CN103506056A - Sieve plate-free fluidized bed and preparation method of boron trichloride - Google Patents
Sieve plate-free fluidized bed and preparation method of boron trichloride Download PDFInfo
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- CN103506056A CN103506056A CN201210217421.0A CN201210217421A CN103506056A CN 103506056 A CN103506056 A CN 103506056A CN 201210217421 A CN201210217421 A CN 201210217421A CN 103506056 A CN103506056 A CN 103506056A
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
- B01J8/1818—Feeding of the fluidising gas
- B01J8/1827—Feeding of the fluidising gas the fluidising gas being a reactant
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
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Abstract
The invention provides a sieve plate-free fluidized bed and a preparation method of boron trichloride. The preparation method of the boron trichloride comprises the following steps: filling a powder raw material, namely alkaline earth metal boride into a bed body of a sieve plate-free fluidized bed through a raw material supply device; starting a carrier gas source, and introducing the carrier gas into the bed body of the sieve-plate-free fluidized bed to ensure that the powder raw material alkaline earth metal boride is in a fluidized state in the bed body of the sieve-plate-free fluidized bed; opening a heating device to heat the bed body, and introducing anhydrous hydrogen chloride serving as a reaction gas after the temperature reaches a specified temperature; and after the reaction reaches a specified period of time, opening and starting the separation device to obtain the required boron trichloride. The fluidized bed without the sieve plate is adopted, and the reaction can be carried out at a lower temperature, so that the energy consumption is reduced; the problem of screen plate hole blockage does not exist in the reaction process, so that the equipment is simple, the operation is easy, the reaction can be continuously carried out, the production efficiency is improved, and the impurity gas phosgene which is difficult to separate is not generated.
Description
Technical field
The present invention relates to the synthetic field of material, more specifically relate to a kind of preparation method of fluid bed and a kind of boron chloride without sieve plate.
Background technology
Boron chloride can be used on the technical process such as diffusion, Implantation, dry etching and manufacture solar cell device of silicon semiconductor device; Also can be used as producing the catalyst in fibre-optic basic material and styrene polymerization reaction, also for the purification process of aluminium, zinc, magnesium and copper alloy, to remove nitride, carbide and oxide from motlten metal; Welding solder flux as alloys such as aluminium, iron, zinc, tungsten and Monels; Boron chloride is also for extinguishing magnesium fire and the propellant in heat-treatment furnace; Can be used as intermediate and the pyrolytic boron nitride of producing diborane, refractory metal boride etc.
The preparation of boron chloride at present mainly contains two kinds of process systems, a kind of is the system that adopts molten salt bath, as US Patent No. 2,097,482, US3,019,089, US3,152,869, US4,125,590 etc., first the salt of boracic is converted into boron carbide, this process conventionally process is made boron oxide by boron salt, then reacts with carbon the boron carbide piece that generates sintering, and last and chlorine reaction generates boron chloride, the oxide of boron reacts the higher temperature of process need that generates boron carbide with carbon, generally more than 800 ℃; The another kind of fluid bed system that has sieve plate that adopts, as Canadian Patent CA 632713 use boron oxides, carbon dust and chlorine are reacted and prepare boron chloride under 600 ℃ of conditions by fluid bed, the method control procedure more complicated, productive rate is low, although reduced reaction temperature, had hypertoxic accessory substance phosgene COCl
2produce COCl
2boiling point is 8.2 ℃, with BCl
312.5 ℃ very approaching, bring difficulty to next step separating-purifying, and the raw material of melting is easy to blocking screen plate hole, need periodic cleaning, cause generating and produce and cannot carry out continuously.
Summary of the invention
In view of the problem that prior art exists, the object of the present invention is to provide a kind of preparation method of fluid bed and boron chloride without sieve plate, it can overcome sieve plate of the prior art and stop up.
Another object of the present invention is to a kind of preparation method of boron chloride, it has solved course of reaction and has produced difficult removing impurities gas phosgene.
