CN101376504A - Method for preparing potassium borofluoride - Google Patents

Method for preparing potassium borofluoride Download PDF

Info

Publication number
CN101376504A
CN101376504A CNA200710055075XA CN200710055075A CN101376504A CN 101376504 A CN101376504 A CN 101376504A CN A200710055075X A CNA200710055075X A CN A200710055075XA CN 200710055075 A CN200710055075 A CN 200710055075A CN 101376504 A CN101376504 A CN 101376504A
Authority
CN
China
Prior art keywords
potassium
ammonium fluoride
potassium fluoborate
concentration
fluoborate
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CNA200710055075XA
Other languages
Chinese (zh)
Inventor
皇甫根利
李世江
侯红军
杨华春
刘海霞
张良
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Duo Fluoride Chemicals Co Ltd
Original Assignee
Duo Fluoride Chemicals Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Duo Fluoride Chemicals Co Ltd filed Critical Duo Fluoride Chemicals Co Ltd
Priority to CNA200710055075XA priority Critical patent/CN101376504A/en
Publication of CN101376504A publication Critical patent/CN101376504A/en
Pending legal-status Critical Current

Links

Landscapes

  • Fertilizers (AREA)

Abstract

The invention relates to a method for preparing potassium fluoborate, which takes ammonium fluoride, boracic acid and potassium hydroxide as main material and concretely comprises the steps as follows: (1) a potassium hydroxide solution, the concentration of which is 35 to 50 percent, is added in a reaction tank, and then the boracic acid is added at room temperature; when the boracic acid is dissolved completely, the temperature reaches 80 to 110 DEG C, and the stirring is continued for 10 to 30 minutes to prepare a mixed solution; (2) an ammonium fluoride solution is injected into a concentration reaction tank, and the needed mixed solution is added, the concentration is conducted through heating after the material feeding is finished; the solid potassium fluoborate is separated out gradually during the concentration process, and a potassium fluoborate paste is obtained; and (3) the potassium fluoborate paste is dried to prepare finished products. The method takes the ammonium fluoride which is generated through the ammonolysis of fluosilicic acid as the raw material to prepare the potassium fluoborate, the development and the utilization relieve the environmental protection pressure of phosphate fertilizer production and the influences on the surrounding environment, and the cost is lower and the raw material is easy to get because the fluosilicic acid is a by-product in a phosphate fertilizer factory, thereby lowering the manufacture cost of the potassium fluoborate.

