CN105731481B - Method and equipment for purifying boron trichloride - Google Patents
Method and equipment for purifying boron trichloride Download PDFInfo
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- CN105731481B CN105731481B CN201410767703.7A CN201410767703A CN105731481B CN 105731481 B CN105731481 B CN 105731481B CN 201410767703 A CN201410767703 A CN 201410767703A CN 105731481 B CN105731481 B CN 105731481B
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Abstract
The invention discloses a purification method of boron trichloride, which comprises the steps of introducing a 3N boron trichloride raw material into a gas cylinder purification pipeline for gasification, sequentially passing the gasified boron trichloride gas through a decomposition tank for heating catalytic decomposition, a water cooler for cooling, an adsorption tank for adsorption and a rectification tower for rectification, removing low-boiling-point impurity gas with a boiling point close to that of boron trichloride, silicon-containing and other metal impurities, and finally filling at low temperature to finish the purification of 5N boron trichloride. The invention also provides a purification device. Compared with the prior art, the method can improve the purification purity of the boron trichloride, and is simple in process and convenient to operate.
Description
Technical field
The invention belongs to chemical industry manufacturing field, it is related to the purification of compound and proposing for preparation more particularly to a kind of boron chloride
Pure method and its equipment.
Background technology
Boron trioxide can be as cationic polymerization catalyst and the raw material of synthesis boron compound, also with can make semiconductor
Dopant or turbid quarter agent, it is but especially high to its purity requirement.
There are many methods of purification of boron chloride, such as absorption, distillation, air lift, but be all only limitted in the prior art how
The difficult phosgene removed in boron chloride is removed, such as US3037337, US3043665, US327581, US4204926, in these patents
Boron, silicon or other metals are selected as the catalyst to decomposing phosgene, but the removal without illustrating other impurity elements.United States Patent (USP)
US6238636 takes boron chloride out of using inert gas, decomposes phosgene, then after active carbon adsorption by heating of Activated carbon, profit
Some gaseous impurities are removed with the method for air lift, and part indifferent gas is finally had in high-purity boron chloride that this method obtains
Body is difficult to remove.
In summary, how to provide a kind of high-purity, impurity content is low or boron chloride free from foreign meter is ability
The technical issues of field technique personnel are urgently to be resolved hurrily.
Invention content
The embodiment of the invention discloses the methods of purification and its equipment of a kind of boron chloride, can improve carrying for boron chloride
Purity, meanwhile, flow is simple, easy to operate.
Boron chloride raw material is passed through gas cylinder purification pipeline by a kind of method of purification of boron chloride in the embodiment of the present invention
Boron trichloride gas after gasification is passed sequentially through and decomposes the decomposition of tank heatable catalytic, water cooler cooling, adsorption tanks suction by interior gasification
The contained low boiling impurity gas close with boron chloride boiling point and siliceous and other metal impurities are removed in attached, rectifying column rectifying
It removes, most completes boron chloride purification through cold-aseptic filling afterwards.
Preferably, include the following steps：
(1) gasify：Boron chloride raw material is passed through in gas cylinder purification pipeline, and heating equipment is set outside gas cylinder, is controlled
Gas pressure of the inside of a bottle ranging from 0.4-0.7Mpa, and keep saturation pressure in gas cylinder constant；
Because of the toxic and strong corrosive of boron chloride in itself, generally by boron chloride in steel gas cylinder, trichlorine
The boiling point for changing boron is relatively low, is 12.5 DEG C, therefore is usually gaseous state under its room temperature, but boron chloride is in steel gas cylinder under room temperature
Pressure is smaller；To promote its pressure, heating equipment outside gas cylinder is set, heating power, control are controlled according to high pressure end pressure
Gas pressure of the inside of a bottle simultaneously keeps saturation pressure in steel cylinder constant, while should avoid in stock bottle that pressure is excessive, leads to drop-in.