To achieve these goals, in first aspect, the invention provides a kind of fluid bed without sieve plate, comprising: bed body; Carrier gas body source, Chao Chuanti top, Cong Chuanti bottom provides vector gas to bed body; Reacting gas feedway, provides reacting gas to bed body; Raw material feed device, provides powder material to bed body; Heater, heats bed body; Slag-drip opening, the reaction slag that the reaction in bed body is generated is discharged; Separator, is connected in a body, and the material after bed precursor reactant is carried out to separation, to obtain final products.
To achieve these goals, in second aspect, the invention provides a kind of preparation method of boron chloride, it adopts the fluid bed without sieve plate described in above-mentioned first aspect, and the preparation method of described boron chloride comprises: powder stock alkaline earth boride is filled in the bed body without the fluid bed of sieve plate by raw material feed device; Open carrier gas body source, vector gas be passed in the bed body without the fluid bed of sieve plate, make powder stock alkaline earth boride at the bed body of the fluid bed without sieve plate in fluidized state; Open heater bed body is heated, in temperature, reach after set point of temperature, pass into reacting gas anhydrous hydrogen chloride; Question response reaches specified sections after the time, opens and starts separator, to obtain required boron chloride.
Beneficial effect of the present invention is as follows.
Employing, without the fluid bed of sieve plate, just can be reacted at lower temperature, has reduced energy consumption; The improvement of this apparatus structure has solved the problem of the easy blocking screen plate hole of course of reaction, makes equipment simple, easy operating, and reaction can be carried out continuously, has improved production efficiency.Adopting alkaline earth boride and hydrogen chloride is raw material, has solved course of reaction and has produced difficult removing impurities gas phosgene.
Accompanying drawing explanation
Fig. 1 is according to the structural representation of the fluid bed without sieve plate of the present invention;
Fig. 2 is according to the horizontal cross-section schematic diagram of the vector gas guiding piece of the fluid bed without sieve plate of the present invention and vector gas entrance structure relation;
Fig. 3 is according to the vertical cross-section schematic diagram of the vector gas guiding piece of the fluid bed without sieve plate of the present invention and vector gas entrance structure relation;
Wherein, description of reference numerals is as follows:
1 body 2 carrier gas body source 3 reacting gas feedway
4 raw material feed device 5 heater 6 slag-drip openings
7 separator 71 gas-solid separating device 72 gas air separations
73 condensing unit 9 reacting gas treating apparatus
10 vector gas guiding piece 101 oblique portion 103 inwalls
21 vector gas entrance A vertical axis
The specific embodiment
Below in conjunction with accompanying drawing, illustrate according to the preparation method of fluid bed and boron chloride without sieve plate of the present invention.
First the fluid bed without sieve plate according to first aspect present invention is described.
As shown in Figure 1, according to the fluid bed without sieve plate of the present invention, comprising: bed body 1; Carrier gas body source 2, the top from the bottom of bed body 1 towards bed body 1 provides vector gas to bed body 1; Reacting gas feedway 3, provides reacting gas to bed body 1; Raw material feed device 4, provides powder material to bed body 4; Heater 5, heats bed body 1; Slag-drip opening 6, the reaction slag that the reaction in bed body 1 is generated is discharged; Separator 7, is connected in a body 1, the reacted material of bed body 1 is carried out to separation, to obtain final products.
According in the fluid bed without sieve plate of the present invention, preferably, bed body 1 be shaped as column type.Preferably, carbon or the carborundum of by high purity quartz, silica, silicon nitride, making or be coated with described material of bed body 1 are made.
As shown in Figure 1, according to the fluid bed without sieve plate of the present invention, preferably, the described fluid bed without sieve plate also comprises: reacting gas treating apparatus 9, for reacting gas feedway 3 is supplied to, the reacting gas of a body 1 dehydrates and heat temperature raising.
As shown in Figure 1, according to the fluid bed without sieve plate of the present invention, preferably, the described fluid bed without sieve plate also comprises: vector gas guiding piece 10, guides for carrier gas body source 2 being supplied to the vector gas of a body 1.
