CN101508443B - Method for producing boron triflouride gas - Google Patents
Method for producing boron triflouride gas Download PDFInfo
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- CN101508443B CN101508443B CN2009100683110A CN200910068311A CN101508443B CN 101508443 B CN101508443 B CN 101508443B CN 2009100683110 A CN2009100683110 A CN 2009100683110A CN 200910068311 A CN200910068311 A CN 200910068311A CN 101508443 B CN101508443 B CN 101508443B
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Abstract
The invention discloses a method for preparing boron trifluoride gas, which comprises the following steps: firstly, liquefying raw material fluorine gas, and removing high-boiling point foreign gas which can not be condensed in the fluorine gas; secondly, performing synthesis reaction on the fluorine gas and boron anhydrous to generate a coarse product-boron trifluoride gas; and thirdly, liquefying the coarse product, removing foreign gas in the coarse product, and obtaining a product-pure boron trifluoride gas, wherein the liquefying temperature for liquefying the raw material fluorine gas and the coarse product-the boron trifluoride gas is between 140 DEG C below zero and 195 DEG C below zero, and the pressure of a buffer tank is controlled to be between -0.04 and -0.01 MPa; and a reactor adopts a vertical reactor of which the lower part is provided with a sieve plate, and the fluorine gas is introduced from the lower part of the sieve plate. The method has simple equipment, convenient operation, and safe operation of equipment, and the purity of the products can reach 99.9 percent.
Description
Technical field
The invention belongs to a kind of preparation boron trifluoride (BF
3) method of gas, being specifically related to a kind of is the method for feedstock production boron triflouride gas with fluorine gas and boron trioxide.
Background technology
In electronic industry, boron triflouride gas mainly is used as the P type doping agent of silicon and germanium extension, diffusion and ion implantation process; In the organic chemical industry, boron triflouride gas mainly as an acidic catalyst of esterification, alkylation, polymerization, isomerization, sulfonation, nitration reaction, also is used to prepare borides such as halogenation boron, element boron, borine and sodium borohydride; Boron trifluoride also is used for nuclear technique and photoconductive fiber; Boron trifluoride and compound thereof are used as solidifying agent in Resins, epoxy; Boron trifluoride can prevent that magnesium and alloy thereof from oxygenizement taking place when fusion is cast, as solder flux, also can make the component of steel or other metallic surface boronation treatment agents when welding magnesium material, also is used as the lubricant of cast steel.
At present, the method for preparing boron triflouride gas has multiple, and the method for preparing boron triflouride gas commonly used has fluoroborate method, fluorite boric anhydride method, fluorite borax method etc.
The main raw material that the fluoroborate method adopts is fluoroborate, boric anhydride and the vitriol oil.Fluoroborate with after boric anhydride mixes by a certain percentage, is joined in the reactor, under agitation add the vitriol oil, have boron triflouride gas to produce behind the heating certain hour, its reaction formula is:
B
2O
3+6KBF
4+6H
2SO
4→8BF
3+6KHSO
4+H
2O，
The main raw material that fluorite boric anhydride method adopts is Calcium Fluoride (Fluorspan) (fluorite), boric anhydride and the vitriol oil.Calcium Fluoride (Fluorspan) with after boric anhydride mixes by a certain percentage, is joined in the reactor, under agitation add the vitriol oil, have boron triflouride gas to produce behind the heating certain hour, its reaction formula is:
B
2O
3+3CaF
2+3H
2SO
4→2BF
3+3CaSO
4+3H
2O
It is the raw material production boron triflouride gas that the fluorite borax method adopts Calcium Fluoride (Fluorspan) (fluorite), borax and the vitriol oil, and its reaction formula is:
Na
2B
4O
7+6CaF
2+7H
2SO
4→4BF
3+6CaSO
4+Na
2SO
4+7H
2O
The shortcoming of aforesaid method is a foreign matter content height in the boron triflouride gas, and purity is low, and residual in reactor have a solid residue that is difficult to remove, and the sulfuric acid consumption is big, and is serious to equipment corrosion.
Summary of the invention
The present invention is for the shortcoming that overcomes prior art and exist proposes, its objective is provide that a kind of equipment is simple, easy to operate, equipment operating safety, the method for preparing boron triflouride gas that product purity is high.
