CN102515191A - Method for preparing boron trifluoride through reacting fluosulfonic acid with boric acid - Google Patents
Method for preparing boron trifluoride through reacting fluosulfonic acid with boric acid Download PDFInfo
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- CN102515191A CN102515191A CN2011104234067A CN201110423406A CN102515191A CN 102515191 A CN102515191 A CN 102515191A CN 2011104234067 A CN2011104234067 A CN 2011104234067A CN 201110423406 A CN201110423406 A CN 201110423406A CN 102515191 A CN102515191 A CN 102515191A
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- acid
- fluosulfonic
- boron trifluoride
- boric acid
- reaction
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Abstract
The invention discloses a method for preparing boron trifluoride through reacting fluosulfonic acid with boric acid. The preparation method is characterized in that boron trifluoride is prepared by mixing fluosulfonic acid with boric acid and reacting according to a pressure of 0.2-0.4MPa and a temperature of 87-93DEG C, wherein the weight ratio of boric acid to fluosulfonic acid is 1:2-4. The preparation method of the invention, which has the advantages of reasonable process and simple preparation, is a simplest and ideal technology for preparing boron trifluoride.
Description
Technical field
The present invention relates to a kind of Chemicals, particularly a kind of from prepare the technology of boron trifluoride by fluosulfonic acid and acid reaction, be suitable for producing on a large scale 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, BF
3
Can under various forms, use, for example use with independent gaseous state, 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.For example:
(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 as lapping, with BF
3
Process minigel, 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 BF under this temperature
3
Solidifying agent 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.
3
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 (PH
3
) 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, if any BF
3
Participate in, 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.
Original technology adopts more than fluorite and the boric acid mixing post-heating to 100 ℃, impurity such as SF during this reacts
4
Deng association simultaneously, boron trifluoride uses as catalyzer will influence result of use
Summary of the invention
Problem to be solved by this invention is, overcomes the deficiency of prior art, and this law replaces expensive boric anhydride (B with cheap fluorosulfuric acid on the basis of fluorite boric anhydride method
2
O
3
), production cost is lower.
The invention discloses following technology contents:
are a kind of to prepare the method for boron trifluoride by fluosulfonic acid and acid reaction, and it is characterized in that: it is that fluosulfonic acid is mixed with boric acid, prepared in reaction boron trifluoride under 0.2-0.4 MPA pressure and 87-93 ℃ of temperature; Its mesoboric acid is 1:2-4 with the weight fraction ratio of fluosulfonic acid.
The more detailed preparation method of the present invention is following:
the invention discloses a kind of from the technology by fluosulfonic acid (add-on is 10 kilograms/hour) and boric acid (ratio that adds fluosulfonic acid is 1:2-4) prepared in reaction boron trifluoride; Utilize the dehydration of fluorosulfuric acid; Under proper temperature, can make the boric acid dehydration obtain the boron trioxide crystal.Reaction formula does
?3HSO 3 F?+?H 3 BO 3 
?BF
3 ＋3H 2 SO 4
Integrated continuous dosing is adopted in
; Solid boric acid feed pot 1 gets into lixator 21 and lixator 22 through feeder; Boric acid after the lixator heating and melting feeds boric acid pump 41 and squeezes into reactor drum 5, and the fluosulfonic acid feed pot 3 in the fluosulfonic acid storage tank is also squeezed into reactor drum 5 through sour pump 42 at this moment, under 0.2-0.4 MPA pressure and 87-93 ℃ of temperature, reacts; Heat is provided by steam; Reaction generates boron triflouride gas and gets in the holding tanks 7 through interchanger 6 cooling backs and collect, and it is that sulfuric acid passes through liquid level monitoring 8 and discharges at any time that reaction reproduces resultant, is provided with the sulfuric acid discharging and exports.
The physico-chemical property of the boron trifluoride of the present invention's preparation:
Molecular weight: 67.805
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/m
3
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 compared with prior art has the following advantages:
(1) present method can continous-stable the production boron trifluoride that feeds intake, solved feed intake original intermittence can not stably manufactured drawback.
(2) integrated continuous dosing 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 technical process of preparation boron trifluoride; Wherein 1, solid boric acid feeder; 101, the outlet one of solid boric acid feeder; 102, the outlet two of solid boric acid feeder; 21, lixator one; The inlet one of 211 lixators one; 212, the inlet two of lixator one; 213, the outlet of lixator one; 22, lixator two; The inlet one of 221 lixators two; 222, the inlet two of lixator two; 223, the outlet of lixator two; 3, fluosulfonic acid feeder; 301, the outlet of fluosulfonic acid feeder; 41, boric acid pump; 411, the inlet of liquid boric acid; 412, the outlet of liquid boric acid; 42, fluosulfonic acid pump; 421, the inlet of fluosulfonic acid; 422, the outlet of fluosulfonic acid; 5, reactor drum; 501, the inlet one of reactor drum; 502, the inlet two of reactor drum; 503, the outlet one of reactor drum; The outlet two of 504 reactor drums; 51, steam jacket; 511, the inlet of steam; 512, the outlet of steam; 6, interchanger; 601, the inlet of interchanger; 602, the outlet of interchanger; 7, BF
3
Gas holder; 701, BF
3
The inlet of gas holder; 702, BF
3
The outlet of gas holder; 8, liquid monitoring; 801, vitriolic inlet; 802, vitriolic outlet; 803, sulfuric acid discharging outlet.