As depicted in figs. 1 and 2, according to the fluid bed without sieve plate of the present invention, preferably, vector gas guiding piece 10 is with the oblique portion 101 of oriented bed body 1 convergent.
As shown in Figure 2, according to the fluid bed without sieve plate of the present invention, preferably, the inwall 103 of 21 position, connection carrier gas access of the relative vector gas guiding piece 10 of direction that the vector gas of carrier gas body source 2 enters into the vector gas entrance 21 of vector gas guiding piece 10 tilts.
As shown in Figure 3, according to the fluid bed without sieve plate of the present invention, preferably, the inwall 103 of 21 position, connection carrier gas access of the relative vector gas guiding piece 10 of direction that the vector gas of carrier gas body source 2 enters into the vector gas entrance 21 of vector gas guiding piece 10 tilt and in the plane of the vertical axis A with respect to bed body 1 carrier gas access 21 direction relatively this vertical axis A be inclined upwardly.
As shown in Figure 2, according to the fluid bed without sieve plate of the present invention, preferably, vector gas entrance 21 is at least two, and wherein at least one pair of vector gas entrance 21 is oppositely arranged along the inwall 103 of vector gas guiding piece 10.
According in the fluid bed without sieve plate of the present invention, preferably, described separator 7 comprises: gas-solid separating device 71, for making the gaseous material of a body 1 reacted material separated with solid matter; Gas air separation 72, for making the multiple gaseous material of a body 1 reacted material separated; And condensing unit 73, by condensation, obtain described final products.Preferably, gas-solid separating device 71 adopts filter type, the Filter column that preferably adopts glass fibre to form.Preferably, gas air separation 72 can be taked to carry out such as but not limited to chemical reaction or chemisorbed mode according to various gas properties contained in the reacted material of bed body 1.Condensing unit 73 can adopt condensation separation mode to obtain final products according to the final physical property that needs acquisition, and more preferably, condensing unit 73 can adopt shell and tube condenser.
Secondly explanation is according to the preparation method of the boron chloride of second aspect present invention.
The described fluid bed without sieve plate that adopts above-mentioned first aspect according to the preparation method of the boron chloride of second aspect present invention, the preparation method of described boron chloride comprises: powder stock alkaline earth boride is filled in the bed body 1 without the fluidized bed plant of sieve plate by raw material feed device 4; Open carrier gas body source 2, vector gas be passed in the bed body 1 without the fluidized bed plant of sieve plate, make powder stock at the bed body 1 of the fluidized bed plant without sieve plate in fluidized state; Open 5 pairs of bed bodies 1 of heater and heat, in temperature, reach after set point of temperature, pass into reacting gas anhydrous hydrogen chloride; Question response reaches specified sections after the time, opens and starts separator 7, to obtain required boron chloride.
According in the preparation method of boron chloride of the present invention, also can comprise step: when opening and starting separator 7, open slag-drip opening, the reaction slag that the reaction in bed body 1 is generated is discharged.
According in the preparation method of boron chloride of the present invention, preferably, described alkaline earth boride is calcium boride or boronation magnesium, and its diameter is 20 ~ 200 orders.
According in the preparation method of boron chloride of the present invention, preferably, reacting gas anhydrous hydrogen chloride dehydrates and heat temperature raising via reacting gas treating apparatus 9 before in being passed into a body 1.
According in the preparation method of boron chloride of the present invention, preferably, course of reaction temperature is 550 ℃ ~ 700 ℃, and the reaction time is 1 ~ 2h.
According in the preparation method of boron chloride of the present invention, preferably, the flow of described alkaline earth boride is 80 ~ 85g/h, and the flow of anhydrous hydrogen chloride is 500 ~ 600g/h.
According in the preparation method of boron chloride of the present invention, preferably, described in open and start separator 7 and comprise and make reacted material condensation to obtain boron chloride to obtain required boron chloride.Preferably, condensation temperature is-10 ℃～-30 ℃.