(2) heatable catalytic decomposes：Boron trichloride gas after the gasification of (1) step is passed through and is preheated to 200 DEG C of decomposition
In tank, with activated carbon catalyst, the phosgene in boron chloride is decomposed into chlorine and carbon monoxide；
Since the gaseous impurity phosgene in boron chloride is difficult to remove by absorption and rectifying, need first to carry out phosgene
Decomposition removes again, this decomposition tank is preheated to 200 DEG C or so, and using activated carbon as reaction by the present invention by heating furnace in advance
Catalyst accelerated decomposition is reacted, and chlorine and an oxygen are broken down by phosgene in the decomposition reaction boron chloride in decomposition reaction tank
Change carbon.
(3) it cools down：Gas after step (2) is reacted is cooled to room temperature, the ambient temperature ranging from 20- by water cooler
25℃；
Since phosgene decomposition reaction is a reversible reaction, phosgene is easily regenerated at high temperature, therefore boron chloride goes out to divide
It to be cooled down at once after solution tank, condensation water interlayer, i.e. water cooling are wrapped on the latter linked purification pipeline of tank is decomposed in the present invention
Device cools down the chlorine being decomposed to form and CO gas and boron trichloride gas that are come out from decomposition tank, makes trichlorine
The temperature for changing boron is cooled to 20-25 DEG C.
(4) it adsorbs：Gas after cooling is passed through the adsorption tanks equipped with adsorbent to adsorb, the gas after cooling
Enter from absorption pot bottom, go out at the top of adsorption tanks, the flow control 0.15-0.4m/s of gas, the adsorbent is activity
Carbon；
The boiling point of the chlorine being decomposed to form and some siliceous organic matters is not much different with boron chloride, should not use rectification method
It removes.Therefore for this step using adsorbent method, the mixed gas formed after decomposition enters absorption from absorption pot bottom
From the bottom up until being exported at the top of adsorption tanks, in order to enable adsorption effect is more preferable, gas flow rate is controlled in 0.15- for tank
0.4m/s sections, no the problems such as taking a shortcut it will cause gas, after absorption, most Cl2, siliceous and some metals it is miscellaneous
Matter is removed.
(5) rectifying：Rectifying column will be introduced after the boron trichloride gas after step (4) is by particulate filter and carries out essence
It evaporates, the rectifying column includes heating kettle, the first condenser and the second condenser, and the boron trichloride gas passes sequentially through heating
Kettle, the first condenser and the second condenser carry out rectifying, and the temperature in second condenser is less than in first condenser
Temperature；
Boron chloride after step (4) by particulate filter after enter in rectifying column.Rectifying column is equipped with heating
Different temperature is set separately in kettle and two condensers, two condensers, in order to reduce the damage of the boron chloride in distillation process
It loses, first condenser of ratio of second condenser temperature setting is low.Meanwhile discharged by the tail gas of second condenser,
Other low-boiling foreign gases are discharged purification pipeline.
(6) room temperature cooling processing will be carried out, and discharge through the boron chloride after step (5) rectifying, the room temperature cooling temperature
Ranging from 20-25 DEG C of degree.
Rectifying finishes, and is cooled to room temperature, while keeps more than the pressure 0.1Mpa in rectifying column heating kettle, can go out at this time
Material.It is placed at boron chloride discharging after the chilled room low-temperature treatment of steel cylinder will be received, receives and cooling is provided with outside steel cylinder sets
It applies, ensures that discharging receives steel cylinder and is in the state of cooling.Hose is connected, first discharging pipeline is evacuated, is ensured in pipeline without sky
Gas opens the valve of rectifying column heating kettle bottom discharge port and receives cylinder valve, by the purification in rectifying tower reactor after the completion of evacuating
In the indoor reception steel cylinder of product press-in freezing, so as to complete boron chloride rectifying and purifying technique.
Preferably, the pressure described in step (1) in gas cylinder is 0.5Mpa.
