CN105803480A - Preparation method of boron trifluoride gas - Google Patents
Preparation method of boron trifluoride gas Download PDFInfo
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- CN105803480A CN105803480A CN201610301967.2A CN201610301967A CN105803480A CN 105803480 A CN105803480 A CN 105803480A CN 201610301967 A CN201610301967 A CN 201610301967A CN 105803480 A CN105803480 A CN 105803480A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/24—Halogens or compounds thereof
- C25B1/245—Fluorine; Compounds thereof
Abstract
The invention relates to a preparation method of boron trifluoride gas. The preparation method includes the following steps that firstly, an inert electrode serves as an anode, an inert electrode serves as a cathode, a mixed aqueous solution of sodium fluoroborate and boric acid serves as anode liquid, an acid solution or an alkali solution or a salt solution serves as cathode liquid, temperature is controlled to be 60 DEG C to 90 DEG C in a double-chamber electrolytic cell with a cation membrane as a partition membrane, and electrolysis is performed in a constant-current electrolysis or constant-voltage electrolysis manner; and secondly, in the electrolysis process, the flow speed of gas is controlled to be stable, generated gas is collected through a purification device and a collection device, and then the purified boron trifluoride gas is obtained. Compared with the prior art, the boron trifluoride gas obtained through the method is purified and free of impurities, the preparation method is reasonable, the technology is simple, cost is low, conditions are mild, the preparation method is an ideal boron trifluoride gas preparation technology, and the technical problems that in the process of preparing the boron trifluoride gas in the prior art, the reaction temperature is very high, conditions are strict, the reaction process is complicated, and cost is high are solved.
Description
[technical field]
The present invention relates to chemical products preparing technical field, the preparation of a kind of boron triflouride gas
Method.
[background technology]
Boron trifluoride is fluorine boride most important, most basic, and boron trifluoride is of many uses, especially as
Catalyst etc., for a long time, the catalytic performance of boron trifluoride is constantly subjected to the attention of people, alkylation,
The reaction such as condensation, polymerization is all very effective catalyst.At other such as acylated, sulfonation, halogenation
Middle boron trifluoride may also function as good catalytic action.Boron trifluoride and complex thereof can be catalyzed splitting of oil
Solve reaction, such as, under the high pressure of 300-400 DEG C, the boron trifluoride of 5%-10% or its complex can be by weights
Oil distillate cracking becomes insaturated gasoline.Based on boron trifluoride, divided catalyst can promote taking off on phenyl ring
Alkyl and dismutation reaction.Boron trifluoride and HF exist at a small amount of water, 300-350 DEG C and reagent can be made to keep
Under the pressure of liquid, it is possible to make alkylbenzene take off alkyl and form benzene or an alkylbenzene.Boron trifluoride and HF can also
Being that ethylbenzene disproportionation becomes NSC 62102 and benzene, diethylbenzene is disproportionated into sym-trimethylbenzene. and benzene.It is the most anti-in catalysis
Answer aspect to have so and be widely applied field, be owing to boron electron structure has the strong tendency of generation complex,
Catalysis active structure is produced in acidic catalyst effect.
Conventional boron trifluoride preparation method has borofluoride method, fluorite boric anhydride method, sodium fluoride boric anhydride method, fluorine
Boric acid heavy nitrogen, fluorite boric anhydride sulfuric acid process, fluorite boric acid sulfuric acid process, borofluoride boric anhydride sulfuric acid process, fluorination
Boron Antimony fluoride method and barium fluoborate heat resolve method etc..But, in the preparation method of these routines, as
In borofluoride method, Potassium borofluoride decomposition temperature needs to reach 600-700 DEG C, and fluoboric acid calcium decomposition temperature is wanted
300-500 DEG C, fluorite boric anhydride method is that the mixture of calcium fluoride Yu boric anhydride is heated to white heat (temperature 900-1200
DEG C), sodium fluoride boric anhydride method needs sodium fluoride and boric anhydride are heated to high temperature fused state.These conventional methods
Or required condition is harsh, or react temperature required high, or process is complicated.
[summary of the invention]
Present invention aim to solve above-mentioned deficiency and the preparation side of a kind of boron triflouride gas is provided
Method, solve of the prior art prepare boron triflouride gas during reaction temperature the highest, condition is harsh,
Course of reaction is complicated, high in cost of production technical problem, and the boron triflouride gas prepared is pure without dephasign.