According in the preparation method of boron chloride of the present invention, described calcium boride is preferably six calcium borides.
When described alkaline earth boride adopts six calcium borides, reaction equation:
CaB
6+20HCl=6BCl
3+CaCl
2+10H
2
In reacted material, mainly contain: BCl
3, carrier gas, hydrogen, BCl
3, oxygen, nitrogen, Cl
2, gas and calcium chloride slag and the calcium boride etc. such as HCl.In gas-solid separating device 71, preferably by the Filter column being formed by glass fibre, calcium chloride slag is separated with other gases with calcium boride, to realize gas solid separation; In gas air separation 72, preferably adopt red-hot copper powder or carbon dust etc. can isolate oxygen and hydrogen, by alkali solid sorbing material, can remove Cl
2and HCl, alkali solid preferably adopts NaOH or potassium hydroxide; Carrying out the gentle gas after separating of gas solid separation, in condensing unit 73, by controlling the condensation temperature of condensing unit, make BCl
3thereby condensation of gas makes BCl
3separated with carrier gas, carrier gas is discharged and is reclaimed from condensing unit 73.Preferably, the carrier gas of discharging from condensing unit 73 is processed and reclaims through the active carbon packed column of alkaline solution immersion, drying and processing, to improve the purity of the carrier gas of recovery.Preferably, alkaline solution adopts sodium hydroxide solution or potassium hydroxide solution.
When described alkaline earth boride adopts boronation magnesium, reaction equation:
MgB
2+8HCl=2BCl
3+MgCl
2+4H
2
In reacted material, mainly contain: BCl
3, carrier gas, hydrogen, BCl
3, oxygen, nitrogen, Cl
2, gas and magnesium chloride slag and the boronation magnesium etc. such as HCl.For separator 7(gas-solid separating device 71, gas air separation 72, condensing unit 73) operation can with adopt the mode of six calcium borides identical above, at this, omit repeat specification.
According in the preparation method of boron chloride of the present invention, preferably, described vector gas is inert gas.Described inert gas can be nitrogen, argon gas, helium or the mist of two kinds of compositions wherein, preferably, selects nitrogen.Preferably, its flow is 0.5m
3/ h ~ 10m
3/ h.
According in the preparation method of boron chloride of the present invention, preferably, pass into and vector gas is passed into after reacting gas anhydrous hydrogen chloride to the amount of turning down the fluidized state that maintains alkaline earth boride without the flow in the bed body 1 of the fluid bed of sieve plate.
The 3rd, the embodiment of the preparation method of boron chloride according to the present invention is described.
By particle diameter, being 20 ~ 30 object powder six calcium borides is filled in the bed body 1 without the fluid bed of sieve plate with 80g/h flow by raw material feed device 4; Open carrier gas body source 2, nitrogen be passed in the bed body 1 without the fluid bed of sieve plate, make powder six calcium borides at the bed body 1 of the fluid bed without sieve plate in fluidized state; Opening 5 pairs of bed bodies 1 of heater heats, in temperature, reach after 550 ℃, with 500g/h flow, to bed body 1, pass into the reacting gas anhydrous hydrogen chloride being dehydrated by reacting gas treating apparatus 9, constantly reduce nitrogen flow to maintain the fluidized state of calcium boride, reaction 1h simultaneously; Open afterwards and start separator 7, the Filter column consisting of the glass fibre in gas-solid separating device 71 is isolated calcium chloride slag and calcium boride, then by copper powder red-hot in gas air separation 72, oxygen and hydrogen are removed, by solid state hydrogen sodium oxide molybdena adsorbent, removed Cl afterwards
2and HCl, finally in the condenser 73 that adopts shell and tube condenser, at-10 ℃, carry out condensation and obtain colourless boron chloride, the nitrogen of discharging from condenser 73 adopt through sodium hydroxide solution soak, the active carbon packed column of drying and processing processes.