Technical scheme of the present invention is: a kind of method for preparing boron triflouride gas may further comprise the steps:
(i) remove foreign gas in the fluorine gas
Freezing with carrying out in the feeding of the fluorine gas in the fluorine gas storage tank 1 purifier, make the fluorine gas liquefaction that contains foreign gas,, incondensible high-boiling-point impurity gas in the purifier is found time with the vacuum unit according to the boiling point difference, heating up then makes the liquid fluorine gasification, obtains highly purified fluorine gas;
(ii) fluorine gas and boric anhydride carry out building-up reactions
At first with the boric anhydride (B in the reactor
2O
3) preheating, in reactor, feed the fluorine gas of removing foreign gas then and contact building-up reactions with boric anhydride, generate the thick product of boron triflouride gas that contains foreign gas, temperature of reaction is 100～160 ℃, the pressure in the reactor is-0.01～0.03Mpa;
(iii) remove the foreign gas in the boron triflouride gas
The thick product of the boron triflouride gas that contains foreign gas that will in reactor, generate feed carry carry out in the freezing trap freezing, make the boron triflouride gas liquefaction that contains foreign gas, according to the boiling point difference, with the vacuum unit incondensible high-boiling-point impurity gas in the freezing trap is found time, heating up then makes the gasification of liquid boron trifluoride, obtains highly purified boron triflouride gas.
The liquefaction temperature that contains the fluorine gas liquefaction of foreign gas and contain the thick product of boron triflouride gas of foreign gas is between-140～-195 ℃.
The pressure-controlling of surge tank-0.04～-0.01Mpa between.
Reactor adopts vertical, is provided with sieve plate with holes in the bottom of reactor, is layered on equably on the sieve plate after boric anhydride is pulverized, and fluorine gas feeds from the bottom of sieve plate.
Present device is simple, easy to operate, the equipment operating safety, and product purity can reach 99.9%.
Description of drawings
Fig. 1 is the process flow sheet for preparing the method for boron triflouride gas of the present invention.
Wherein:
1 storage tank, 2 valves
3 purifiers, 4 surge tanks
5 reactors, 6 freezing traps
7 vacuum units, 8 sieve plates
Embodiment
Below, in conjunction with the accompanying drawings and embodiments the method for preparing boron triflouride gas of the present invention is elaborated:
As shown in Figure 1, a kind of method for preparing boron triflouride gas, wherein employed equipment comprises fluorine gas storage tank 1, fluorine gas storage tank 1 is communicated with fluorine gas purifier 3 by pipeline, fluorine gas purifier 3 is communicated with fluorine gas surge tank 4 by pipeline, fluorine gas surge tank 4 is communicated with reactor 5 by pipeline, reactor 5 adopts vertical, be provided with sieve plate with holes 8 in the bottom of reactor 5, reactor 5 is communicated with freezing trap 7 by pipeline, and fluorine gas purifier 3, fluorine gas surge tank 4, reactor 5 are communicated with vacuum unit 7 by pipeline respectively.
A plurality of sealed valves 2 are set on pipeline.
The method for preparing boron triflouride gas of the present invention may further comprise the steps:
(i) remove foreign gas in the fluorine gas
At first, to carry out cryogenic liquefaction in the feeding of the fluorine gas in the fluorine gas storage tank 1 purifier 3, the liquid nitrogen cold trap that utilizes purifier 3 outsides with the temperature maintenance of purifier 3 between-140～-195 ℃, this moment, fluorine gas was liquefied, when the volume of liquid reaches volumetrical 2/3rds height in the purifier 3, stop for fluorine gas.Start vacuum unit 7, Open valve, incondensible foreign gases such as high boiling point materials such as hydrogen, oxygen and nitrogen in the purifier 3 are found time, be evacuated to pressure in the purifier 3 always between-0.09～0.2Mpa.
Make liquid fluorine gasization by the temperature that improves purifier 3 again, so just can remove foreign gas in the fluorine gas, obtain fluorine gas purity more than 99%.
Detailed process is: when the liquid fluorine liquid level in the purifier 3 reaches 1/2nd height of purifier 3, close purifier 3 early gates, and stop at adding liquid nitrogen in the liquid nitrogen cold trap, and liquid nitrogen cold trap is withdrawn from purifier 3.Then purifier 3 is heated up naturally, liquid fluorine begins gasification, and after the pressure in the purifier 3 began to raise, the valve before the unlatching surge tank 4 was put into surge tank 4 with the fluorine gas in the purifier 3.The pressure of surge tank 4 generally is controlled at-0.04～0Mpa, and pressure is higher than 0Mpa has relatively high expectations to surge tank and valve, wayward; Pressure is lower than-and 0.04Mpa is unfavorable for the synthetic of boron triflouride gas in the reactor 5.When the pressure of surge tank 4 is higher than 0Mpa, close the valve before the surge tank 4, purifier 3 is cooled off once more.Generally speaking, purifier 3 once cools off the amount of fluorine gas and the amount of 4 splendid attire fluorine gas of surge tank should match each other.