Design the preparation method of a kind of boron triflouride gas for achieving the above object, comprise the following steps:
1) with inert electrode as anode, with inert electrode as negative electrode, mixed with Sodium fluoroborate and boric acid
Heshui solution is anolyte, with acid solution, aqueous slkali or saline solution as catholyte, at sun
Ionic membrane is in the two-compartment cell of barrier film, controls temperature and is 60-90 DEG C, uses Constant Electric Current
Solve or the mode of constant-potential electrolysis is electrolysed；
2) in electrolytic process, controlling gas flow rate stable, the gas of generation passes through purifier respectively
It is collected with collection device, obtains pure boron triflouride gas.
Further, step 1) in, described acid solution be concentration be 0.1-1mol/L aqueous hydrochloric acid solution or
Concentration is the aqueous sulfuric acid of 0.1-1mol/L.
Further, step 1) in, described aqueous slkali be concentration be that the sodium hydroxide of 0.1-1mol/L is water-soluble
Liquid or concentration are the potassium hydroxide aqueous solution of 0.1-1mol/L.
Further, step 1) in, described saline solution be concentration be the sodium-chloride water solution of 0.1-1mol/L
Or concentration is the aqueous sodium carbonate of 0.1-1mol/L.
Further, step 1) in, described cationic membrane is perfluorinated sulfonic acid cation exchange membrane.
Further, step 1) in, the electric current of constant-current electrolysis is 0.08-0.8A, and electric current density is
1-100mA/cm2, voltage range 10-300V of constant-potential electrolysis.
Further, step 1) in, described inert electrode is glass-carbon electrode, graphite electrode, Ti electrode or platinum
Electrode.
Further, step 1) in, the concentration of described Sodium fluoroborate is 0.1-5mol/L, described boric acid
Concentration is 0.1-2mol/L.
The present invention compared with the existing technology, has the advantage that
(1) cationic membrane owing to using in preparation process has certain selective penetrated property, particularly
Nafion series perfluorinated sulfonic acid cation exchange membrane can allow the Na in anode chamber+Ion permeable ionic membrane enters
Cathode chamber, so that Sodium fluoroborate is converted into fluoboric acid, fluoboric acid changes into trifluoro under conditions of being heated
Change boron, then pass through purifier and the gas collector of the concentrated sulphuric acid equipped with saturated diboron trioxide,
Collecting pure boron triflouride gas, its reaction condition is gentle, and reaction temperature is low, the boron trifluoride obtained
Gas is pure, without dephasign；
(2) be the mixed solution of Sodium fluoroborate and boric acid due to anolyte, by-product HF also can further with
Boric acid in anolyte reacts, and generates boron trifluoride, and reaction equation is: H3BO3+3HF→
BF3·H2O→BF3+3H2O, therefore, this preparation method have the boron triflouride gas purity of final gained high,
Feature without dephasign；
(3) the catholyte scope used by the present invention is wide, and acid solution, alkali liquor and saline solution are the most permissible, and electrolytic process
Either constant-current electrolysis or the mode of constant-potential electrolysis, can obtain pure uniform boron triflouride gas；
(4) anolyte of the present invention uses Sodium fluoroborate and the mixed solution of boric acid, and by-product can continue and boron
Acid reacts, so the conversion ratio of boron triflouride gas is higher, and anode slot residual impurity after the reaction
Seldom, it is easy to clear up and safeguard；
(5) due to the fact that and can prepare boron triflouride gas, and follow-up place in the short time by a step
Reason is simple, and therefore its preparation process technique is simple, easily operates, invests little, and synthetic quantity is big, can directly use
In small-sized boron trifluoride generator or industrialized production；
(6) present invention solve of the prior art prepare boron triflouride gas during reaction temperature very
Height, condition is harsh, and course of reaction is complicated, high in cost of production technical problem.
[detailed description of the invention]
The invention provides the preparation method of a kind of boron triflouride gas, comprise the following steps: 1) with dual chamber sun
Ion-exchange membrane electrolyzer is generator, with inert electrode as anode, with inert electrode as negative electrode, with Sodium fluoroborate
Be anolyte with the mixed aqueous solution of boric acid, with acid solution, aqueous slkali or saline solution as catholyte, sun from
Sub-film is in the two-compartment cell of barrier film, controls temperature and is 60-90 DEG C, uses constant-current electrolysis or constant-potential electrolysis
Mode is electrolysed；2) in electrolytic process, controlling gas flow rate stable, the gas of generation is respectively by purifying
Device and collection device are collected, and obtain pure boron triflouride gas.This preparation method is used to obtain
The pure free from admixture of boron triflouride gas, preparation method is reasonable, and technique is simple, with low cost, mild condition,
It it is a kind of preferably boron trifluoride technology of preparing.