100 ~ 120 object powder six calcium borides are filled in the bed body 1 without the fluid bed of sieve plate with 85g/h flow by raw material feed device 4; Open carrier gas body source 2, argon gas be passed in the bed body 1 without the fluid bed of sieve plate, make powder six calcium borides at the bed body 1 of the fluid bed without sieve plate in fluidized state; Opening 5 pairs of bed bodies 1 of heater heats, in temperature, reach after 700 ℃, with 600g/h flow, to bed body 1, pass into the reacting gas anhydrous hydrogen chloride being dehydrated by reacting gas treating apparatus 9, constantly reduce argon flow amount to maintain the fluidized state of calcium boride, reaction 1.5h simultaneously; Open afterwards and start separator 7, the Filter column consisting of the glass fibre in gas-solid separating device 71 is isolated calcium chloride slag and calcium boride, then by carbon dust red-hot in gas air separation 72, oxygen and hydrogen are removed, by solid state hydrogen potassium oxide adsorbent, removed Cl afterwards
2and HCl; Finally in the condenser 73 that adopts shell and tube condenser, at-30 ℃, carry out condensation, obtain colourless boron chloride, the argon gas that condenser 73 is discharged reclaims, and the nitrogen employing process potassium hydroxide solution of discharging from condenser 73 soaks, the active carbon packed column of drying and processing is processed.
180 ~ 200 object powder boronation magnesium are filled in the bed body 1 without the fluid bed of sieve plate with 82g/h flow by raw material feed device 4; Open carrier gas body source 2, helium be passed in the bed body 1 without the fluid bed of sieve plate, make powder boronation magnesium at the bed body 1 of the fluid bed without sieve plate in fluidized state; Opening 5 pairs of bed bodies 1 of heater heats, in temperature, reach after 650 ℃, with 550g/h flow, to bed body 1, pass into the reacting gas anhydrous hydrogen chloride being dehydrated by reacting gas treating apparatus 9, constantly reduce helium gas flow to maintain the fluidized state of calcium boride, reaction 2h simultaneously; Open afterwards and start separator 7, the Filter column consisting of the glass fibre in gas-solid separating device 71 is isolated magnesium chloride slag and boronation magnesium, then by carbon dust red-hot in gas air separation 72, oxygen and hydrogen are removed, by solid state hydrogen potassium oxide adsorbent, removed Cl afterwards
2and HCl; Finally in the condenser 73 that adopts shell and tube condenser, carry out condensation and obtain colourless boron chloride at-10 ℃, the helium employing process sodium hydroxide solution of discharging from condenser 73 soaks, the active carbon packed column of drying and processing is processed.
The testing result of embodiment is finally described.
Table 1 has provided the testing result of embodiment 1-3.During detection, condenser 8(being adopted to shell and tube condenser) gas of input detects.Detection means adopts FTIS (FTIR) and uv analyzer (UV analyzer)
The testing result of table 1 embodiment 1-3
| |
|
|
|
| Boron chloride purity | 99.9% | 99.7% | 99.5% |
| N 2 | 0.05% | ----- | ----- |
| Ar | ----- | 0.04% | ----- |
| He | ----- | ----- | 0.01% |
| Oxygen | 0.005% | 0.006% | 0.007% |
| Total hydrocarbon content (CH4) | 0.005% | 0.004% | 0.013% |
| Carbon dioxide | 0.03% | 0.05% | 0.07% |
| Chlorine | 0.01% | 0.2% | 0.4% |
As seen from Table 1, the preparation method of boron chloride of the present invention can obtain the boron chloride that purity is high.
Claims (10)
1. without a fluid bed for sieve plate, comprising:
Bed body (1);
Carrier gas body source (2), the top from the bottom of bed body (1) towards bed body (1) provides vector gas to bed body (1);
Reacting gas feedway (3), provides reacting gas to bed body (1);
Raw material feed device (4), provides powder material to bed body (4);
Heater (5), heats bed body (1);
Slag-drip opening (6), the reaction slag that the reaction in bed body (1) is generated is discharged;
Separator (7), is connected in a body (1), the reacted material of bed body (1) is carried out to separation, to obtain final products.
