CN106800299A - The quick preparation technology of high-purity boron trifluoride and recovery process for purification - Google Patents
The quick preparation technology of high-purity boron trifluoride and recovery process for purification Download PDFInfo
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- CN106800299A CN106800299A CN201710062207.5A CN201710062207A CN106800299A CN 106800299 A CN106800299 A CN 106800299A CN 201710062207 A CN201710062207 A CN 201710062207A CN 106800299 A CN106800299 A CN 106800299A
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- boron trifluoride
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- WTEOIRVLGSZEPR-UHFFFAOYSA-N boron trifluoride Chemical compound FB(F)F WTEOIRVLGSZEPR-UHFFFAOYSA-N 0.000 title claims abstract description 189
- 229910015900 BF3 Inorganic materials 0.000 title claims abstract description 93
- 238000005516 engineering process Methods 0.000 title claims abstract description 17
- 238000000746 purification Methods 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000011084 recovery Methods 0.000 title claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 31
- 238000006243 chemical reaction Methods 0.000 claims abstract description 25
- 229910001512 metal fluoride Inorganic materials 0.000 claims abstract description 13
- 230000008569 process Effects 0.000 claims abstract description 13
- -1 tetrafluoroborate Chemical compound 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims description 18
- 239000003054 catalyst Substances 0.000 claims description 15
- 229910001496 lithium tetrafluoroborate Inorganic materials 0.000 claims description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 12
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 claims description 12
- 239000002904 solvent Substances 0.000 claims description 7
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 6
- 229910052744 lithium Inorganic materials 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 229910001220 stainless steel Inorganic materials 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 5
- 238000007670 refining Methods 0.000 claims description 5
- 239000010935 stainless steel Substances 0.000 claims description 5
- ZQXCQTAELHSNAT-UHFFFAOYSA-N 1-chloro-3-nitro-5-(trifluoromethyl)benzene Chemical compound [O-][N+](=O)C1=CC(Cl)=CC(C(F)(F)F)=C1 ZQXCQTAELHSNAT-UHFFFAOYSA-N 0.000 claims description 4
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 4
- 229910052796 boron Inorganic materials 0.000 claims description 4
- 230000008859 change Effects 0.000 claims description 3
- UNWSCLFRWCYCHG-UHFFFAOYSA-N ethyl acetate;trifluoroborane Chemical compound FB(F)F.CCOC(C)=O UNWSCLFRWCYCHG-UHFFFAOYSA-N 0.000 claims description 3
- 238000003682 fluorination reaction Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 5
- 230000008901 benefit Effects 0.000 abstract description 4
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical group [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 description 18
- 239000007789 gas Substances 0.000 description 12
- 239000012530 fluid Substances 0.000 description 6
- 239000000376 reactant Substances 0.000 description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- AFFLGGQVNFXPEV-UHFFFAOYSA-N n-decene Natural products CCCCCCCCC=C AFFLGGQVNFXPEV-UHFFFAOYSA-N 0.000 description 4
- 238000006116 polymerization reaction Methods 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 3
- 229920002367 Polyisobutene Polymers 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000000314 lubricant Substances 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 229910000619 316 stainless steel Inorganic materials 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- NIQCNGHVCWTJSM-UHFFFAOYSA-N Dimethyl phthalate Chemical compound COC(=O)C1=CC=CC=C1C(=O)OC NIQCNGHVCWTJSM-UHFFFAOYSA-N 0.000 description 2
- VQTUBCCKSQIDNK-UHFFFAOYSA-N Isobutene Chemical compound CC(C)=C VQTUBCCKSQIDNK-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 239000010436 fluorite Substances 0.000 description 2
- 230000000977 initiatory effect Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 239000011343 solid material Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- WVDDGKGOMKODPV-UHFFFAOYSA-N Benzyl alcohol Chemical compound OCC1=CC=CC=C1 WVDDGKGOMKODPV-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- UYAGPULHTNCMOT-UHFFFAOYSA-N [B].FB(F)F Chemical compound [B].FB(F)F UYAGPULHTNCMOT-UHFFFAOYSA-N 0.000 description 1