Wherein, acid solution is that concentration is the aqueous hydrochloric acid solution of 0.1-1mol/L or concentration is 0.1-1mol/L's
Aqueous sulfuric acid；Aqueous slkali is that concentration is the sodium hydrate aqueous solution of 0.1-1mol/L or concentration is
The potassium hydroxide aqueous solution of 0.1-1mol/L；Saline solution be concentration be 0.1-1mol/L sodium-chloride water solution or
Concentration is the aqueous sodium carbonate of 0.1-1mol/L；Cationic membrane is perfluorinated sulfonic acid cation exchange membrane；Constant current
The electric current of electrolysis is 0.08-0.8A, and electric current density is 1-100mA/cm2, the voltage range of constant-potential electrolysis
10-300V；Anode use inert electrode, described inert electrode be glass-carbon electrode, graphite electrode, Ti electrode or
Platinum electrode；Negative electrode use inert electrode, described inert electrode be glass-carbon electrode, graphite electrode, Ti electrode or
Platinum electrode；The concentration of Sodium fluoroborate is 0.1-5mol/L, and the concentration of described boric acid is 0.1-2mol/L.
The present invention is made further explained below below in conjunction with specific embodiment:
Embodiment 1
The preparation method of a kind of boron triflouride gas, specifically includes following steps:
(1) with inert electrode as electrode, with the mixed aqueous solution of 90ml Sodium fluoroborate and boric acid as anolyte,
With acid solution as catholyte, in the two-compartment cell that cationic membrane is barrier film, use the mode of constant-current electrolysis,
Controlling temperature range is the 60-90 DEG C of aqueous solution carrying out being electrolysed Sodium fluoroborate；Described inert electrode is titanium net；Institute
The concentration stating Sodium fluoroborate aqueous solution is 0.1mol/L；The concentration of described boric acid is 0.1mol/L；Described acid is molten
Liquid be concentration be the aqueous hydrochloric acid solution of 0.1mol/L；Described cationic membrane is perfluorinated sulfonic acid cation exchange membrane；
The electric current of described constant-current electrolysis is 0.6A, and electric current density is 31.5mA/cm2；
(2), after control gas flow rate is stable, boron triflouride gas is collected with gas collecting bottle.
Embodiment 2
The preparation method of a kind of boron triflouride gas, specifically includes following steps:
(1) with inert electrode as electrode, with the mixed aqueous solution of 90ml Sodium fluoroborate and boric acid as anolyte,
With aqueous slkali as catholyte, in the two-compartment cell that cationic membrane is barrier film, use the mode of constant-potential electrolysis,
Controlling temperature range is the 60-90 DEG C of aqueous solution carrying out being electrolysed Sodium fluoroborate；Described inert electrode is platinum guaze；Institute
The concentration stating Sodium fluoroborate aqueous solution is 5mol/L；The concentration of described boric acid is 2mol/L；Described aqueous slkali is
The sodium hydrate aqueous solution of 0.1mol/L；Described cationic membrane is perfluorinated sulfonic acid cation exchange membrane；Described perseverance
The voltage of piezoelectricity solution is 10V；
(2), after control gas flow rate is stable, boron triflouride gas is collected with gas collecting bottle.
Embodiment 3
The preparation method of a kind of boron triflouride gas, specifically includes following steps:
(1) with inert electrode as electrode, with the mixed aqueous solution of 90ml Sodium fluoroborate and boric acid as anolyte,
With saline solution as catholyte, in the two-compartment cell that cationic membrane is barrier film, use the mode of constant-current electrolysis,
Controlling temperature range is the 60-90 DEG C of aqueous solution carrying out being electrolysed Sodium fluoroborate；Described inert electrode is glass carbon or stone
Ink；The concentration of described Sodium fluoroborate aqueous solution is 2mol/L；The concentration of described boric acid is 1mol/L；Described acid
Solution be concentration be the aqueous hydrochloric acid solution of 0.1mol/L；Described cationic membrane is perfluorinated sulfonic acid cation exchange membrane；
The electric current of described constant-current electrolysis is 0.8A, and electric current density is 100mA/cm2；
(2), after control gas flow rate is stable, boron triflouride gas is collected with gas collecting bottle.
The present invention is not limited by above-mentioned embodiment, other any spirit without departing from the present invention
With the change made under principle, modify, substitute, combine, simplify, all should be the substitute mode of equivalence, all
Within being included in protection scope of the present invention.
Claims (8)
1. the preparation method of a boron triflouride gas, it is characterised in that comprise the following steps:
1) with inert electrode as anode, with inert electrode as negative electrode, mixed with Sodium fluoroborate and boric acid
Heshui solution is anolyte, with acid solution, aqueous slkali or saline solution as catholyte, at sun
Ionic membrane is in the two-compartment cell of barrier film, controls temperature and is 60-90 DEG C, uses Constant Electric Current
Solve or the mode of constant-potential electrolysis is electrolysed；
2) in electrolytic process, controlling gas flow rate stable, the gas of generation passes through purifier respectively
It is collected with collection device, obtains pure boron triflouride gas.