2. the fluid bed without sieve plate according to claim 1, is characterized in that, the described fluid bed without sieve plate also comprises: vector gas guiding piece (10), guides for carrier gas body source (2) being supplied to the vector gas of a body (1).
3. the fluid bed without sieve plate according to claim 2, is characterized in that, vector gas guiding piece (10) is with the oblique portion (101) of oriented bed body (1) convergent.
4. the fluid bed without sieve plate according to claim 2, it is characterized in that, the inwall (103) of position of connection carrier gas access (21) of the relative vector gas guiding piece of direction (10) that the vector gas of carrier gas body source (2) enters into the vector gas entrance (21) of vector gas guiding piece (10) tilts.
5. the fluid bed without sieve plate according to claim 2, it is characterized in that, the inwall (103) of position of connection carrier gas access (21) of the relative vector gas guiding piece of direction (10) that the vector gas of carrier gas body source (2) enters into the vector gas entrance (21) of vector gas guiding piece (10) tilt and the plane of the vertical axis with respect to bed body (1) (A) in relative this vertical axis (A) of the direction of carrier gas access (21) be inclined upwardly.
6. the fluid bed without sieve plate according to claim 4, is characterized in that, vector gas entrance (21) is at least two, and wherein at least one pair of vector gas entrance (21) is oppositely arranged along the inwall (103) of vector gas guiding piece (10).
7. a preparation method for boron chloride, it adopts the fluid bed without sieve plate as described in any one in claim 1-6, and the preparation method of described boron chloride comprises:
Powder stock alkaline earth boride is filled in the bed body (1) without the fluid bed of sieve plate by raw material feed device (4);
Open carrier gas body source (2), vector gas be passed in the bed body (1) without the fluid bed of sieve plate, make powder stock alkaline earth boride at the bed body (1) of the fluid bed without sieve plate in fluidized state;
Open heater (5) bed body (1) is heated, in temperature, reach after set point of temperature, pass into reacting gas anhydrous hydrogen chloride;
Question response reaches specified sections after the time, opens and starts separator (7), to obtain required boron chloride.
8. the preparation method of boron chloride according to claim 7, is characterized in that, also comprises step: when opening and starting separator (7), open slag-drip opening (6), the reaction slag that the reaction in bed body (1) is generated is discharged.
9. the preparation method of boron chloride according to claim 7, is characterized in that, reacting gas anhydrous hydrogen chloride dehydrates and heat temperature raising before in being passed into a body (1).
10. the preparation method of boron chloride according to claim 7, it is characterized in that, pass into and vector gas is passed into after reacting gas anhydrous hydrogen chloride to the amount of turning down the fluidized state that maintains alkaline earth boride without the flow in the bed body (1) of the fluid bed of sieve plate.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210217421.0A CN103506056B (en) | 2012-06-28 | 2012-06-28 | Sieve plate-free fluidized bed and preparation method of boron trichloride |
| PCT/CN2013/077478 WO2014000592A1 (en) | 2012-06-28 | 2013-06-19 | Fluidized bed without sieve plate and method for preparing boron trichloride |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210217421.0A CN103506056B (en) | 2012-06-28 | 2012-06-28 | Sieve plate-free fluidized bed and preparation method of boron trichloride |
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|---|---|
