CN211255274U - Experimental device for prepare high-purity boron trichloride - Google Patents
Experimental device for prepare high-purity boron trichloride Download PDFInfo
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- CN211255274U CN211255274U CN201922247286.4U CN201922247286U CN211255274U CN 211255274 U CN211255274 U CN 211255274U CN 201922247286 U CN201922247286 U CN 201922247286U CN 211255274 U CN211255274 U CN 211255274U
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- boron trichloride
- rectifying tower
- purity boron
- adsorber
- experimental device
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- FAQYAMRNWDIXMY-UHFFFAOYSA-N trichloroborane Chemical compound ClB(Cl)Cl FAQYAMRNWDIXMY-UHFFFAOYSA-N 0.000 title claims abstract description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000002994 raw material Substances 0.000 claims abstract description 16
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 15
- 239000010959 steel Substances 0.000 claims abstract description 15
- 239000006096 absorbing agent Substances 0.000 claims abstract description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 10
- 238000005070 sampling Methods 0.000 claims description 10
- 239000011521 glass Substances 0.000 claims description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- 239000003463 adsorbent Substances 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 239000002808 molecular sieve Substances 0.000 claims description 2
- 239000000523 sample Substances 0.000 claims description 2
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 2
- 238000005485 electric heating Methods 0.000 claims 2
- 238000004321 preservation Methods 0.000 claims 2
- 239000000945 filler Substances 0.000 claims 1
- 229910001220 stainless steel Inorganic materials 0.000 claims 1
- 238000002474 experimental method Methods 0.000 abstract description 4
- 238000000034 method Methods 0.000 abstract description 4
- 238000006386 neutralization reaction Methods 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 2
- 238000007701 flash-distillation Methods 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 16
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 8
- 238000001816 cooling Methods 0.000 description 5
- 229910002092 carbon dioxide Inorganic materials 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 3
- YGYAWVDWMABLBF-UHFFFAOYSA-N Phosgene Chemical compound ClC(Cl)=O YGYAWVDWMABLBF-UHFFFAOYSA-N 0.000 description 3
- 239000000460 chlorine Substances 0.000 description 3
- 229910052801 chlorine Inorganic materials 0.000 description 3
- 229910015844 BCl3 Inorganic materials 0.000 description 2
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 229910003902 SiCl 4 Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 2
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 2
- 239000012774 insulation material Substances 0.000 description 2
- 239000002085 irritant Substances 0.000 description 2
- 231100000021 irritant Toxicity 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 229910052582 BN Inorganic materials 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000003287 bathing Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- UORVGPXVDQYIDP-BJUDXGSMSA-N borane Chemical class [10BH3] UORVGPXVDQYIDP-BJUDXGSMSA-N 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 238000005271 boronizing Methods 0.000 description 1
- QGJOPFRUJISHPQ-NJFSPNSNSA-N carbon disulfide-14c Chemical compound S=[14C]=S QGJOPFRUJISHPQ-NJFSPNSNSA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- DIWKDXFZXXCDLF-UHFFFAOYSA-N chloroethyne Chemical compound ClC#C DIWKDXFZXXCDLF-UHFFFAOYSA-N 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000003517 fume Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 235000019614 sour taste Nutrition 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The utility model discloses an experimental device for preparing high-purity boron trichloride, which comprises a raw material steel cylinder, an absorber I, a water bath, an absorber II, a rectifying tower, a finished product tank, a neutralizer and a vacuum pump; a condenser and a head tank are connected with the top end of the rectifying tower, a reboiler is arranged at the bottom of the rectifying tower, and a bath kettle is arranged in the reboiler at the bottom; the outlet of the finished product of high-purity boron trichloride is positioned at the lower part of the elevated tank. The utility model discloses the rectifying column adopts well tower feeding, the ejection of compact of top of the tower, and top of the tower condenser flash distillation vapour advances neutralization apparatus to handle, carries out effectual control to the safety of experiment, utilizes the method of inhaling additional rectification to prepare high-purity boron trichloride. The raw materials sequentially enter an absorber I, a water bath, an absorber II, a rectifying tower and a finished product tank to finally obtain the high-purity boron trichloride which can be used for preparing various substances.
Description
Technical Field
The utility model relates to a gas purification technique, concretely relates to prepare experimental apparatus of high-purity boron trichloride.
