CN109368652A - A kind of method that tail gas absorption waste liquid prepares potassium fluoborate - Google Patents

A kind of method that tail gas absorption waste liquid prepares potassium fluoborate Download PDF

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Publication number
CN109368652A
CN109368652A CN201811412740.0A CN201811412740A CN109368652A CN 109368652 A CN109368652 A CN 109368652A CN 201811412740 A CN201811412740 A CN 201811412740A CN 109368652 A CN109368652 A CN 109368652A
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CN
China
Prior art keywords
water
waste liquid
tail gas
added
potassium fluoborate
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Pending
Application number
CN201811412740.0A
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Chinese (zh)
Inventor
姚强
盛晓东
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JIANGSU XINTAI MATERIAL TECHNOLOGY Co Ltd
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JIANGSU XINTAI MATERIAL TECHNOLOGY Co Ltd
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Application filed by JIANGSU XINTAI MATERIAL TECHNOLOGY Co Ltd filed Critical JIANGSU XINTAI MATERIAL TECHNOLOGY Co Ltd
Priority to CN201811412740.0A priority Critical patent/CN109368652A/en
Publication of CN109368652A publication Critical patent/CN109368652A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B35/00Boron; Compounds thereof
    • C01B35/06Boron halogen compounds
    • C01B35/063Tetrafluoboric acid; Salts thereof
    • C01B35/066Alkali metal tetrafluoborates
    • 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
    • B01D53/14Separation 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 by absorption
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F11/00Compounds of calcium, strontium, or barium
    • C01F11/20Halides
    • C01F11/24Chlorides

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Analytical Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Treating Waste Gases (AREA)
  • Gas Separation By Absorption (AREA)

Abstract

The invention discloses a kind of methods that tail gas absorption waste liquid prepares potassium fluoborate, comprising the following steps: 1) tap water is added in tail gas water scrubber, potassium hydroxide solution and water is added in caustic wash tower;2) it is passed through hydrogen fluoride and chlorine hydride mixed gas body, total acidity changes water at 35 ~ 40% in water scrubber, and solution pH value changes absorbing liquid for 7 ~ 8 or so in caustic wash tower;3) waste liquid in caustic wash tower is squeezed into potassium fluoborate dissolving tank, is heated using steam;4) borax and potassium chloride stirring and dissolving is added;5) lysate is squeezed into reaction kettle, waste liquid in water scrubber is added until reaction end;6) reaction kettle is put into cooling reactor and is cooled down;7) reaction solution is put into suction filtration tank;8) filter cake is rinsed after the completion of filtering;9) it is packed after filter cake is dried.Alkali cleaning can be absorbed devil liquor recovery using potassium fluoborate is prepared, reduce production cost by a kind of method for preparing potassium fluoborate using tail gas absorption waste liquid of the present invention.