Preferably, adsorption tanks described in step (4) divide two layers, and the 1/5 of adsorption tanks height is accounted for for one layer above the adsorption tanks,
And removal chlorine activated carbon is housed, account for the 4/5 of adsorption tanks height for one layer below the adsorption tanks, the activity equipped with removal organosilicon
Charcoal.
Preferably, the temperature setting of first condenser is-20-- 40 DEG C, and the temperature of second condenser is set
It is set to-40-- 80 DEG C.
Invention additionally discloses a kind of equipment of the method for purification of boron chloride, the gas including being used to contain boron chloride raw material
Bottle, heating unit decompose tank, water cooler, adsorption tanks, rectifying column and receive steel cylinder, and the gas cylinder decomposes tank and the adsorption tanks
Outer wall be provided with the heating unit, the gas cylinder decomposes tank, water cooler, adsorption tanks, rectifying column and receives steel cylinder by carrying
Pure pipeline is sequentially connected.General heating furnace of choosing heats gas cylinder, decomposition tank and adsorption tanks as heating unit, the present invention
In in order to preferably be decomposed to the phosgene in boron chloride, by the boron chloride containing phosgene from decompose tank bottom draw
Entering, exported from top, the time reacted in this way is just more abundant, and discomposing effect is more preferable, and the reaction principle in adsorption tanks such as decomposes tank,
Boron chloride to be purified is imported from the bottom of absorber, is exported from top and is introduced rectifying column.
Preferably, the rectifying column includes heating kettle and condenser, and the condenser is cold including the first condenser and second
Condenser, the heating kettle, the first condenser and the second condenser pass sequentially through purification pipeline connection forming circuit.
Preferably, the condenser tail portion is also provided with reflux line, and the condenser is by the reflux line by trichlorine
Change boron to pass back into rectifying column heating kettle.
Preferably, evacuation pipeline is further included, the evacuation pipeline is connect with the purification pipeline, is filled in the evacuation pipeline
Full inert gas, the inert gas are nitrogen.
Preferably, several control valves are provided on the evacuation pipeline and the purification pipeline.
As can be seen from the above technical solutions, the embodiment of the present invention has the following advantages：
The present invention gives boron chloride supercharging using gas cylinder is heated by the way of, using the vapour pressure of boron chloride itself, simultaneously
Using the mode for cooling down gas cylinder, pressure differential is formed so as to discharge, avoids passing through and introduces impurity using the mode of mechanical pump, also avoid
The problem of inert gas impurity content is excessive in the product after purification is caused to generate using inert gas supercharging discharging.Meanwhile it adopts
The larger gaseous impurity of some boiling points difference can be removed with the rectificating method in the present invention, realizes the boron chloride production after purification
Product purity is higher, has not only removed a large amount of impurity that boron chloride raw material contains in itself, but also secondary will not bring inert gas, Neng Gouti into
For a kind of boron trichloride gas of high-purity.
Description of the drawings
Fig. 1 is the purifying technique flow chart of boron chloride in the embodiment of the present invention.
Specific embodiment
The embodiment of the invention discloses a kind of methods of purification of boron chloride, implement referring specifically to Fig. 1, Fig. 1 for the present invention
The purifying technique flow chart of boron chloride in example, in the embodiment of the present invention, in order to be purified to 3N boron chloride raw materials, will put
The gas cylinder 1 of boron chloride raw material is put, tank 2, water cooler 3, adsorption tanks 4, rectifying column 6 is decomposed and receives steel cylinder 10 by purifying pipeline
11 are sequentially connected, and form the purifying technique pipeline of a closing, boron chloride raw material is passed through gas cylinder 1 and is purified in pipeline 11 pass through
Boron trichloride gas after gasification is passed sequentially through and decomposes the decomposition of 2 heatable catalytic of tank by heating supercharging gasification, water cooler 3 cools down, inhales
Attached tank 4 adsorbs, 6 rectifying of rectifying column, and contained low boiling impurity gas and siliceous and other metal impurities are removed, are finally cooled to
Room temperature is filling, completes boron chloride purifying technique.Rectifying column 6 includes heating kettle 7 and condenser in the present embodiment, and condenser includes
First condenser 8 and the second condenser 9, heating kettle 7, the first condenser 8 and the second condenser 9 pass sequentially through purification pipeline 11 and connect
Forming circuit is connect, condenser tail portion is also provided with reflux line, and boron chloride is passed back into rectifying column 6 by condenser by reflux line
In heating kettle 7, boron chloride is cooled to room temperature after rectifying, and discharge, by previous process, purer 5N trichlorines can be obtained
Change boron.