Background
Boron trichloride is a colorless fuming liquid or gas, has irritant sour taste and is easy to deliquesce. Is dissolved in benzene and carbon disulfide, has high chemical reaction activity and is explosively decomposed when meeting water. With copper and its alloys, there is a possibility of generating explosive chloroethyne, which is highly corrosive to most metals in the presence of moisture and can also corrode glass and the like. White, corrosive, dense fumes can be generated in humid air. The hydrogen chloride gas can react violently when meeting water and releases irritant and corrosive hydrogen chloride gas.
Can be used for preparing high-purity boron, catalyst for organic synthesis, fluxing agent for silicate decomposition, and can be used for boronizing steel, doping source of semiconductor, and additive of deoxidant, nitride and carbide in alloy refining. It can also be used to make boron nitride and borane compounds.
At present, high-purity boron trichloride is basically difficult to obtain at home, so that the development of an experimental device for preparing the boron trichloride to obtain the high-purity boron trichloride has positive practical significance.
SUMMERY OF THE UTILITY MODEL
The utility model aims at providing an experimental apparatus of preparation high-purity boron trichloride prepares high-purity boron trichloride to industrial-grade boron trichloride purification, makes this kind of method can obtain extensive popularization.
In order to achieve the purpose of the utility model, the utility model adopts the technical proposal that: an experimental device for preparing high-purity boron trichloride comprises a raw material steel cylinder, an adsorber I, a water bath, an adsorber II, a rectifying tower, a finished product tank, a neutralizer and a vacuum pump which are connected in sequence; the outlet of the raw material steel cylinder is connected with a pressure reducing valve and a flowmeter; a condenser and a head tank are connected to the top end of the rectifying tower, a reboiler is arranged at the bottom of the rectifying tower, and a bath kettle is arranged in the reboiler at the bottom; the vacuum pump is a rotary vane vacuum pump; the outlet pipeline of the second adsorber is connected with a needle valve sampling port; the elevated tank is connected with a needle valve sampling port.
In the technical scheme, the pressure reducing valve is selected from the models of 0-5MPa of inlet pressure and 0-1.6MPa of outlet pressure.
In the technical scheme, the flowmeter is a 0-1L/min glass tube flowmeter.
In the technical scheme, the glass device for the experiment is a pressure-resistant 1MPa glass instrument.
In the technical scheme, an adsorbent is filled in the first adsorber, and the adsorbent is activated carbon.
In the technical scheme, the second adsorber is filled with an adsorbent which is a 13X molecular sieve.
In the technical scheme, the water bath is an open water bath, and the bottom of the water bath is inserted with a temperature measuring probe.
In the technical scheme, a reboiler is used for bathing a pot through a heat source; the cold source of the condenser comes from cooling circulating water.
In the technical scheme, the rectifying tower adopts middle tower feeding and tower top discharging.
In the technical scheme, the finished tank is made of polyurethane external thermal insulation material.
In the technical scheme, sodium hydroxide lye is filled in the neutralizer.
In the technical scheme, the needle valve is a tetrafluoro needle valve.
Because of the application of the technical scheme, compared with the prior art, the utility model has the following advantages:
1. the utility model discloses an experimental apparatus for prepare high-purity boron trichloride for the first time, utilize and inhale the method of additional rectification and prepare high-purity boron trichloride. Raw materials sequentially enter an absorber I, a water bath, an absorber II, a rectifying tower and a finished product tank, and finally high-purity boron trichloride is obtained and can be used for preparing various substances;
2. in the experimental device of high-purity boron trichloride, the rectifying tower adopts the feeding of the middle tower, the discharging of the top of the tower, and the flash steam of the condenser at the top of the tower enters the neutralizer for processing, so as to effectively control the safety of the experiment;
3. the utility model discloses an experimental apparatus of preparation high-purity boron trichloride purifies efficiently, and the material of especially separation can obtain properly handling, easily operates moreover, is suitable for popularization and application.
Drawings
FIG. 1 is a schematic structural diagram of an experimental apparatus for preparing high-purity boron trichloride.