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 a kind of to prepare the method for boron trifluoride by fluosulfonic acid and acid reaction, and it is that fluosulfonic acid is mixed with boric acid, prepared in reaction boron trifluoride under 0.2 MPA pressure and 87 ℃ of temperature; Its mesoboric acid is 1:2 with the weight fraction ratio of fluosulfonic acid.Wherein said flow process: adopt integrated continuous dosing; Solid boric acid feed pot 1 gets into lixator 21 and lixator 22 through feeder, and the boric acid after the lixator heating and melting feeds boric acid pump 41 and squeezes into reactor drum 5, and the fluosulfonic acid feed pot 3 in the fluosulfonic acid storage tank is also squeezed into reactor drum 5 through sour pump 42 at this moment; Under 0.2MPA pressure and 87 ℃ of temperature, react; Heat is provided by steam, and reaction generates boron triflouride gas and gets in the holding tanks 7 through interchanger 6 cooling backs and collect, and it is that sulfuric acid passes through liquid level monitoring 8 and discharges at any time that reaction reproduces resultant; Be provided with sulfuric acid discharging outlet, see Fig. 1.
Embodiment 2
are a kind of to prepare the method for boron trifluoride by fluosulfonic acid and acid reaction, and it is characterized in that: it is that fluosulfonic acid is mixed with boric acid, prepared in reaction boron trifluoride under 0.4 MPA pressure and 93 ℃ of temperature; Its mesoboric acid is 1:4 with the weight fraction ratio of fluosulfonic acid, sees Fig. 1.
A kind ofly prepare the method for boron trifluoride by fluosulfonic acid and acid reaction, it is that fluosulfonic acid is mixed with boric acid, prepared in reaction boron trifluoride under 0.2 MPA pressure and 87 ℃ of temperature; Its mesoboric acid is 1:2 with the weight fraction ratio of fluosulfonic acid;
wherein said flow process: adopt integrated continuous dosing; Solid boric acid feed pot 1 gets into lixator 21 and lixator 22 through feeder, and the boric acid after the lixator heating and melting feeds boric acid pump 41 and squeezes into reactor drum 5, and the fluosulfonic acid feed pot 3 in the fluosulfonic acid storage tank is also squeezed into reactor drum 5 through sour pump 42 at this moment; Under 0.2MPA pressure and 87 ℃ of temperature, react; Heat is provided by steam, and reaction generates boron triflouride gas and gets in the holding tanks 7 through interchanger 6 cooling backs and collect, and it is that sulfuric acid passes through liquid level monitoring 8 and discharges at any time that reaction reproduces resultant; Be provided with sulfuric acid discharging outlet, see Fig. 1.
are a kind of to prepare the method for boron trifluoride by fluosulfonic acid and acid reaction, and it is characterized in that: it is that fluosulfonic acid is mixed with boric acid, prepared in reaction boron trifluoride under 0.3 MPA pressure and 90 ℃ of temperature; Its mesoboric acid is 1:3 with the weight fraction ratio of fluosulfonic acid.See Fig. 1
Claims (1)
1. one kind prepares the method for boron trifluoride by fluosulfonic acid and acid reaction, it is characterized in that:
It is that fluosulfonic acid is mixed with boric acid, prepared in reaction boron trifluoride under 0.2-0.4 MPA pressure and 87-93 ℃ of temperature; Its mesoboric acid is 1:2-4 with the weight fraction ratio of fluosulfonic acid; Described flow process: adopt integrated continuous dosing; Solid boric acid feed pot 1 gets into lixator 21 and lixator 22 through feeder; Boric acid after the lixator heating and melting feeds boric acid pump 41 and squeezes into reactor drum 5, and the fluosulfonic acid feed pot 3 in the fluosulfonic acid storage tank is also squeezed into reactor drum 5 through sour pump 42 at this moment, under 0.2-0.4 MPA pressure and 87-93 ℃ of temperature, reacts; Heat is provided by steam; Reaction generates boron triflouride gas and gets in the holding tanks 7 through interchanger 6 cooling backs and collect, and it is that sulfuric acid passes through liquid level monitoring 8 and discharges at any time that reaction reproduces resultant, is provided with the sulfuric acid discharging and exports.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011104234067A CN102515191A (en) | 2011-12-16 | 2011-12-16 | Method for preparing boron trifluoride through reacting fluosulfonic acid with boric acid |
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|---|---|---|---|
| CN2011104234067A CN102515191A (en) | 2011-12-16 | 2011-12-16 | Method for preparing boron trifluoride through reacting fluosulfonic acid with boric acid |
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Cited By (1)
| 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 |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US1898532A (en) * | 1928-06-22 | 1933-02-21 | Ig Farbenindustrie Ag | Process of preparing boron trifluoride |
| US2416133A (en) * | 1944-06-16 | 1947-02-18 | Gen Chemical Corp | Manufacture of boron trifluoride |
| CN101214970A (en) * | 2008-01-17 | 2008-07-09 | 核工业理化工程研究院华核新技术开发公司 | Technique and deice for preparing high purity boron trifluoride gas |
-
2011
- 2011-12-16 CN CN2011104234067A patent/CN102515191A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US1898532A (en) * | 1928-06-22 | 1933-02-21 | Ig Farbenindustrie Ag | Process of preparing boron trifluoride |
| US2416133A (en) * | 1944-06-16 | 1947-02-18 | Gen Chemical Corp | Manufacture of boron trifluoride |
| CN101214970A (en) * | 2008-01-17 | 2008-07-09 | 核工业理化工程研究院华核新技术开发公司 | Technique and deice for preparing high purity boron trifluoride gas |
Cited By (1)
| 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 |
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Application publication date: 20120627 |