- 238000007259 addition reaction Methods 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 230000029936 alkylation Effects 0.000 description 1
- 238000005804 alkylation reaction Methods 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 150000005415 aminobenzoic acids Chemical class 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910021538 borax Inorganic materials 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000011365 complex material Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- FBSAITBEAPNWJG-UHFFFAOYSA-N dimethyl phthalate Natural products CC(=O)OC1=CC=CC=C1OC(C)=O FBSAITBEAPNWJG-UHFFFAOYSA-N 0.000 description 1
- 229960001826 dimethylphthalate Drugs 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 1
- 238000005468 ion implantation Methods 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- 238000006053 organic reaction Methods 0.000 description 1
- 239000003209 petroleum derivative Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000012985 polymerization agent Substances 0.000 description 1
- 239000002685 polymerization catalyst Substances 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 235000011121 sodium hydroxide Nutrition 0.000 description 1
- 239000004328 sodium tetraborate Substances 0.000 description 1
- 235000010339 sodium tetraborate Nutrition 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B35/00—Boron; Compounds thereof
- C01B35/06—Boron halogen compounds
- C01B35/061—Halides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B35/00—Boron; Compounds thereof
- C01B35/06—Boron halogen compounds
- C01B35/063—Tetrafluoboric acid; Salts thereof
- C01B35/066—Alkali metal tetrafluoborates
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
Abstract
The invention discloses the quick preparation technology of high-purity boron trifluoride and recovery process for purification.It is raw material to use solid-state boron trifluoride complex, carries out reaction and prepares gaseous state high-purity boron trifluoride；Tetrafluoroborate is generated using the boron trifluoride reaction in metal fluoride and material, is then peeled off, reclaimed refined tetrafluoroborate.The quick preparation technology of high-purity boron trifluoride of the invention and reclaim process for purification and have that technological process is simple, it is quick to prepare, the advantages of reclaiming that product cost is low, be worth high.
Description
Technical field
The present invention relates to the quick preparation technology of high-purity boron trifluoride and recovery process for purification, belong to fine chemical technology neck
Domain.
Background technology
High-purity boron trifluoride gas is silicon and germanium extension, the p-type doped source of diffusion and ion implantation process and prepares optical fiber
The raw material of prefabricated component；The boron trifluoride complex that high-purity boron trifluoride, boron trifluoride and part are constituted is used as alkylation, isomery
Catalyst in the various chemical reactions such as change, polymerization, decomposition, dehydration is applied to many organic reactions and petroleum product；High-purity three
Boron fluoride is also applied in ratio neutron counter and controllable neutron reactor.
Preparing the method for boron triflouride gas has various, and the conventional method for preparing boron triflouride gas has borofluoride
Method, fluorite boric anhydride method, fluorite borax method etc..CN101214970B discloses a kind of technique side for preparing high-purity boron trifluoride gas
Method is to produce boron triflouride gas with pure boron direct synthesis technique with fluorine gas, and impure boron triflouride gas are by dedusting and essence
Evaporating can stably prepare high-purity boron trifluoride gas；The above method is complicated, and scale, investment are very big.
Will after being terminated using the reaction of catalyst boron trifluoride, boron trifluoride complex, it is necessary to from reactant mixture
Catalyst is separated, removed.Be typically employed in the aqueous solution of the alkaline matters such as ammonia, caustic soda and after wash the method for removing with water.
United States Patent (USP) 4227027 contains more than 2 by the addition in the reactant mixture containing boron trifluoride catalyst
There is addition reaction in the boron trifluoride in the polyalcohol and composition catalyst of alkyl, so as to remove boron trifluoride, add by Dui
The method that heat resolve reclaims boron trifluoride is carried out into product.