Wherein: 1. a raw material steel cylinder, 1-1, a pressure reducing valve, 1-2, a glass flow meter, 1-3, a tetrafluoro needle valve, 2, a first adsorber, 2-1, a first adsorber inlet stop valve, 2-2, a first adsorber outlet stop valve, 3, a water bath, 3-1, a temperature controller 4, a second adsorber, 4-1, a second adsorber inlet stop valve, 4-2, a second adsorber outlet stop valve, 4-3, a tee joint, 4-4, a tetrafluoro needle valve, 4-5, a tee joint, 4-6, a tetrafluoro needle valve, 5, a rectifying tower, 5-1, a condenser, 5-2, a reboiler, 5-3, a bath kettle, 5-4, a temperature controller, 5-5, a head tank, 5-6, a tetrafluoro needle valve, 5-7, a tee joint, 5-8 and a tetrafluoro needle valve, 5-9 of a stop valve, 5-10 of a tee joint, 6 of a finished product tank, 6-1 of the finished product tank, 7 of a neutralizer, 7-1 of alkali liquor, 7-2 of a neutralizer outlet valve, 7-3 of a needle valve, 7-4 of the tee joint, 7-5 of the stop valve, 7-6 of the tee joint, 8 of a vacuum pump, 8-1 of a vacuum pump inlet one-way valve, 8-2 of the vacuum pump inlet stop valve, 8-3 of the vacuum pump outlet stop valve and 8-4 of a vacuum pump bypass stop valve.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative work belong to the protection scope of the present invention.
In the first embodiment, referring to fig. 1, an experimental apparatus for preparing high-purity boron trichloride includes a raw material steel cylinder, a first adsorber, a water bath, a second adsorber, a rectifying tower, a finished product tank, a neutralizer and a vacuum pump, which are connected in sequence; the outlet of the raw material steel cylinder is connected with a pressure reducing valve and a flowmeter; a condenser and a head tank are connected to the top end of the rectifying tower, a reboiler is arranged at the bottom of the rectifying tower, and a bath kettle is arranged in the reboiler at the bottom; the vacuum pump is a rotary vane vacuum pump; the outlet pipeline of the second adsorber is connected with a needle valve sampling port; the high-level groove is connected with a needle valve sampling port; in the figure, a single arrow indicates the gas running direction, and a double arrow indicates the cooling circulating water running direction.
The working process of the experimental device comprises the following steps:
(1) sequentially connecting experimental equipment, pipelines, valves and the like according to an experimental flow drawing, and well ensuring the safety and the stability of the experimental equipment;
(2) closing the outlet valve of the raw material steel cylinder, the inlet and outlet valves of the neutralizer, the bypass valve of the vacuum pump and the sampling valve, and fully opening all the valves; vacuumizing the system by using a vacuum pump, and closing the vacuum pump and an air inlet valve thereof when the system is vacuumized to the limit;
(3) opening an outlet valve of the raw material steel cylinder, closing the outlet valve of the steel cylinder after the pressure of the system reaches 2bar, repeating the step 2 for 3 times, and closing an inlet valve and an outlet valve of a vacuum pump after the system is vacuumized to keep the micro negative pressure of the system;
(4) opening an outlet valve of the raw material steel cylinder, regulating the pressure to 0.3MPa through a pressure reducing valve, regulating the flow to 500ml/min, and slowly entering an adsorber I;
(5) heating the first adsorber to 250 deg.c electrically, cooling the material gas in water bath via the first adsorber, and cooling in the second adsorber after the temperature is normal. Then, after sampling and analyzing from a sampling port to be qualified, opening a stop valve in front of the rectifying tower to enter the rectifying tower for rectifying treatment;
(6) the tower kettle of the rectifying tower is heated by a bath kettle, and a cold source of a condenser at the tower top is provided by cooling circulating water; the temperature is controlled to be 45-50 ℃, the temperature of the condenser is controlled to be 5-10 ℃, and the rectification pressure is 2.5 bar;
(7) the finished product of the condenser at the top of the tower enters a head tank, a sampling analysis port is arranged on the head tank, the finished product enters a finished product tank after being analyzed to be qualified, the pipeline of the head tank is divided into two paths, one path of the pipeline flows back to the upper part of the rectifying tower, and the other path of the pipeline is a finished product pipeline;
(8) after the experiment is finished, the non-condensable gas enters a neutralizer for neutralization reaction treatment.