Description

A kind of method that tail gas absorption waste liquid prepares potassium fluoborate
Technical field
The present invention relates to the sides that the synthesis technology of potassium fluoborate more particularly to a kind of tail gas absorption waste liquid prepare potassium fluoborate Method.
Background technique
In current lithium hexafluoro phosphate production process, a large amount of HF, HCl gases can be generated, are needed using the absorption of two-stage water, one It can be just discharged into atmosphere after grade Alkali absorption processing, during Alkali absorption, original uses 2 solution of Ca (OH) as absorbing liquid, has absorbed Cheng Houhui generates a large amount of CaF2, CaCl2 mixed solution waste liquids, and waste liquid can squeeze into plant area's sewage treatment, can just arrange after treatment Enter garden sewage conduct, wastes a large amount of HF raw material in the process, and generate a large amount of waste materials, substantially increase sewage treatment post Workload, be added significantly to production cost.
Summary of the invention
To solve the above problems, the present invention provides a kind of method that tail gas absorption waste liquid prepares potassium fluoborate, it can be by alkali It washes and absorbs devil liquor recovery using potassium fluoborate is prepared, mitigate sewage treatment works load, reduce production cost.
To achieve the goals above, the technical scheme is to design a kind of tail gas absorption waste liquids to prepare potassium fluoborate Method, which comprises the following steps:
Step 1: tap water is added in tail gas water scrubber, potassium hydroxide solution and water are added in caustic wash tower;
Step 2: it is passed through the hydrogen fluoride of output and chlorine hydride mixed gas body in lithium hexafluoro phosphate production process, total acid in water scrubber Degree changes water at 35 ~ 40%, and solution pH value changes absorbing liquid for 7 ~ 8 or so in caustic wash tower;
Step 3: waste liquid in caustic wash tower is squeezed into potassium fluoborate dissolving tank, using being steam heated to 60 ~ 70 DEG C;
Step 4: borax and potassium chloride stirring and dissolving is added, and solution temperature is kept to stablize at 60 ~ 70 DEG C;
Step 5: lysate is squeezed into reaction kettle, waste liquid in water scrubber is added until reaction end, it need to will be in reaction kettle when reaction Temperature controls between 70 ~ 80 DEG C;
25 ~ 30 DEG C are cooled to Step 6: reaction kettle is put into cooling reactor;
Step 7: reaction solution is put into suction filtration tank, extraction liquid is fluorine-containing hydrochloric acid, as Calcium Chloride Production raw material;
Step 8: being rinsed using tap water to filter cake after the completion of filtering, flushing liquor is low concentration fluorine-containing hydrochloric acid, squeezes into hexafluoro It is used in lithium phosphate water scrubber as absorbing liquid;
Step 9: filter cake is packed after being dried.
Further, the ratio of potassium hydroxide solution and water is preferably in a proportion of 1 between 1:30 ~ 1:100 in step 1: 50。
The advantages and beneficial effects of the present invention are: a kind of side for preparing potassium fluoborate using tail gas absorption waste liquid of the present invention Alkali cleaning can be absorbed devil liquor recovery using potassium fluoborate is prepared, mitigate sewage treatment works load, reduce production cost by method.
Specific embodiment
With reference to embodiment, the specific embodiment of the present invention is further described.Following embodiment is only used for more Add and clearly demonstrate technical solution of the present invention, and not intended to limit the protection scope of the present invention.
Embodiment:
A kind of method that tail gas absorption waste liquid prepares potassium fluoborate, comprising the following steps:
Step 1: tap water is added in tail gas water scrubber, potassium hydroxide solution and water, potassium hydroxide solution are added in caustic wash tower Ratio with water is 1:50;
Step 2: it is passed through the hydrogen fluoride of output and chlorine hydride mixed gas body in lithium hexafluoro phosphate production process, total acid in water scrubber Degree changes water at 35 ~ 40%, and solution pH value changes absorbing liquid for 7 ~ 8 or so in caustic wash tower;
Step 3: waste liquid in caustic wash tower is squeezed into potassium fluoborate dissolving tank, using being steam heated to 60 ~ 70 DEG C;
Step 4: borax and potassium chloride stirring and dissolving is added, and solution temperature is kept to stablize at 60 ~ 70 DEG C;
Step 5: lysate is squeezed into reaction kettle, waste liquid in water scrubber is added until reaction end, it need to will be in reaction kettle when reaction Temperature controls between 70 ~ 80 DEG C;
25 ~ 30 DEG C are cooled to Step 6: reaction kettle is put into cooling reactor;
Step 7: reaction solution is put into suction filtration tank, extraction liquid is fluorine-containing hydrochloric acid, as Calcium Chloride Production raw material;
Step 8: being rinsed using tap water to filter cake after the completion of filtering, flushing liquor is low concentration fluorine-containing hydrochloric acid, squeezes into hexafluoro It is used in lithium phosphate water scrubber as absorbing liquid;
Step 9: filter cake is packed after being dried.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art For member, without departing from the technical principles of the invention, several improvements and modifications can also be made, these improvements and modifications Also it should be regarded as protection scope of the present invention.

Claims (3)