Unexamined Patent 6-287211 publications make the boron trifluoride gas of generation and relative to trifluoro by heating response mixture
Change the ligand contact of boron excess amount, new complex is formed, to the method for cycling and reutilization in reactive tank.Match somebody with somebody there is boron trifluoride
Position body catalyst is heated in the case of coexisting to reactant mixture, is produced not it is possible to the composition to reactant mixture
Good influence, has the shortcomings that purposes limitation is very big.
Unexamined Patent 2-45429 publications are, as catalyst, to carry out olefines and aromatic series with boron trifluoride ether complex
The alkylated reaction of compound, adds phosphoric acid, acetic acid, the benzene of 0.05-2 moles before the reaction or in the backward reaction system of reaction
The weak acid such as phenol, then standing is layered catalyst member, and the catalyst layer of separation is intactly used as into urging for lower secondary response
Agent.
It is that boron trifluoride/weak acid that weak acid of the recovery by adding is replaced after reclaiming is complex-catalyzed as the acid of part
Agent, rather than the boron trifluoride ether composition catalyst at the initial stage of recovery；So its rate of recovery is very low, about 27% weight.
The polymerization catalyst of United States Patent (USP) 4152499 is used by gaseous state boron trifluoride or the boron trifluoride formed with water or alcohols
Complex, within the temperature range of -50 DEG C to 300 DEG C, makes isobutene polymerisation obtain polyisobutene.European patent (EP-A)
No. 145,235 use the boron trifluoride alcohol composition catalyst for forming complex by boron trifluoride and C1-C8 alcohol to be urged as polymerization
Agent obtains polyisobutene.CN102807640B is based on the initiation system and the method for preparing polyisobutene of boron trifluoride,
The initiation system is made up of BF3, proton donor and electron donor, and proton donor may be selected from water, methyl alcohol, ethanol, phenol, adjacent first
Phenol, aromatic alcohol or aminobenzoic acids.
CN1217726A is by disperseing and dissolving at least one of non-conducting fluids of boron trifluoride complex
Apply direct current and alternating voltage, boron trifluoride complex sedimentation separation is made from non-conducting fluids, mol ratio can not be changed
Reclaim complex.It is used in the manufacture using the olefin oligomer of boron trifluoride complex by by the method, by urging for reclaiming
Agent can be reused in reaction same as before.
CN1289344A makes the fluid containing boron trifluoride or boron trifluoride complex be contacted with metal fluoride, has
Optionally adsorb the boron trifluoride in the complex.The tetrafluoro boric acid slaine that will be generated is in 100-600 DEG C of temperature model
Enclose interior heating, be allowed to be separated into boron trifluoride and metal fluoride, in this way can economically, with what can be recycled
State reclaims boron trifluoride, does not result in environmental pollution.
The recovery technology of above-mentioned boron trifluoride is to have accomplished the recovery of portion of boron trifluoride boron, recycled..
The content of the invention
It is an object of the invention to provide the quick preparation technology of high-purity boron trifluoride and reclaim process for purification, with it is simple, economical,
Mode free from environmental pollution, quickly, expeditiously prepares high-purity boron trifluoride, and to containing boron trifluoride or its complex
Material in remove the method for price boron trifluoride high and harmful, with technological process it is simple, prepare quick, reclaim product
The advantages of low cost, value high.
The quick preparation technology of high-purity boron trifluoride of the invention and recovery process for purification are achieved through the following technical solutions：
1st, the quick preparation technology of high-purity boron trifluoride and recovery process for purification, it is characterised in that：High-purity boron trifluoride is quickly prepared
Technique is that under uniform temperature, certain pressure, it is raw material to use solid-state boron trifluoride complex under high pure nitrogen protection,
Indirectly heat solid-state boron trifluoride complex in stainless steel reactor, prepares gaseous state boron trifluoride；High-purity boron trifluoride reclaims essence
Method processed is to generate tetrafluoroborate with the boron trifluoride reaction in chemical reactor using metal fluoride, is then peeled off, returns
Receive refined tetrafluoroborate.
2nd, the quick preparation technology of high-purity boron trifluoride according to claim 1, it is characterised in that：Reaction temperature is 50
DEG C -200 DEG C, reaction pressure is 0.05MPa-1.0MPa.
