CN102432030A - Method for preparing boron trifluoride - Google Patents
Method for preparing boron trifluoride Download PDFInfo
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- CN102432030A CN102432030A CN2011104234014A CN201110423401A CN102432030A CN 102432030 A CN102432030 A CN 102432030A CN 2011104234014 A CN2011104234014 A CN 2011104234014A CN 201110423401 A CN201110423401 A CN 201110423401A CN 102432030 A CN102432030 A CN 102432030A
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- boron trifluoride
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Abstract
The invention discloses a method for preparing boron trifluoride by reacting a mixture of boric acid and sulfuric acid with hydrogen fluoride. The method comprises the following step of: reacting the mixture of 400 to 500 liter/hour of boric acid and 1,000 to 1,200 liter/hour of sulfuric acid with 100 to 120 liter/hour of hydrogen fluoride at the temperature of between 700 and 800 DEG C under the dehydration action of 1,000 to 1,200 liter/hour of fuming sulfuric acid to obtain a boron trifluoride crystal. The preparation method has a reasonable process, makes the boron trifluoride prepared easily and is the simplest ideal technology for preparing the boron trifluoride.
Description
Technical field
The present invention relates to a kind of Chemicals, particularly a kind of from preparing the technology of boron trifluoride with hydrogen fluoride reaction by boric acid and vitriolic mixture, be suitable for the large-scale industrial production boron trifluoride
Background technology
boron trifluoride is a kind of important catalyst of organic synthesis and petrochemical complex widespread use, in a lot of organic chemical reactionses such as processes such as alkylation, polymerization, isomerizing, addition, condensation and decomposition, application is arranged all.It why aspect catalyzed reaction just like this wide application field, be because the boron electron structure has the strong tendency that generates complex compound, produce the catalytic activity structure at an acidic catalyst, this point is extremely important.In many reactions, be that the catalyzer on basis is more active than the halogenide catalysis efficiency of the sour metal of nature's mystery with the boron trifluoride, and be unlikely and cause disadvantageous side reaction.As catalyzer, BF3 can use under various forms, for example uses with independent gaseous state, and perhaps inorganic the and organic agent with many types together uses; And the complex compound of processing it is used.Simultaneously, it can adopt distillation or chemical process recoverys of regenerating again, reuses through making with extra care.BF
3
Reach other compound and in epoxy resin, use solidifying agent, in gathering enzyme dyeing keratin-fiber, the pure dissolubility resol of manufacturing, also be widely used.Prior art can only be used boric anhydride B
2
O
3
With sulfuric acid reaction, cost is very high, and is very big to equipment corrosion.
(1) organic catalyst compound:
BF
3
In many organic syntheses, take on katalysis.As in the suitability for industrialized production of middle molecular weight PIB, adopt BF
3
Catalystsystem not only can be simplified production equipment, shortens the production cycle, reduce labour intensity, and can significantly improve the yield of PIB.
(2) ion boriding
It is 1917 that
" boronising " term occurs in document for the first time, but the special detail file of relevant boronising processing layer just occurred after 50 years.
boronising or boronation is a kind of austenite chemistry thermal treatment that is applied to black and nonferrous materials, makes its surface generate the hardened layer that contains boride.The hardness of boride layer has good wear resistance and corrosion stability up to 2000HV.
need not on gas circuit, to heat because boron trifluoride is more easy to operate, in burner hearth, be more evenly distributed, and because the content of its boron is higher, so be usually used in the carrier gas of boron in the ion boriding.
(3) be used as the normal temperature quick curing agent
BF
3
It is epoxy resin normal temperature quick curing agent.BF
3
Need to separate packing as solidifying agent, with using with acid with epoxy resin.Mixing ratio error influences bonding quality during operation, and technology is loaded down with trivial details.The solid matter of at present selecting different melting points is processed minigel as lapping with BF3, through cyst wall blocking-up epoxy resin and BF
3
Effect, thus process single one-tenth product and can stablize storage, select release temperature through capsule material fusing point, capsule material is emitted the BF3 solidifying agent under this temperature, mixes with epoxy resin, impels its fast setting.And can improve the kindliness of cured epoxy resin through selecting the stickiness and the molecular chain length of capsule materials/substances.