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| CN103506056B CN103506056B (en) | 2015-09-30 |
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| WO (1) | WO2014000592A1 (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103950947A (en) * | 2014-05-20 | 2014-07-30 | 方治文 | Preparation method of high-purity boron trichloride-11 |
| TWI555705B (en) * | 2014-03-18 | 2016-11-01 | 曼瑟森三汽油公司 | Reduction of sicl4 in the presence of bcl3 |
| CN106319216A (en) * | 2015-07-06 | 2017-01-11 | 广东先导稀材股份有限公司 | Gas-gas reaction device |
| WO2020003925A1 (en) * | 2018-06-26 | 2020-01-02 | 昭和電工株式会社 | Method for producing boron trichloride |
| CN114572992A (en) * | 2022-03-09 | 2022-06-03 | 福建福豆新材料有限公司 | Hydrogen chloride removal device for purifying boron trichloride and boron trichloride purification system |
| CN114570294A (en) * | 2022-04-21 | 2022-06-03 | 苏州金宏气体股份有限公司 | Boron trifluoride continuous production device and method based on fluidized bed reactor |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3839538A (en) * | 1971-03-20 | 1974-10-01 | Elektroschmelzwerk Kampten Gmb | Process for the manufacture of boron halides |
| CN201390803Y (en) * | 2008-12-02 | 2010-01-27 | 广州有色金属研究院 | Fluidized bed reaction equipment without sieve plate for preparing polysilicon granules |
| CN201431874Y (en) * | 2009-03-20 | 2010-03-31 | 仙桃市中星电子材料有限公司 | Spiral fluidizing chlorination furnace without sieve plates |
| CN101912752A (en) * | 2010-08-20 | 2010-12-15 | 中国航天空气动力技术研究院 | Solid particle player |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2735041B1 (en) * | 1995-06-07 | 1997-07-11 | Gec Alsthom Stein Ind | FLUIDIZED BED REACTOR FOR HEAT TREATMENT OF WASTE |
| DE102004051477B4 (en) * | 2004-10-22 | 2008-10-02 | Alstom Technology Ltd. | Method for regulating the amount of circulating fluid in a circulating fluidized bed reactor system |
| CN102230732B (en) * | 2011-07-01 | 2013-06-19 | 广州有色金属研究院 | Closed automatic slag discharge device for boiling chlorination furnace |
-
2012
- 2012-06-28 CN CN201210217421.0A patent/CN103506056B/en active Active
-
2013
- 2013-06-19 WO PCT/CN2013/077478 patent/WO2014000592A1/en active Application Filing
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3839538A (en) * | 1971-03-20 | 1974-10-01 | Elektroschmelzwerk Kampten Gmb | Process for the manufacture of boron halides |
| CN201390803Y (en) * | 2008-12-02 | 2010-01-27 | 广州有色金属研究院 | Fluidized bed reaction equipment without sieve plate for preparing polysilicon granules |
| CN201431874Y (en) * | 2009-03-20 | 2010-03-31 | 仙桃市中星电子材料有限公司 | Spiral fluidizing chlorination furnace without sieve plates |
| CN101912752A (en) * | 2010-08-20 | 2010-12-15 | 中国航天空气动力技术研究院 | Solid particle player |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI555705B (en) * | 2014-03-18 | 2016-11-01 | 曼瑟森三汽油公司 | Reduction of sicl4 in the presence of bcl3 |
| CN103950947A (en) * | 2014-05-20 | 2014-07-30 | 方治文 | Preparation method of high-purity boron trichloride-11 |
| CN106319216A (en) * | 2015-07-06 | 2017-01-11 | 广东先导稀材股份有限公司 | Gas-gas reaction device |
| WO2020003925A1 (en) * | 2018-06-26 | 2020-01-02 | 昭和電工株式会社 | Method for producing boron trichloride |
| US12049406B2 (en) | 2018-06-26 | 2024-07-30 | Resonac Corporation | Method of producing boron trichloride |
| CN114572992A (en) * | 2022-03-09 | 2022-06-03 | 福建福豆新材料有限公司 | Hydrogen chloride removal device for purifying boron trichloride and boron trichloride purification system |
| CN114570294A (en) * | 2022-04-21 | 2022-06-03 | 苏州金宏气体股份有限公司 | Boron trifluoride continuous production device and method based on fluidized bed reactor |
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| CN103506056B (en) | 2015-09-30 |
| WO2014000592A1 (en) | 2014-01-03 |
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