(ii) fluorine gas and boric anhydride carry out building-up reactions
Fluorine gas and boric anhydride (B
2O
3) in reactor 5, contacting the generation building-up reactions, this reaction is thermopositive reaction, obtains containing the thick product of boron triflouride gas of foreign gas after the reaction, reaction equation is:
2B
2O
3+6F
2→4BF
3+3O
2
The structure of reactor 5 needs enough surfaces allows boric anhydride contact with fluorine gas, makes fluorine gas and boric anhydride complete reaction.For this reason, reactor 5 adopts vertical, is provided with sieve plate with holes 8 in the bottom of reactor 5, is layered on equably on the sieve plate 8 after boric anhydride is pulverized, and fluorine gas feeds from the bottom of sieve plate 8, and fluorine gas can fully be contacted with boric anhydride, and reaction is intermittently carried out.Can electricity consumption in reactor 5 bottoms, mode such as water-bath carries out preheating to the boric anhydride in the reactor 5.
Detailed process is: add an amount of boric anhydride in reactor 5, the sealing leak hunting qualified after, reactor is preheating to about 80 ℃, stop the heating, reactor is evacuated to-0.1Mpa, valve before the slow unlatching reactor 5, certain because of reactor volume, the amount that at every turn charges into fluorine gas is controlled according to reactor pressure, generally be controlled at-0.01～0.03Mpa, off-response device early gate after pressure reaches, at this moment the pressure of reactor can descend gradually, and temperature can raise gradually.When reactor pressure no longer changes, think that fluorine gas reacts completely, need the gas in the reactor is put into freezing trap.Productive rate was better when reactor temperature range was controlled at 100～160 ℃.After charging into fluorine gas, when reactor pressure and temperature no longer change, think that boric anhydride reacts completely, can finish reaction.
Generally speaking, the amount that at every turn adds boric anhydride should be complementary in proportion with the fluorine gas of each purification.Because exothermic heat of reaction, reactor can only pass through naturally cooling, comes the controlling reactor temperature so need to control the amount and the reacting space that feed fluorine gas in reaction process.
(iii) remove the foreign gas in the boron triflouride gas
Identical with the purification process of above-mentioned fluorine gas, at first liquid nitrogen cold trap on freezing trap 6 outer cover is kept the liquid nitrogen liquid level and is reached freezing trap 2/3rds height, and the temperature maintenance that makes freezing trap 6 is after-140～-195 ℃, open the valve before the freezing capture 6, make boron trifluoride (BF
3) the thick product of gas enters freezing trap 6 from reactor 5, when the pressure in the reactor 5 no longer changes, thinks that freezing capture process finishes.By dosing temperature maintenance that liquid nitrogen keeps freezing trap 6 between-140～-195 ℃, make boron triflouride gas liquefaction.After treating boron triflouride gas liquefaction, close the valve before the freezing capture 6, start vacuum unit 7, open the valve before freezing capture 6 upper valve and the vacuum unit 7, incondensible foreign gases in the purifier 3 such as high boiling point materials such as hydrogen, oxygen and nitrogen are found time, keep make freezing trap pressure maintain-0.09～0.2Mpa between.The time visual response of cryogenic liquefaction carries out process and decides.
Then, stop at adding liquid nitrogen in the liquid nitrogen cold trap, and liquid nitrogen cold trap is withdrawn from freezing trap, freezing trap is heated up naturally, boron trifluoride liquid begins gasification.After the pressure of freezing trap begins to raise, open cylinder valve, boron triflouride gas is filled into steel cylinder.The purity of boron triflouride gas can reach more than 99.9%.
With the reactor cleaning, drying, in reactor, add 2 kilograms of analytically pure boric anhydrides, reactor is found time to be preheated to behind the leak test 80 ℃ and be evacuated to once more-0.1Mpa.Arrive-188 ℃ with liquid nitrogen freezing fluorine gas purifier, open the preceding valve of purifier, fluorine gas in the fluorine gas storage tank enters the fluorine gas purifier and liquefies, liquefying time is about 2 hours, after liquefaction is finished, close the preceding valve of fluorine gas purifier, use the vacuum unit to find time to remove most of hydrogen, high boiling point such as oxygen and nitrogen material, the pressure of purifier is-during 0.09Mpa, stop to use liquid nitrogen, the fluorine gas purifier is heated up naturally, liquid fluorine begins gasification, fluorine gas with gasification enters the fluorine gas surge tank by pipeline gradually, and the pressure for the treatment of the fluorine gas surge tank is during for-0.04Mpa, and the purifier temperature stops when reaching-160 ℃ heating up.At this moment, open the preceding valve of reactor, fluorine gas enters reactor by pipeline and boric anhydride carries out building-up reactions, generates the thick product of boron triflouride gas that contains foreign gas.Temperature of reactor is controlled at 100 ℃, and the pressure that at every turn charges into fluorine gas is the valve before the off-response device behind the 0.01Mpa, and each reaction times is about 30 seconds, and reaction finishes post-reactor pressure and no longer descends.
