obtained after dry 7h.Gained ammonium magnesium phosphate be white particle, through object phase, structural characterization analyze, product at It is grouped as single, no other objects mutually mix, and crystalline structure is good, and integral particle size distribution is uniform, can be used for fertilizer and Shui Chu Manage reagent.
Embodiment 3
A kind of processing method of the fluorine-containing ammonia-containing water of acid phosphorus acid type, the treating method comprises following steps:
(1) in home-made contrivance, 2L waste water (fluorine content 9g/L, ammonia-nitrogen content 5g/L, phosphoric acid quality concentration are taken It 50wt%) puts into tetrafluoro cucurbit, while magnesia and water being added in pretreatment tank for 1:2 by solid-liquid mass ratio, stirring It mixes 2h and obtains magnesia slurry 2L;
(2) 40 DEG C of jacket temperature are set, cucurbit is heated, makes fluorine in wastewater component in the form of hydrogen fluoride gas through tetrafluoro Connector, straight tube enter in reactor tank;
(3) it after the detector detection hydrogen fluoride concentration that reactor tank is equipped with reaches critical setting value 0.8ppm, is promoted Magnesia slurry is pumped into reactor tank by pump startup, and controlling its feed flow rate is 30L/h, utilizes the nozzle being arranged inside reactor tank It is set to come into full contact with absorption hydrogen fluoride gas, until gas concentration is then reacted lower than heating and slurry feed is stopped after critical value In-tank mixing material continues to stir and evenly mix 2h, and then blowing is filtered, washed, and obtains magnesium fluoride, purity after 5h is dried at 70 DEG C 98.7%.Gained magnesium fluoride is pure white superfine powder, is detected granularity and reaches 300 mesh, product exquisiteness can be used without obvious impurity In the reagents raw material such as ceramics, metal smelt;
(4) starting elevator pump is pumped into magnesia slurry, under stiring mixes well it with distillation tail water, uses in the process Mass concentration is that 50wt% ammonium hydroxide adjusts pH to 6, then continues to be stirred to react 3h, then be filtered, washed, dries 8h at 90 DEG C Ammonium magnesium phosphate, purity 94.8% are obtained afterwards.Gained ammonium magnesium phosphate is white particle, is analyzed through object phase, structural characterization, product composition group At single, no other objects are mutually mixed, and crystalline structure is good, and integral particle size distribution is uniform, can be used for fertilizer and water process is tried Agent.

Claims (9)