3rd, the quick preparation technology of high-purity boron trifluoride according to claim 1, it is characterised in that：Solid-state boron trifluoride
Complex compound is boric carbonic acid dimethyl ester complex trifluoride, or boron trifluoride ethyl acetate complex compound, or the mixture of the two.
4th, high-purity boron trifluoride according to claim 1 reclaims process for purification, it is characterised in that：Metal fluoride is
Lithium fluoride, tetrafluoroborate is LiBF4；Metal fluoride fluorinating lithium addition is chemical catalyst boron trifluoride quality
1 times to 20 times.
5th, high-purity boron trifluoride according to claim 1 reclaims process for purification, it is characterised in that：Metal fluoride with
Boron trifluoride reaction temperature is 20 DEG C -150 DEG C.
6th, high-purity boron trifluoride according to claim 1 reclaims process for purification, it is characterised in that：Tetrafluoroborate
It is dimethyl carbonate to reclaim refining solvent, or ethyl acetate, or the mixture of the two；It is four to reclaim refining solvent addition
3 times to 30 times of borofluoride quality.
Present invention has the advantages that：
1st, using the boric carbonic acid dimethyl ester complex trifluoride of solid-state, or boron trifluoride ethyl acetate complex compound, or the two
Mixture be raw material, normal temperature and pressure conditionses can just meet needs, it is not necessary to build complicated process units and special dangerous material
Storehouse.
2nd, the reaction temperature of the quick preparation technology of high-purity boron trifluoride is 50 DEG C -200 DEG C, and reaction pressure is 0.05MPa-
1.0MPa；Mild condition, pressure are low, quick as needed whenever and wherever possible can prepare.
3rd, LiBF4 is generated using the boron trifluoride reaction in metal fluoride fluorinating lithium and chemical reactor, is had
Reaction temperature is low, react thoroughly advantage, can greatly improve the rate of recovery of boron trifluoride.
4th, the LiBF4 separated, is dissolved in dimethyl carbonate and ethyl acetate, can be complexed boron trifluoride
The dimethyl carbonate or ethyl acetate in thing separate are recycled as refining solvent.
5th, the LiBF4 generated using the boron trifluoride reaction in metal fluoride fluorinating lithium and chemical reactor, be
Critically important lithium battery material, market value is high, serves increment effect.
With reference to specific embodiment, the present invention is further detailed explanation, but and is not so limited of the invention
Protection domain.
Specific embodiment
The quick Preparation equipment of boron trifluoride is 316 stainless steel reactors with heating jacket that volume is 10 liters, instead
Answer device with high pure nitrogen displacement pipeline, gas boron trifluoride discharging pipeline and solid material charge door, reactor top is installed
There are pressure gauge and thermometer.
It is the pilot-plant for being applied to positive decene batchwise polymerization synthetic lubricant fluid, catalyst that boron trifluoride reclaims purification apparatus
It is boron trifluoride；Equipment includes the stainless steel stirring reaction of the jacketed that positive decene polymerization synthetic lubricant fluid pilot-plant is 50 liters
Device, 50 liters of stainless steel stand device and 20 liters of distillation treater.
The high-purity high-purity boron trifluoride of embodiment 1 is quickly prepared
316 stainless steel boron trifluoride reaction devices first are replaced with high pure nitrogen, 3 kilograms of boron trifluorides are added under high pure nitrogen protection
Carbonic acid dimethyl ester complex（Boron trifluoride content is 42%）, close solid material charge door.Start heat temperature raising, make chuck heat
Matchmaker's temperature is maintained at 90-95 DEG C, decomposes boric carbonic acid dimethyl ester complex trifluoride and produces gaseous state high-purity boron trifluoride；Reactor
It is slow to open gas boron trifluoride discharging pipeline when interior pressure reaches 0.2MPa, for reactor provides high-purity boron trifluoride gas
Catalyst.