It is described in more detail below by specific embodiment.
(1), pre-preparation step：System installation connection used by purifying technique is finished and evacuated first, takes off light
Air column decomposes tank 2 and is preheating to 200 DEG C, and the water cooler 3 of chuck is packed into cooling circulating water, and the recirculated water is from the bottom of water cooler 3
Into top outflow sets first condenser temperature as -20 DEG C, and second condenser temperature is -50 DEG C.Two condensers
Logical cryogen 1 hour or more, ensures that condenser temperature reaches set temperature.
(2), the gas cylinder 1 equipped with raw material with system pipeline is connected, close raw material gas cylinder 1 and decomposes the purification between tank 2
Valve V on pipeline 11113, open the valve V of evacuation pipeline being connect with raw material gas cylinder 1214 are evacuated.
(3), valve V is closed after the completion of evacuating214, open 1 switch valve of raw material gas cylinder, observation switch valve side pressure reducing valve high pressure
End pressure adjusts flow to 1Nm3/ h, initial experiment flow is from 0.3Nm3/ h starts.
(4), the heating furnace 5 heated to the gas cylinder 1 equipped with raw material is opened, gas cylinder 1 is heated and carried by heating furnace 5
Pressure of the inside of a bottle is risen, according to high pressure end pressure control heating power, control pressure is kept in 0.5Mpa or so in raw material gas cylinder 1
Saturation pressure is constant.
(5), boron trichloride gas being passed sequentially through de- phosgene column (decomposing tank 2) to decompose, water cooler 3 cools down,
Absorber 4 carries out adsorption-edulcoration.
(6), the valve V on purification pipeline 11 between adsorption tanks 4 and rectifying column 6 is opened415, after the absorption of adsorption tanks 4
Boron chloride superheated steam enter rectifying column 6.Heating kettle 7 in rectifying column 6 is opened, control pressure does not surpass in 0.2Mpa, temperature
Cross 40 DEG C.
(7), the valve V on the purification pipeline 11 between 6 and first condenser 8 of rectifying column is opened818, steam gas entrance
First condenser 8.After pressure reaches 0.1Mpa in the first condenser 8, open 8 top of the first condenser and the second condenser 9 it
Between purification pipeline 11 on valve V1019, and open 8 top vent pressure reducing valve V of the first condenser1523、V1624 go to absorb emptying,
Flow is set as 0.1Nm3Then/h opens the valve V evacuated on pipeline 12 that 9 top of the second condenser is set1120、V1725,
And it is then emptied by tail gas absorber under normal pressure.
(8), after 3N boron trichloride gas discharges, the valve V between adsorption tanks 5 and rectifying column 6 is closed415, to tri-chlorination
Boron carries out rectifying.