Open the preceding valve of freezing trap, the thick product of boron triflouride gas enters freezing trap and liquefies, the temperature of freezing trap is-140 ℃, after liquefaction is finished, close the valve before the freezing capture 6, start vacuum unit 7, open the valve before freezing capture 6 upper valve and the vacuum unit 7, incondensible foreign gas such as high boiling point materials such as hydrogen, oxygen and nitrogen in the purifier 3 are found time, keep that freezing trap pressure is maintained-0.09Mpa.
Slowly promote the temperature of freezing trap by thawing naturally then, purified boron trifluoride liquid begins gasification, and boron triflouride gas is filled in the steel cylinder.Through 3 hours reaction, can obtain 3.5 kilograms of boron triflouride gas altogether, purity reaches 99.9%.All are by the foreign gas that the vacuum unit is found time, enter flare system handle up to standard after discharging again.
With the reactor cleaning, drying, in reactor, add 2 kilograms of analytically pure boric anhydrides, reactor is found time to be preheated to behind the leak test 80 ℃ and be evacuated to once more-0.1Mpa.Arrive-192 ℃ with liquid nitrogen freezing fluorine gas purifier, open the preceding valve of purifier, fluorine gas in the fluorine gas storage tank enters the fluorine gas purifier and liquefies, liquefying time is about 1.5 hours, after liquefaction is finished, close the preceding valve of fluorine gas purifier, use the vacuum unit to find time to remove high boiling point materials such as most of hydrogen, oxygen and nitrogen.
Stop to use liquid nitrogen then, the fluorine gas purifier is heated up naturally, liquid fluorine begins gasification, and the fluorine gas with gasification enters the fluorine gas surge tank by pipeline gradually, and the pressure for the treatment of the fluorine gas surge tank is during for-0.025Mpa, and the purifier temperature stops when reaching-150 ℃ heating up.At this moment, open the preceding valve of reactor, fluorine gas enters reactor by pipeline and boric anhydride carries out building-up reactions, generates the thick product of boron triflouride gas that contains foreign gas.Temperature of reactor is controlled at 130 ℃, and the pressure that at every turn charges into fluorine gas is the valve before the off-response device behind the 0.02Mpa, and each reaction times is about 20 seconds, and reaction finishes post-reactor pressure and no longer descends.
Open the preceding valve of freezing trap, the thick product of boron triflouride gas enters freezing trap and liquefies, and the temperature of freezing trap is-160 ℃.After liquefaction is finished, close the valve before the freezing capture 6, start vacuum unit 7, open the valve before freezing capture 6 upper valve and the vacuum unit 7, incondensible foreign gas such as high boiling point materials such as hydrogen, oxygen and nitrogen in the purifier 3 are found time, keep that freezing trap pressure is maintained-0.14Mpa.
Slowly promote the temperature of freezing trap by thawing naturally then, purified boron trifluoride liquid begins gasification, and boron triflouride gas is filled in the steel cylinder.Through 2.5 hours reaction, can obtain 3.45 kilograms of boron triflouride gas altogether, purity reaches 99.9%.All are by the foreign gas that the vacuum unit is found time, enter flare system handle up to standard after discharging again.
Embodiment 3
With the reactor cleaning, drying, in reactor, add 2 kilograms of analytically pure boric anhydrides, reactor is found time to be preheated to behind the leak test 80 ℃ and be evacuated to once more-0.1Mpa.Arrive-195 ℃ with liquid nitrogen freezing fluorine gas purifier, open the preceding valve of purifier, fluorine gas in the fluorine gas storage tank enters the fluorine gas purifier and liquefies, liquefying time is about 1 hour, after liquefaction is finished, close the preceding valve of fluorine gas purifier, use the vacuum unit to find time to remove high boiling point materials such as most of hydrogen, oxygen and nitrogen.Stop to use liquid nitrogen, the fluorine gas purifier is heated up naturally, liquid fluorine begins gasification, and the fluorine gas with gasification enters the fluorine gas surge tank by pipeline gradually, and the pressure for the treatment of the fluorine gas surge tank is during for-0.01Mpa, and the purifier temperature stops when reaching-160 ℃ heating up.