The high-purity boron trifluoride of embodiment 2 reclaims refined
The stainless steel of 50 liters of jacketed stirs positive decene polymerization synthetic lubricant fluid reactor, and total material addition is 25 kilograms,
Boron trifluoride addition is 0.8 kilogram.
After reaction reaches terminal, under high pure nitrogen protection and stirring, it is more than to purity is slowly added in reactant
99.5% 100 3 kilograms of mesh powder lithium fluoride.
At being 30-60 DEG C in temperature, lithium fluoride is set fully to react generation LiBF4 with boron trifluoride, then by material
Add 50 liters of stainless steels to stand device, make the LiBF4 and feed separation of unreacted powder lithium fluoride and generation.
First to addition n-hexane solvent in lithium fluoride and LiBF4 mixture, decene polymer in washed mixture,
Filtering, obtains 3.77 kilograms of lithium fluoride and LiBF4 mixture, the rate of recovery 97%.
12 kilograms of dimethyl carbonate is added to lithium fluoride and LiBF4 mixture again, LiBF4 is completely dissolved
To in dimethyl carbonate, lithium fluoride is separated with LiBF4；Unreacted lithium fluoride can be recycled.
The lithium tetrafluoroborate solution being dissolved into dimethyl carbonate above is taken to 20 liters of distillation treater, solvent carbon is boiled off
Dimethyl phthalate obtains 1.07 kilograms of solid LiBF4.
To those of ordinary skill in the art, under the premise without departing from the principles of the invention, it is possible to equipment
Structure, flow make some improvements and modifications, and these improvements and modifications also should be regarded as protection scope of the present invention.
Claims (6)
1. the quick preparation technology of high-purity boron trifluoride and reclaim process for purification, it is characterised in that：High-purity boron trifluoride is quickly prepared
Technique is that under uniform temperature, certain pressure, it is raw material to use solid-state boron trifluoride complex under high pure nitrogen protection,
Indirectly heat solid-state boron trifluoride complex in stainless steel reactor, prepares gaseous state boron trifluoride；High-purity boron trifluoride reclaims essence
Method processed is to generate tetrafluoroborate with the boron trifluoride reaction in chemical reactor using metal fluoride, is then peeled off, returns
Receive refined tetrafluoroborate.
2. the quick preparation technology of high-purity boron trifluoride according to claim 1, it is characterised in that：Reaction temperature is 50 DEG C-
200 DEG C, reaction pressure is 0.05MPa-1.0MPa.
3. the quick preparation technology of high-purity boron trifluoride according to claim 1, it is characterised in that：Solid-state boron trifluoride is complexed
Thing is boric carbonic acid dimethyl ester complex trifluoride, or boron trifluoride ethyl acetate complex compound, or the mixture of the two.
4. high-purity boron trifluoride according to claim 1 reclaims process for purification, it is characterised in that：Metal fluoride is fluorination
Lithium, tetrafluoroborate is LiBF4；Metal fluoride fluorinating lithium addition is 1 times of chemical catalyst boron trifluoride quality
To 20 times.
5. high-purity boron trifluoride according to claim 1 reclaims process for purification, it is characterised in that：Metal fluoride and trifluoro
It is 20 DEG C -150 DEG C to change boron reaction temperature.
6. high-purity boron trifluoride according to claim 1 reclaims process for purification, it is characterised in that：The recovery of tetrafluoroborate
Refining solvent is dimethyl carbonate, or ethyl acetate, or the mixture of the two；It is tetrafluoro boron to reclaim refining solvent addition
3 times to 30 times of hydrochlorate quality.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710062207.5A CN106800299A (en) | 2017-02-01 | 2017-02-01 | The quick preparation technology of high-purity boron trifluoride and recovery process for purification |
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| CN201710062207.5A CN106800299A (en) | 2017-02-01 | 2017-02-01 | The quick preparation technology of high-purity boron trifluoride and recovery process for purification |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113105586A (en) * | 2021-03-26 | 2021-07-13 | 广东新华粤树脂科技有限公司 | Method for recovering boron trifluoride catalyst in C9 petroleum resin preparation process |
Citations (5)
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