(4) nuclear technology field is used
generate trimethyl borate with boron trifluoride-10-etherate and calcium chloride reaction, hydrolysis then, and after inspissation, the high-purity boric acid that obtains can be used for nuclear reactor as neutron moderator.
BF3
Some complex compound with 10 BF
3
Form enrichment 10B, can be used for separating the isotropic substance of boron.And 10 BF
3
Can the ratio in nuclear technique be to be used as the neutron absorbing medium in the sub-telltale, and be used for the control of nuclear reactor.
(5) source ion implantation of process for fabrication of semiconductor device
boron trifluoride is used as source ion implantation in process for fabrication of semiconductor device, can improve the performance of semiconducter device.
IV family Siliciumatom crystal in the periodic table of elements is doping V family's atomic time, can conduct electricity because of out-shell electron has more a unbound electron.We claim N type impurity V family impurity, and call donor to the atom that generates unbound electron.When doping III family's atomic time, opposite with above-mentioned situation, hole appears because of lacking an electronics.In this hole, contiguous electronics can be jumped into, and can move in order.This III type impurity is called p type impurity, and the principle in production hole then is called acceptor.
are common, and phosphorus and arsenic use as N type impurity, and boron then uses as p type impurity, and this impurity is called doping.Usually, doping ratio is 1 impurity that mixes in 106-107 the Siliciumatom, to form a conduction region.
doping method has thermal diffusion method and ion implantation.Thermodiffusion is to place diffusion furnace to silicon chip, in the atmosphere of impurity gas, is heated to about 1000 ℃, and at this moment impurity atoms just diffuses in the silicon crystallization, thereby forms a kind of method of conduction region.The normally used gas of thermal diffusion method has diborane (B for the P type
2
H
6
), the N type has phosphuret-(t)ed hydrogen (PH3) and hydrogen arsenide (AsH
3
).
ion implantation is in a vacuum in electric field, quickening after the impurity atoms ionize, squeezes into intracrystalline technology to ion then.The gas that ion implantation is used has boron trifluoride (BF
3
), phosphuret-(t)ed hydrogen and hydrogen arsenide.Ion implantation is selected required ion because of its inside is equipped with spectrometry mass, so the influence of few impurities.In addition, ion implantation amount can be controlled, and the ion implantation degree of depth and position can be regulated through electric field adjusting, therefore superior than thermal diffusion method.
(6) metallurgical and welding
BF
3
Can prevent that magnesium and alloy thereof from oxygenizement taking place when fusion is cast, when welding magnesium material, be used as solder flux.It also is used as the component of steel or other metallic surface puffing agent, also is used as the lubricant of cast steel, in the arc welding of titanium, participates in if any BF3, and weld seam just has stronger shock resistance.
(7) synthetic diborane
Use BF
3
Can prepare borine.It and alkalimetal hydride are reacted into diborane.Generate organoboron compound with the Grignard reagent react.
(8) medical
Along with the technical progress of medical field, new antibiotic medicine constantly is developed
.The building-up process of these microbiotic new drugs needs boron triflouride gas as catalyzer
Summary of the invention
problem to be solved by this invention is; Overcome the deficiency of prior art; A kind of preparation method of boron trifluoride is provided, under oleum 1000-1200 liter/hour continuous dehydration that adds, under 700-800 ℃ of temperature; Continuously 400-500 liter/hour boric acid and 1000-1200 liter/hour vitriolic mixture are prepared boron trifluoride with 100-120 liter/hour hydrogen fluoride reaction, its mesoboric acid and vitriolic volume ratio are 1:10.Hydrogen fluoride reaction prepares boron trifluoride this law can generate this law on the basis of fluorite boric anhydride method, with cheap borax (Na
2
B
4
O
7
) the expensive boric anhydride (B of replacement
2
O
3
), production cost is lower.