2. preparation method as claimed in claim 1, it is characterised in that: step 1) in, described acid solution is dense
Aqueous hydrochloric acid solution or concentration that degree is 0.1-1mol/L are the aqueous sulfuric acid of 0.1-1mol/L.
3. preparation method as claimed in claim 1, it is characterised in that: step 1) in, described aqueous slkali is dense
Sodium hydrate aqueous solution or concentration that degree is 0.1-1mol/L are the potassium hydroxide aqueous solution of 0.1-1mol/L.
4. preparation method as claimed in claim 1, it is characterised in that: step 1) in, described saline solution is dense
Sodium-chloride water solution or concentration that degree is 0.1-1mol/L are the aqueous sodium carbonate of 0.1-1mol/L.
5. preparation method as claimed in claim 1, it is characterised in that: step 1) in, described cationic membrane is
Perfluorinated sulfonic acid cation exchange membrane.
6. preparation method as claimed in claim 1, it is characterised in that: step 1) in, the electric current of constant-current electrolysis
For 0.08-0.8A, electric current density is 1-100mA/cm2, voltage range 10-300V of constant-potential electrolysis.
7. preparation method as claimed in claim 1, it is characterised in that: step 1) in, described inert electrode is
Glass-carbon electrode, graphite electrode, Ti electrode or platinum electrode.
8. preparation method as claimed in claim 1, it is characterised in that: step 1) in, described Sodium fluoroborate
Concentration is 0.1-5mol/L, and the concentration of described boric acid is 0.1-2mol/L.
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| CN105803480B CN105803480B (en) | 2018-02-13 |
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3635673A (en) * | 1970-07-31 | 1972-01-18 | United States Steel Corp | Fluorination of boric acid and phosphorous acid |
| DE2128682A1 (en) * | 1971-06-09 | 1973-02-08 | Basf Ag | Boron trifluoride prodn - by dissolving boron cpd in sulphuric acid, adding sulphur trioxide and introducing fluorspar |
| CN101393867A (en) * | 2007-09-21 | 2009-03-25 | 大日本网屏制造株式会社 | Substrate processing apparatus |
| CN102180475A (en) * | 2010-11-23 | 2011-09-14 | 王嘉兴 | Method for preparing boron fluoride and hydrochloric acid by using boron slurry washing liquor |
| CN102249256A (en) * | 2011-06-10 | 2011-11-23 | 格兰特医药科技(南通)有限公司 | Process for preparing boron trifluoride gas |
| CN102432030A (en) * | 2011-12-16 | 2012-05-02 | 天津市泰亨气体有限公司 | Method for preparing boron trifluoride |
| CN102515191A (en) * | 2011-12-16 | 2012-06-27 | 天津市泰亨气体有限公司 | Method for preparing boron trifluoride through reacting fluosulfonic acid with boric acid |
| CN103364259A (en) * | 2013-07-09 | 2013-10-23 | 青岛隆盛晶硅科技有限公司 | Pretreatment method for detecting impurities in polycrystalline silicon by heating volatile silicon in paraffin bath |
-
2016
- 2016-05-09 CN CN201610301967.2A patent/CN105803480B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3635673A (en) * | 1970-07-31 | 1972-01-18 | United States Steel Corp | Fluorination of boric acid and phosphorous acid |
| DE2128682A1 (en) * | 1971-06-09 | 1973-02-08 | Basf Ag | Boron trifluoride prodn - by dissolving boron cpd in sulphuric acid, adding sulphur trioxide and introducing fluorspar |
| CN101393867A (en) * | 2007-09-21 | 2009-03-25 | 大日本网屏制造株式会社 | Substrate processing apparatus |
| CN102180475A (en) * | 2010-11-23 | 2011-09-14 | 王嘉兴 | Method for preparing boron fluoride and hydrochloric acid by using boron slurry washing liquor |
| CN102249256A (en) * | 2011-06-10 | 2011-11-23 | 格兰特医药科技(南通)有限公司 | Process for preparing boron trifluoride gas |
| CN102432030A (en) * | 2011-12-16 | 2012-05-02 | 天津市泰亨气体有限公司 | Method for preparing boron trifluoride |
| CN102515191A (en) * | 2011-12-16 | 2012-06-27 | 天津市泰亨气体有限公司 | Method for preparing boron trifluoride through reacting fluosulfonic acid with boric acid |
| CN103364259A (en) * | 2013-07-09 | 2013-10-23 | 青岛隆盛晶硅科技有限公司 | Pretreatment method for detecting impurities in polycrystalline silicon by heating volatile silicon in paraffin bath |
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| CN105803480B (en) | 2018-02-13 |
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