1. a kind of method that tail gas absorption waste liquid prepares potassium fluoborate, which comprises the following steps:
Step 1: tap water is added in tail gas water scrubber, potassium hydroxide solution and water are added in caustic wash tower;
Step 2: it is passed through the hydrogen fluoride of output and chlorine hydride mixed gas body in lithium hexafluoro phosphate production process, total acid in water scrubber Degree changes water at 35 ~ 40%, and solution pH value changes absorbing liquid for 7 ~ 8 or so in caustic wash tower;
Step 3: waste liquid in caustic wash tower is squeezed into potassium fluoborate dissolving tank, using being steam heated to 60 ~ 70 DEG C;
Step 4: borax and potassium chloride stirring and dissolving is added, and solution temperature is kept to stablize at 60 ~ 70 DEG C;
Step 5: lysate is squeezed into reaction kettle, waste liquid in water scrubber is added until reaction end, it need to will be in reaction kettle when reaction Temperature controls between 70 ~ 80 DEG C;
25 ~ 30 DEG C are cooled to Step 6: reaction kettle is put into cooling reactor;
Step 7: reaction solution is put into suction filtration tank, extraction liquid is fluorine-containing hydrochloric acid, as Calcium Chloride Production raw material;
Step 8: being rinsed using tap water to filter cake after the completion of filtering, flushing liquor is low concentration fluorine-containing hydrochloric acid, squeezes into hexafluoro It is used in lithium phosphate water scrubber as absorbing liquid;
Step 9: filter cake is packed after being dried.
2. the method that a kind of tail gas absorption waste liquid according to claim 1 prepares potassium fluoborate, which is characterized in that step 1 The ratio of middle potassium hydroxide solution and water is between 1:30 ~ 1:100.
3. the method that a kind of tail gas absorption waste liquid according to claim 2 prepares potassium fluoborate, which is characterized in that step 1 The ratio of middle potassium hydroxide solution and water is 1:50.
CN201811412740.0A 2018-11-26 2018-11-26 A kind of method that tail gas absorption waste liquid prepares potassium fluoborate Pending CN109368652A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201811412740.0A CN109368652A (en) 2018-11-26 2018-11-26 A kind of method that tail gas absorption waste liquid prepares potassium fluoborate

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Application Number Priority Date Filing Date Title
CN201811412740.0A CN109368652A (en) 2018-11-26 2018-11-26 A kind of method that tail gas absorption waste liquid prepares potassium fluoborate

Publications (1)

Publication Number Publication Date
CN109368652A true CN109368652A (en) 2019-02-22

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111498861A (en) * 2020-04-23 2020-08-07 无锡中天固废处置有限公司 Polarizing plate waste liquid treatment method

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4126488A (en) * 1976-07-23 1978-11-21 Deutsche Gold- Und Silber-Scheideanstalt Vormals Roessler Boriding agent for boriding mass produced parts of ferrous and non-ferrous metals
CN103332700A (en) * 2013-07-23 2013-10-02 森田化工(张家港)有限公司 Method for preparing potassium borofluoride through fluorine-containing wastewater
CN104891517A (en) * 2015-06-09 2015-09-09 天津金牛电源材料有限责任公司 Method for producing potassium borofluoride by utilizing lithium hexafluorophosphate recovery acid mixture
CN106693599A (en) * 2017-01-19 2017-05-24 森田新能源材料(张家港)有限公司 Device and method for treating waste gas in lithium hexafluorophate preparation process
CN108147436A (en) * 2018-02-26 2018-06-12 江苏新泰材料科技有限公司 Combined coefficient is improved in lithium hexafluoro phosphate production process reduces the synthetic method of unit consumption

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4126488A (en) * 1976-07-23 1978-11-21 Deutsche Gold- Und Silber-Scheideanstalt Vormals Roessler Boriding agent for boriding mass produced parts of ferrous and non-ferrous metals
CN103332700A (en) * 2013-07-23 2013-10-02 森田化工(张家港)有限公司 Method for preparing potassium borofluoride through fluorine-containing wastewater
CN104891517A (en) * 2015-06-09 2015-09-09 天津金牛电源材料有限责任公司 Method for producing potassium borofluoride by utilizing lithium hexafluorophosphate recovery acid mixture
CN106693599A (en) * 2017-01-19 2017-05-24 森田新能源材料(张家港)有限公司 Device and method for treating waste gas in lithium hexafluorophate preparation process
CN108147436A (en) * 2018-02-26 2018-06-12 江苏新泰材料科技有限公司 Combined coefficient is improved in lithium hexafluoro phosphate production process reduces the synthetic method of unit consumption

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111498861A (en) * 2020-04-23 2020-08-07 无锡中天固废处置有限公司 Polarizing plate waste liquid treatment method
CN111498861B (en) * 2020-04-23 2022-07-26 无锡中天固废处置有限公司 Polarizing plate waste liquid treatment method

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Application publication date: 20190222