Description

A kind of method for preparing potassium fluoborate
Technical field
The present invention relates to a kind of method for preparing potassium fluoborate, relating in particular to a kind of is the method that main raw material prepares potassium fluoborate with Neutral ammonium fluoride, boric acid and potassium hydroxide.
Background technology
Potassium fluoborate is of many uses, is mainly used in the fusing assistant of heat weldable brazing, and the raw material of boron-containing alloy is produced in the magnalium casting, in addition, is used as stopping composition in the heavy emery wheel of making the abrasive material tackiness agent with resin.Use the related industries of potassium fluoborate, scale is stable, and is stable to the demand of potassium fluoborate, so the Expanding Market of potassium fluoborate.Conventional production methods adopts hydrofluoric acid Repone K method more, or uses the market raw material sources are well sold and in short supply and valency is high salt of wormwood or potassium hydroxide borate method.Hydrofluoric acid is mainly made by fluorite and sulfuric acid reaction, so strategic resource fluorite of traditional technology consume valuable, country strengthens the control dynamics to fluorite now, the price of fluorite is more and more higher, the price of corresponding hydrofluoric acid also will inevitably raise, thereby influences the cost of potassium fluoborate, therefore, seeking new fluorine source instead of hydrogen fluoric acid is to reduce the potassium fluoborate cost, promotes the important channel of potassium fluoborate competitive power.
Summary of the invention
The object of the invention is to provide a kind of method for preparing potassium fluoborate, to improve the quality of products, reduces production costs.
To achieve these goals, having technical program of the present invention lies in adopting a kind of method for preparing potassium fluoborate, is main raw material with Neutral ammonium fluoride, boric acid and potassium hydroxide, specifically may further comprise the steps:
(1) adding concentration in reactive tank is 35%-50% potassium hydroxide solution, adds boric acid then at normal temperatures, and when treating that boric acid has dissolved fully, temperature reaches 80 ℃-110 ℃, continues stirring and can make mixing solutions in 10-30 minutes;
(2) ammonium fluoride solution is squeezed into the concentration response groove, and added required mixing solutions, behind reinforced the finishing, reactive tank begins to heat up and concentrates, and has the solid potassium fluoborate to separate out in the concentration process gradually, gets potassium fluoroborate ointment;
(3), can make finished product with the potassium fluoroborate ointment drying.
It is standby that the ammonia that reaction is emitted in the described step (2) absorbs into ammoniacal liquor through refrigeration cycle.
The concentration of described ammonium fluoride solution is 10%-45%.
Described Neutral ammonium fluoride can be made by the by-product fluosilicic acid ammonolysis reaction of phophatic fertilizer production process.
Reaction formula of the present invention is:
KOH+H 3BO 3+4NH 4F=KBF 4+4H 2O+4NH 3
Neutral ammonium fluoride among the present invention can add ammoniacal liquor by the byproduct silicofluoric acid of phosphate fertilizer industry carry out ammonia and separate and obtain, and its reaction formula is as follows:
H 2SiF 6+6NH 3·H 2O=6NH 4F+SiO 2↓+4H 2O
The present invention is to be that raw material replaces hydrogen fluoride with the Neutral ammonium fluoride; wherein; Neutral ammonium fluoride is made through ammonolysis reaction by the byproduct silicofluoric acid adding ammoniacal liquor of phophatic fertilizer production process; silicofluoric acid is the by-product harmful waste of phophatic fertilizer production process; purposes seldom; it has caused environment protection and has had a strong impact on; and Neutral ammonium fluoride that the present invention utilizes silicofluoric acid ammonia to separate just to be generated prepares potassium fluoborate for raw material; the development and use of silicofluoric acid have been alleviated the environmental protection pressure of production of phosphate fertilizer and to the influence of surrounding environment; and because silicofluoric acid is the by product of phosphate fertilizer plant; lower and the raw material of cost is easy to get, thereby has reduced the production cost of potassium fluoborate.The present invention has good social benefit, economic benefit and environmental benefit, is easy to apply.
The potassium fluoborate product quality analysis result who utilizes method of the present invention to produce
Figure A200710055075D00051
Embodiment
Embodiment 1
Present embodiment prepares the method for potassium fluoborate, is main raw material with Neutral ammonium fluoride, boric acid, potassium hydroxide, specifically may further comprise the steps:
(1) adding concentration in reactive tank is 35% potassium hydroxide solution, adds boric acid then at normal temperatures, and when treating that boric acid has dissolved fully, temperature reaches 80 ℃-110 ℃, continues stirring and can make mixing solutions in 15 minutes;
(2) be that 25% ammonium fluoride solution is squeezed into the concentration response groove with concentration, and add required mixing solutions, behind reinforced the finishing, reactive tank begins to heat up and concentrates, and has the solid potassium fluoborate to separate out in the concentration process gradually, potassium fluoroborate ointment;
(3), can make finished product with the potassium fluoroborate ointment drying.
It is standby that the ammonia that reaction is emitted in the described step (2) absorbs into ammoniacal liquor through refrigeration cycle.
Neutral ammonium fluoride in the present embodiment can be made by the by-product fluosilicic acid ammonolysis reaction of phophatic fertilizer production process.
Embodiment 2
Present embodiment prepares the method for potassium fluoborate, is main raw material with Neutral ammonium fluoride, boric acid and potassium hydroxide, specifically may further comprise the steps:
(1) adding concentration in reactive tank is 40% potassium hydroxide solution, adds boric acid then at normal temperatures, and when treating that boric acid has dissolved fully, temperature reaches 80 ℃-110 ℃, continues stirring 20 minutes, makes mixing solutions;
(2) 35% ammonium fluoride solution is squeezed into the concentration response groove, and add required mixing solutions, behind reinforced the finishing, reactive tank begins to heat up and concentrates, and has the solid potassium fluoborate to separate out in the concentration process gradually, gets potassium fluoroborate ointment;
(3), can make finished product with the potassium fluoroborate ointment drying.
It is standby that the ammonia that reaction is emitted in the described step (2) absorbs into ammoniacal liquor through refrigeration cycle.
Neutral ammonium fluoride in the present embodiment can be made by the by-product fluosilicic acid ammonolysis reaction of phophatic fertilizer production process.
Embodiment 3
The method that present embodiment prepares potassium fluoborate is to be main raw material with Neutral ammonium fluoride, boric acid and potassium hydroxide, specifically may further comprise the steps:
(1) adding concentration in reactive tank is 45% potassium hydroxide solution, adds boric acid then at normal temperatures, and when treating that boric acid has dissolved fully, temperature reaches 80 ℃-110 ℃, continues stirring and can make mixing solutions in 25 minutes;
(2) 45% ammonium fluoride solution is squeezed into the concentration response groove, and add required mixing solutions, behind reinforced the finishing, reactive tank begins to heat up and concentrates, and has the solid potassium fluoborate to separate out in the concentration process gradually, gets potassium fluoroborate ointment;
(3), can make finished product with the potassium fluoroborate ointment drying.
It is standby that the ammonia that reaction is emitted in the described step (2) absorbs into ammoniacal liquor through refrigeration cycle.
Neutral ammonium fluoride in the present embodiment can be made by the by-product fluosilicic acid ammonolysis reaction of phophatic fertilizer production process.
It should be noted last that: above embodiment is the unrestricted technical scheme of the present invention in order to explanation only, although the present invention is had been described in detail with reference to the foregoing description, those of ordinary skill in the art is to be understood that: still can make amendment or be equal to replacement the present invention, and not breaking away from any modification or partial replacement of the spirit and scope of the present invention, it all should be encompassed in the middle of the claim scope of the present invention.