(9), rectifying finishes, and is cooled to room temperature, and the range of room temperature chooses 20-25 DEG C, while keep pressure value in heating kettle 7
In more than 0.1Mpa, can discharge at this time.Discharge port is placed on after receiving 10 chilled room low-temperature treatment of steel cylinder, connects hose, is closed
It closes heating kettle 7 in rectifying column 6 and receives the valve V purified on pipeline 11 between steel cylinder 10616th, 9 bottom of the second condenser with
Heating kettle 7 and the triangle joint received between steel cylinder 10 purify the valve V on pipeline 111221st, receive steel cylinder 10 and heating kettle 7 it
Between purification pipeline 11 on valve V717, open the V evacuated on pipeline 12 being connect with receiving steel cylinder 101322, to valve
V717 are evacuated to the purification pipeline 11 received between steel cylinder 10.V is opened after the completion of evacuating616th, heating kettle 7 is with receiving steel cylinder
The valve V on purification pipeline 11 between 10717 with reception cylinder valve, the boron chloride production after being purified in 6 tower reactor of rectifying column
In the indoor reception steel cylinder 10 of product press-in freezing.
After above-mentioned purifying technique, every impurity content in boron chloride is significantly lower than the standard in industry, such as
Shown in following table table 1：
Table 1
The method of purification and its equipment of a kind of boron chloride provided by the present invention are described in detail above, for
The thought of those of ordinary skill in the art, according to the present invention embodiment, has in specific embodiments and applications
Change part, in conclusion the content of the present specification should not be construed as limiting the invention.
Claims (9)
1. a kind of method of purification of boron chloride, which is characterized in that 3N boron chloride raw materials are passed through gas in gas cylinder purification pipeline
Change, the boron trichloride gas after gasification is passed sequentially through and decomposes the decomposition of tank heatable catalytic, water cooler cooling, adsorption tanks absorption, essence
Tower rectifying is evaporated, contained low boiling impurity gas and siliceous and other metal impurities are removed, most completes 5N tri- through cold-aseptic filling afterwards
The purification of boron chloride；Include the following steps：
(1) gasify：Boron chloride raw material is passed through in gas cylinder purification pipeline, and heating equipment is set outside gas cylinder, controls gas cylinder
Interior pressure ranging from 0.4-0.7MPa, and keep saturation pressure in gas cylinder constant；
(2) heatable catalytic decomposes：Boron trichloride gas after the gasification of (1) step is passed through and is preheated to 200 DEG C of decomposition reaction
In tank, with activated carbon catalyst, the phosgene in boron chloride is decomposed into chlorine and carbon monoxide；
(3) it cools down：Gas after step (2) is reacted is cooled to room temperature, the ambient temperature ranging from 20-25 by water cooler
℃；
(4) it adsorbs：Gas after cooling is passed through the adsorption tanks equipped with adsorbent to adsorb, the gas after cooling is from suction
Attached pot bottom enters, goes out at the top of adsorption tanks, and for the flow control of gas in 0.15-0.4m/s, the adsorbent is activated carbon；
(5) rectifying：Rectifying column will be introduced after the boron trichloride gas after step (4) is by particulate filter and carries out rectifying, institute
It states rectifying column and includes heating kettle, the first condenser and the second condenser, the boron trichloride gas passes sequentially through heating kettle, first
Condenser and the second condenser carry out rectifying, and the temperature in second condenser is less than the temperature in first condenser；
(6) room temperature cooling processing will be carried out, and discharge through the boron chloride after step (5) rectifying, the room temperature cooling temperature model
Enclose is 20-25 DEG C.
2. a kind of method of purification of boron chloride as described in claim 1, which is characterized in that described in step (1) in gas cylinder
Pressure be 0.5Mpa.
A kind of 3. method of purification of boron chloride as claimed in claim 2, which is characterized in that adsorption tanks described in step (4)
Divide two layers, the 1/5 of adsorption tanks height is accounted for for one layer above the adsorption tanks, and removal chlorine activated carbon is housed, under the adsorption tanks
One layer of face accounts for the 4/5 of adsorption tanks height, the activated carbon equipped with removal organosilicon.
A kind of 4. method of purification of boron chloride as claimed in claim 2, which is characterized in that the temperature of first condenser
- 20-- 40 DEG C are set as, the temperature of second condenser is set as-40-- 80 DEG C.