At this moment, open the preceding valve of reactor, fluorine gas enters reactor by pipeline and boric anhydride carries out building-up reactions, generates the thick product of boron triflouride gas that contains foreign gas.Temperature of reactor is controlled at 160 ℃, and the pressure that at every turn charges into fluorine gas is the valve before the off-response device behind the 0.03Mpa, and each reaction times is about 10 seconds, and reaction finishes post-reactor pressure and no longer descends.Open the preceding valve of freezing trap, the thick product of boron triflouride gas enters freezing trap and liquefies, and the temperature of freezing trap is-195 ℃.After liquefaction is finished, close the valve before the freezing capture 6, start vacuum unit 7, open the valve before freezing capture 6 upper valve and the vacuum unit 7, incondensible foreign gas such as high boiling point materials such as hydrogen, oxygen and nitrogen in the purifier 3 are found time, keep that freezing trap pressure is maintained-0.02Mpa.
Slowly promote the temperature of freezing trap by thawing naturally then, purified boron trifluoride liquid begins gasification, and boron triflouride gas is filled in the steel cylinder.Through 2 hours reaction, can obtain 3.4 kilograms of boron triflouride gas altogether, purity reaches 99.9%.All are by the foreign gas that the vacuum unit is found time, enter flare system handle up to standard after discharging again.
Present device is simple, easy to operate, the equipment operating safety, and product purity can reach 99.9%.
Claims (4)
1. a method for preparing boron triflouride gas is characterized in that: may further comprise the steps
(i) remove foreign gas in the fluorine gas
Freezing with carrying out in the feeding purifier of the fluorine gas in the fluorine gas storage tank (1) (3), make the fluorine gas liquefaction that contains foreign gas, according to the boiling point difference, with vacuum unit (7) incondensible high-boiling-point impurity gas in the purifier (3) is found time, heat up then and make the liquid fluorine gasification, obtain highly purified fluorine gas, highly purified fluorine gas feeds surge tank (4);
(ii) fluorine gas and boric anhydride carry out building-up reactions
At first with the boric anhydride (B in the reactor (5)
2O
3) preheating, in reactor (5), feed the fluorine gas of removing foreign gas then and contact building-up reactions with boric anhydride, generation contains the thick product of boron triflouride gas of foreign gas, and temperature of reaction is 100～160 ℃, and the pressure in the reactor (5) is-0.01～0.03MPa;
(iii) remove the foreign gas in the thick product of boron triflouride gas
Carry out freezing in the thick product feeding freezing trap of the boron triflouride gas that contains foreign gas that will in reactor (5), generate (6), make the boron triflouride gas liquefaction that contains foreign gas, according to the boiling point difference, with vacuum unit (7) incondensible high-boiling-point impurity gas in the freezing trap (6) is found time, heating up then makes the gasification of liquid boron trifluoride, obtains highly purified boron triflouride gas product.
2. the method for preparing boron triflouride gas according to claim 1 is characterized in that: the liquefaction temperature that contains the fluorine gas liquefaction of foreign gas and contain the thick product of boron triflouride gas of foreign gas is between-140～-195 ℃.
3. the method for preparing boron triflouride gas according to claim 1 is characterized in that: surge tank (4) is communicated with purifier (3) and reactor (5) respectively by pipeline, the pressure-controlling of surge tank (4)-0.04～-0.01MPa between.
4. the method for preparing boron triflouride gas according to claim 1, it is characterized in that: reactor (5) adopts vertical, be provided with sieve plate with holes (8) in the bottom of reactor (5), be layered on equably on the sieve plate (8) after boric anhydride is pulverized, fluorine gas feeds from the bottom of sieve plate (8).
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| CN101993088A (en) * | 2010-10-15 | 2011-03-30 | 天津市泰源工业气体有限公司 | Technology of method for preparing high-purity boron trifluoride by rectification and adsorption combined purification mode |
| CN102432030A (en) * | 2011-12-16 | 2012-05-02 | 天津市泰亨气体有限公司 | Method for preparing boron trifluoride |
| CN113968877A (en) * | 2021-10-29 | 2022-01-25 | 湖南法恩莱特新能源科技有限公司 | Preparation method of lithium difluoroborate |
| CN114560473A (en) * | 2021-12-23 | 2022-05-31 | 西安近代化学研究所 | Preparation method of boron trifluoride and boron trifluoride mixed gas |
| CN114570294B (en) * | 2022-04-21 | 2023-10-13 | 金宏气体股份有限公司 | Boron trifluoride continuous production device and method based on ebullated bed reactor |
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