Disclosing that
the present invention is more concrete is a kind of from prepared the technology of boron trifluoride with hydrogen fluoride reaction by boric acid and vitriolic mixture; Utilize the dehydration of oleum; Under proper temperature, can make the boric acid dehydration obtain the boron trioxide crystal.Reaction formula does
H
3
BO
3
+?3HF ?
BF
3
?+?3H
2
O
H
2
O?+?H
2
SO
4
·S0
3
?
2H
2
SO
4
A kind of device for preparing boron trifluoride by boric acid and sulfuric acid mixture with hydrogen fluoride reaction that
are shown in Figure 1; Comprise knockout tower, mixing tank and reaction tower; Knockout tower is respectively equipped with the inlet 101 of knockout tower, the outlet 1 of knockout tower, the outlet 2 103 of knockout tower, the outlet 3 104 of knockout tower; The outlet two of knockout tower is through the inlet 1 of pipeline ligation tower; The outlet three of knockout tower connects the inlet 1 of mixing tank through pipeline; The outlet 203 of mixing tank is through the inlet 2 302 of pipeline ligation tower, and mixing tank is provided with the inlet 2 202 of mixing tank, and reaction tower is provided with the outlet 304 of the inlet 2 303 and the reaction tower of reaction tower.
The quality determination result of the boron trifluoride of the present invention's preparation is following:
Fusing point (101.325kPa) :-127.1 ℃
Boiling point (101.325KPa) :-99.8 ℃
Fluid density (100.3 ℃, 101.325kpa): 1589kg/m
3
Gas density (20 ℃, 101.325kpa): 2.867kg/m3
Specific density (air=1.20 ℃, 101.325kpa): 2.380
Specific volume (21.1 ℃, 101.325kpa): 0.3496 m
3
/ kg
The gas-liquid volumetric ratio (15 ℃, 10OKPa): 560L/L
Critical temperature :-12.2 ℃
Emergent pressure: 4985KPa
Critical density: 594kkg/m
3
The method that the present invention prepares boron trifluoride with hydrogen fluoride reaction by boric acid and sulfuric acid mixture compared with prior art has the following advantages:
(1) present method can continous-stable the production boron trifluoride, solved that original intermittence, essence fed intake can not stably manufactured drawback.
(2) integrated continuous rectification can better utilised cold and heat, makes production cost lower.
Steady quality behind
(3) continuous production can large-scale industrial production.
Description of drawings:
Fig. 1 is the process flow sheet of boron trioxide; Wherein: 1, the inlet 3 304 of the inlet 2 303 of the inlet 1 of the outlet 3 of the inlet 2 203 of the inlet 1 of the outlet 32 of the outlet 2 104 of the outlet 1 of the inlet 102 of knockout tower 101, knockout tower, knockout tower, knockout tower, knockout tower, mixing tank 201, mixing tank, mixing tank, mixing tank, reaction tower 301, reaction tower, reaction tower, reaction tower, the outlet of reaction tower.
Embodiment:
The present invention is explained below in conjunction with embodiment in
; The scheme of embodiment described here; Do not limit the present invention; One of skill in the art can make improvements and change according to spirit of the present invention, and described these improvement and variation all should be regarded as within the scope of the invention, and scope of the present invention and essence are limited claim.
are under 1000 liters of/hour dehydrations that add continuously of oleum; Under 700-800 ℃ of temperature; Continuously 400 liters of/hour boric acid and 1000 liters of/hour vitriolic mixtures are prepared boron trifluoride with 100 liters of/hour hydrogen fluoride reactions, its mesoboric acid and vitriolic volume ratio are 1:10 prepared in reaction boron trifluoride.