Claims (4)

1, a kind of method for preparing potassium fluoborate, it is characterized in that: with Neutral ammonium fluoride, boric acid and potassium hydroxide is main raw material, specifically may further comprise the steps:
(1) adding concentration in reactive tank is 35%-50% potassium hydroxide solution, adds boric acid then at normal temperatures, and when treating that boric acid has dissolved fully, temperature reaches 80 ℃-110 ℃, continues stirring 10-30 minutes, makes mixing solutions;
(2) ammonium fluoride solution is squeezed into the concentration response groove, and added required mixing solutions, behind reinforced the finishing, heating up concentrates, and has the solid potassium fluoborate to separate out in the concentration process gradually, gets potassium fluoroborate ointment;
(3), can make finished product with the potassium fluoroborate ointment drying.
2, the method for preparing potassium fluoborate according to claim 1 is characterized in that: it is standby that the ammonia that reaction is emitted in the described step (2) absorbs into ammoniacal liquor through refrigeration cycle.
3, the method for preparing potassium fluoborate according to claim 1 is characterized in that: the concentration of described ammonium fluoride solution is 10%-45%.
4, the method for preparing potassium fluoborate according to claim 1 is characterized in that: described Neutral ammonium fluoride makes after can being separated by the by-product fluosilicic acid ammonia in the production of phosphate fertilizer.
CNA200710055075XA 2007-08-31 2007-08-31 Method for preparing potassium borofluoride Pending CN101376504A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CNA200710055075XA CN101376504A (en) 2007-08-31 2007-08-31 Method for preparing potassium borofluoride

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CNA200710055075XA CN101376504A (en) 2007-08-31 2007-08-31 Method for preparing potassium borofluoride

Publications (1)

Publication Number Publication Date
CN101376504A true CN101376504A (en) 2009-03-04

Family

ID=40420249

Family Applications (1)

Application Number Title Priority Date Filing Date
CNA200710055075XA Pending CN101376504A (en) 2007-08-31 2007-08-31 Method for preparing potassium borofluoride

Country Status (1)

Country Link
CN (1) CN101376504A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101914809A (en) * 2010-08-11 2010-12-15 中国科学院新疆理化技术研究所 Nonlinear optical crystal of potassium borate chloride compound and preparation method as well as application thereof
CN107098356A (en) * 2016-02-23 2017-08-29 达州励志环保科技有限公司 A kind of preparation method of potassium fluoborate

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101914809A (en) * 2010-08-11 2010-12-15 中国科学院新疆理化技术研究所 Nonlinear optical crystal of potassium borate chloride compound and preparation method as well as application thereof
CN101914809B (en) * 2010-08-11 2014-03-12 中国科学院新疆理化技术研究所 Nonlinear optical crystal of potassium borate chloride compound and preparation method as well as application thereof
CN107098356A (en) * 2016-02-23 2017-08-29 达州励志环保科技有限公司 A kind of preparation method of potassium fluoborate

Similar Documents

Publication Publication Date Title
CN100577567C (en) Method for linked production of ammonium fluoride and white carbon black
CN102951611B (en) The method that a kind of fluorine-containing waste liquid of phosphatic fertilizer company or hexafluosilicic acid prepare anhydrous hydrogen fluoride
CN103332700B (en) Method for preparing potassium borofluoride through fluorine-containing wastewater
CN106865500B (en) A kind of cycle production process preparing hydrogen fluoride with fluosilicic acid
CN101289195B (en) Process for preparing potassium borofluoride and co-production of white carbon black and sodium fluosilicate
CN103601217B (en) Sodium fluoride production process and sodium fluoride mother liquor recycling process
CN101891504A (en) Method for producing granular monoammonium phosphate with raffinate
CN103803561A (en) Method for recycling fluorine-containing waste gas in phosphorus chemical industry production
CN100577568C (en) Method for linked production of ammonium acid fluoride and white carbon black
CN102887532B (en) Process for preparing potassium fluoride and co-producing white carbon black from fluosilicic acid
CN101898769B (en) Method for producing high-purity ammonium bifluoride
CN104326475A (en) Method for preparing potassium fluoride by employing fluosilicic acid with co-production of white carbon black
CN101376509B (en) Method for preparing potassium fluoride
CN101376514A (en) Preparation of magnesium fluoride
CN102887528B (en) Production technology of ammonium bifluoride
CN101376508A (en) Method for producing lithium fluoride
CN101570337B (en) Production method of battery- grade lithium fluoride
CN101376504A (en) Method for preparing potassium borofluoride
CN101134590A (en) Method for producing aluminun fluoride with combined production of white carbon black and ammonia sulfate
CN101376513B (en) Preparation of magnesium fluoride
CN103539127B (en) A kind of decomposition technique of potassium felspar sand
CN108483965A (en) A kind of technique preparing accelerator using industrial waste phosphoric acid
CN102874855B (en) Lithium-containing sodium cryolite and preparation method thereof
CN101376519A (en) Method for preparing barium fluoride
CN107285292A (en) The method that reaction of high order prepares battery-grade iron phosphate

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C12 Rejection of a patent application after its publication
RJ01 Rejection of invention patent application after publication

Open date: 20090304