5. a kind of equipment of such as method of purification of Claims 1-4 any one of them boron chloride, trichlorine is contained including being used for
Gas cylinder, heating unit, decomposition reaction tank, water cooler, adsorption tanks, rectifying column and reception steel cylinder, the gas cylinder for changing boron raw material divide
The outer wall of solution retort and the adsorption tanks is provided with the heating unit, the gas cylinder, decomposition reaction tank, water cooler, absorption
Tank, rectifying column and reception steel cylinder are sequentially connected by purifying pipeline.
6. the equipment of the method for purification of boron chloride as claimed in claim 5, which is characterized in that the rectifying column includes heating
Kettle and condenser, the condenser include the first condenser and the second condenser, and the heating kettle, the first condenser and second are cold
Condenser passes sequentially through purification pipeline connection forming circuit.
7. the equipment of the method for purification of boron chloride as claimed in claim 6, which is characterized in that also open the condenser tail portion
There is reflux line, the condenser is passed back into boron chloride in rectifying column heating kettle by reflux line.
8. the equipment of the method for purification of boron chloride as claimed in claim 5, which is characterized in that further include evacuation pipeline, institute
It states evacuation pipeline to connect with the purification pipeline, full of inert gas in the evacuation pipeline, the inert gas is nitrogen.
9. the equipment of the method for purification of boron chloride as claimed in claim 8, which is characterized in that the evacuation pipeline and described
Several control valves are provided on purification pipeline.
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| CN201410767703.7A CN105731481B (en) | 2014-12-12 | 2014-12-12 | Method and equipment for purifying boron trichloride |
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| CN201410767703.7A CN105731481B (en) | 2014-12-12 | 2014-12-12 | Method and equipment for purifying boron trichloride |
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106957061B (en) * | 2017-05-25 | 2023-06-16 | 江西瑞合特种材料有限公司 | Boron trichloride production device and method with low phosgene content |
| CN108163868A (en) * | 2017-12-29 | 2018-06-15 | 和立气体（上海）有限公司 | A kind of boron chloride purification devices |
| CN108408734A (en) * | 2018-05-22 | 2018-08-17 | 福建久策气体集团有限公司 | A kind of high-purity boron chloride preparation method and device |
| CN108821302A (en) * | 2018-09-05 | 2018-11-16 | 欧中电子材料（重庆）有限公司 | A kind of purification process and device of boron chloride |
| CN110117015A (en) * | 2019-05-16 | 2019-08-13 | 大连科利德光电子材料有限公司 | The purification devices and method of boron chloride |
| CN113125372A (en) * | 2021-04-21 | 2021-07-16 | 中国科学院合肥物质科学研究院 | Impurity gas detection device and method for electronic-grade boron trichloride purification system |
| CN113582192A (en) * | 2021-07-22 | 2021-11-02 | 重庆同辉气体有限公司 | Boron trichloride purification device |
| CN115724437A (en) * | 2022-12-14 | 2023-03-03 | 陕西天鼎工程技术有限公司 | Purification method of boron trichloride |
| CN117486226B (en) * | 2023-11-01 | 2024-04-19 | 滁州昶旭电子材料有限公司 | Purification process and purification system of high-purity boron trichloride |
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| US6790419B1 (en) * | 1999-06-11 | 2004-09-14 | Honeywell Intellectual Properties Inc. | Purification of gaseous inorganic halide |
| CN104098105A (en) * | 2014-07-25 | 2014-10-15 | 大连保税区科利德化工科技开发有限公司 | Purification method for boron trichloride |
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| JPH10265216A (en) * | 1997-03-25 | 1998-10-06 | Nissan Chem Ind Ltd | Purification of boron trichloride |
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| US6790419B1 (en) * | 1999-06-11 | 2004-09-14 | Honeywell Intellectual Properties Inc. | Purification of gaseous inorganic halide |
| CN104098105A (en) * | 2014-07-25 | 2014-10-15 | 大连保税区科利德化工科技开发有限公司 | Purification method for boron trichloride |
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| Title |
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