Write out the process of preparation according to the description of Fig. 1:
A kind of device for preparing boron trifluoride by boric acid and sulfuric acid mixture with hydrogen fluoride reaction shown in Figure 1; Comprise knockout tower, mixing tank and reaction tower; Knockout tower is respectively equipped with the inlet 101 of knockout tower, the outlet 1 of knockout tower, the outlet 2 103 of knockout tower, the outlet 3 104 of knockout tower; The outlet two of knockout tower is through the inlet 1 of pipeline ligation tower, and the outlet three of knockout tower is through the inlet 1 of pipeline connection mixing tank, and the outlet 203 of mixing tank is through the inlet 2 302 of pipeline ligation tower; Mixing tank is provided with the inlet 2 202 of mixing tank, and reaction tower is provided with the outlet 304. of the inlet 2 303 and the reaction tower of reaction tower
are under 1200 liters of/hour dehydrations that add continuously of oleum; Under 800 ℃ of temperature; Continuously 500 liters of/hour boric acid and 1200 liters of/hour vitriolic mixtures are prepared boron trifluoride with 120 liters of/hour hydrogen fluoride reactions, its mesoboric acid and vitriolic volume ratio are 1:10 prepared in reaction boron trifluoride.
A kind of device for preparing boron trifluoride by boric acid and sulfuric acid mixture with hydrogen fluoride reaction shown in Figure 1; Comprise knockout tower, mixing tank and reaction tower; Knockout tower is respectively equipped with the inlet 101 of knockout tower, the outlet 1 of knockout tower, the outlet 2 103 of knockout tower, the outlet 3 104 of knockout tower; The outlet two of knockout tower is through the inlet 1 of pipeline ligation tower, and the outlet three of knockout tower is through the inlet 1 of pipeline connection mixing tank, and the outlet 203 of mixing tank is through the inlet 2 302 of pipeline ligation tower; Mixing tank is provided with the inlet 2 202 of mixing tank, and reaction tower is provided with the outlet 304 of the inlet 2 303 and the reaction tower of reaction tower
Claims (1)
1. the preparation method of a boron trifluoride; It is characterized in that: under oleum 1000-1200 liter/hour continuous dehydration that adds; Under 700-800 ℃ of temperature; Continuously 400-500 liter/hour boric acid and 1000-1200 liter/hour vitriolic mixture are prepared boron trifluoride with 100-120 liter/hour hydrogen fluoride reaction, its mesoboric acid and vitriolic volume ratio are 1:10.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011104234014A CN102432030A (en) | 2011-12-16 | 2011-12-16 | Method for preparing boron trifluoride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011104234014A CN102432030A (en) | 2011-12-16 | 2011-12-16 | Method for preparing boron trifluoride |
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| Publication Number | Publication Date |
|---|---|
| CN102432030A true CN102432030A (en) | 2012-05-02 |
Family
ID=45980440
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105803480A (en) * | 2016-05-09 | 2016-07-27 | 上海应用技术学院 | Preparation method of boron trifluoride gas |
| CN106248520A (en) * | 2016-07-19 | 2016-12-21 | 苏州金宏气体股份有限公司 | A kind of detect the method and device of hydrogen fluoride content in boron trifluoride unstripped gas |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101508443A (en) * | 2009-03-31 | 2009-08-19 | 核工业理化工程研究院华核新技术开发公司 | Method for producing boron triflouride gas |
| 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 |
-
2011
- 2011-12-16 CN CN2011104234014A patent/CN102432030A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101508443A (en) * | 2009-03-31 | 2009-08-19 | 核工业理化工程研究院华核新技术开发公司 | Method for producing boron triflouride gas |
| 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 |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105803480A (en) * | 2016-05-09 | 2016-07-27 | 上海应用技术学院 | Preparation method of boron trifluoride gas |
| CN106248520A (en) * | 2016-07-19 | 2016-12-21 | 苏州金宏气体股份有限公司 | A kind of detect the method and device of hydrogen fluoride content in boron trifluoride unstripped gas |
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Application publication date: 20120502 |