1. a kind of processing system of the fluorine-containing ammonia-containing water of acid phosphorus acid type, which is characterized in that the processing system includes cucurbit (1), reactor tank (3), elevator pump (4), pretreatment tank (5);
Cucurbit (1) bottom is furnished with electric heating cover (2), and bottleneck is furnished with motor (6) and tetrafluoro connector (7);
Equipped with detector (10), motor (12) and nozzle (13) at the top of the reactor tank (3);
It are furnished with motor (15) at the top of the pretreatment tank (5);
The cucurbit (1) is connected to by tetrafluoro connector (7) and tetrafluoro straight tube (8) with reactor tank (3);The tetrafluoro straight tube (8) It is fixed using fixed bracket (9);
The reactor tank (3) is connected to by elevator pump (4) with pretreatment tank (5).
2. processing system according to claim 1, which is characterized in that the cucurbit (1), reactor tank (3) and pre- place Managing tank (5) capacity is 5L;The reactor tank (3) is carbon steel Fluorine-lined material, and pretreatment tank (5) is stainless steel material, tank body material Matter thickness is 8mm.
3. processing system according to claim 1, which is characterized in that install polypropylene plastics at reactor tank (3) end socket Expect nozzle (13), and be equipped with detector (10), detection range is 0~100ppm.
4. processing system according to claim 1, which is characterized in that the cucurbit (1), reactor tank (3), pretreatment tank (5) three is equipped with blender, and material is consistent with tank body, and motor (6), (12), the revolving speed of (15) is adjustable, and 0~40 turn of range/ Minute.
5. processing system according to claim 1, which is characterized in that waste water is heated in the cucurbit (1) evaporates Hydrogen fluoride gas (11) enter in reactor tank (3) through tetrafluoro connector (7) and tetrafluoro straight tube (8), pass through detector (10) Response signal is issued, elevator pump (4) starting will pre-process the magnesia slurry (14) mixed in tank (5) after reaching setting critical value It is pumped into reactor tank, it is evenly dispersed through nozzle (13) and come into full contact with, stir and evenly mix with hydrogen fluoride gas (11), it is lower than critical value Elevator pump (4), which is closed, afterwards stops charging.
6. a kind of method of the processing fluorine-containing ammonia-containing water of acid phosphorus acid type of processing system described in claim 1, which is characterized in that institute The method of stating includes the following steps:
(1) it adds waste water into tetrafluoro cucurbit, the fixed tetrafluoro cucurbit is placed in above electric heating cover, is connect using tetrafluoro It is connected and is fixed with reactor tank by head, straight tube;
(2) magnesia is put into pretreatment tank, adds water and stirs mixing and forms slurries;
(3) electric heating cover is opened, waste water in cucurbit is heated, the volatilization of fluorine in wastewater hydrogen is entered in reactor tank by straight tube, benefit Detected with detector, after hydrogen fluoride gas concentration reaches critical setting value, promoted pump startup and will step (2) it is prepared Magnesia slurry be pumped into reactor tank, control its flow velocity, come into full contact with slurries simultaneously using the nozzle being arranged inside reactor tank Hydrogen fluoride gas is absorbed, until gas detection closes elevator pump after being lower than critical setting value;
(4) by finally formed mixed material in step (3) described reactor tank, continue to stir and evenly mix, blowing filtering, drying, i.e., Obtain magnesium fluoride;
(5) magnesia slurry prepared by step (2) is pumped into step (3) to distill in resulting mother liquor, is stirred and evenly mixed, and be added Ammonium hydroxide adjusts pH, and filtering, drying are to get ammonium magnesium phosphate.
7. according to the method described in claim 6, ammonia-nitrogen content is it is characterized in that, the fluorine in wastewater content is 8~9g/L 5~6g/L, 40~50wt% of phosphoric acid quality concentration;It is 1:1.5~2 that step (2) described magnesia, which mixes solid-liquid mass ratio with water, Stirring and evenly mixing the time is 1~2h.
8. according to the method described in claim 6, it is characterized in that, electric heating cover set temperature described in step (3) be 30~ 40℃;The critical setting value of hydrogen fluoride gas is 0.5~1ppm;Magnesia mixed liquor feed flow rate is 20~30L/h;Step (4) Described in mixed material stirs and evenly mixs the time in reactor tank is 1~2h, solid drying temperature is 60~70 DEG C, drying time 3 ~5h.
9. according to the method described in claim 6, it is characterized in that, the ammoniacal liquor mass concentration used described in step (5) is 30 ~40wt%, pH are adjusted to 5~6, are persistently stirred to react 2~3h of time, and solid drying temperature is 80~90 DEG C, and drying time is 6~8h.
CN201910489867.0A 2019-06-06 2019-06-06 A kind of processing method of the fluorine-containing ammonia-containing water of acid phosphorus acid type Pending CN110104864A (en)

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CN112811740A (en) * 2021-01-28 2021-05-18 关向辉 Method for removing fluorine and hardness from industrial wastewater
CN114229985A (en) * 2021-12-15 2022-03-25 湖南有色郴州氟化学有限公司 Novel method for removing ammonia nitrogen by catalytic oxidation of magnesium-based oxyfluoride
CN114229985B (en) * 2021-12-15 2023-09-19 湖南有色郴州氟化学有限公司 Method for removing ammonia nitrogen by catalytic oxidation of magnesium-based oxyfluoride

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Application publication date: 20190809