In the utility model, the first adsorber is heated to decompose the phosgene in the raw material gas into chlorine and oxygen at high temperature, and the activated carbon in the first adsorber adsorbs the chlorine and partial moisture, and the chlorine is 1 ppm; the water bath cools the high-temperature gas in the first adsorber to normal temperature; the second adsorber deeply adsorbs carbon dioxide and moisture in the feed gas, wherein the carbon dioxide is 2ppm, and the moisture is 2 ppm; the gas enters a rectifying tower after being adsorbed, a bath kettle at the bottom of the rectifying tower provides a heat source, a condenser at the top of the rectifying tower provides a cold source, an outlet of the condenser at the top of the rectifying tower is connected with a head tank, one path of the outlet of the head tank reflows to an upper tower of the rectifying tower, the other path of the outlet of the head tank is connected with a finished product tank, and light components at the top of the tower are discharged to a neutralizer for neutralization treatment.
In the utility model, the connection is air pipe connection for gas transmission between each component, 1/4-inch clean pipes are adopted for connection, and the pipes and the valves are connected by VCRs; the finished product pipelines out of the rectifying tower are all insulated by adopting insulation materials, each part is provided with a gas inlet and a gas outlet, and according to the experimental scheme of the invention, experimenters in the field are connected according to the site requirements.
The volume components of the raw material gas which can be processed are as follows: 99.9 percent or more of BCl3, 100ppm or less of O2, 400ppm or less of N2, 20ppm or less of CO2, 20ppm or less of CO, 10ppm or less of CH4, 100ppm or less of Cl2, 100ppm or less of COCl2 and 100ppm or less of SiCl 4.
The gas volume components of the finished product are as follows: more than or equal to 99.9999 percent of BCl3, less than or equal to 1ppm of O2, less than or equal to 4ppm of N2, less than or equal to 2ppm of CO2, less than or equal to 0.5ppm of CO, less than or equal to 0.5ppm of CH4, less than or equal to 2ppm of H2O, less than or equal to 1ppm of Cl2, less than or equal to 1ppm of COCl2 and less than or equal to 2ppm of SiCl 4.
In the technical scheme, the working pressure of the rectifying tower is 2.5 bar.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (11)
1. The utility model provides an experimental apparatus for prepare high-purity boron trichloride which characterized in that: the experimental device for preparing the high-purity boron trichloride comprises a raw material steel cylinder, an adsorber I, a water bath, an adsorber II, a rectifying tower, a finished product tank, a neutralizer and a vacuum pump which are connected in sequence; the outlet of the raw material steel cylinder is connected with a pressure reducing valve and a glass tube flowmeter; a water bath tank is connected between the first adsorber and the second adsorber; a condenser and a head tank are connected to the top end of the rectifying tower, a reboiler is arranged at the bottom of the rectifying tower, and a bath kettle is arranged in the reboiler at the bottom; the light component at the top of the rectifying tower is emptied and is connected with a noncondensable gas pipeline at the top of the condenser by a tee joint; the inlet of the neutralizer is respectively connected with the light component branch at the top of the rectifying tower and the second rear branch of the absorber; the inlet of the vacuum pump is connected with a light component pipeline at the top of the rectifying tower and a neutralizer inlet pipeline through a tee joint by a VCR; the outlet of the second adsorber is provided with a tee joint which is respectively connected with the rectifying tower and the front tee joint of the neutralizer; the outlet pipeline of the second adsorber is connected with a sampling analysis port; the elevated tank is connected with a sampling analysis port.
2. The experimental device for preparing high-purity boron trichloride according to claim 1, which is characterized in that: the water bath is an open water bath.
3. The experimental device for preparing high-purity boron trichloride according to claim 1, which is characterized in that: the rectifying tower is a double-section glass device, stainless steel wire mesh filler is filled in the rectifying tower, the height of each section is 0.7 m, and the rectifying tower adopts a vacuum jacket for heat preservation and flange connection for heat preservation in the rectifying section.
4. The experimental device for preparing high-purity boron trichloride according to claim 1, which is characterized in that: the condenser at the top end of the rectifying tower is a coiled glass device and is connected by a flange.
5. The experimental device for preparing high-purity boron trichloride according to claim 1, which is characterized in that: the volume of a reboiler at the bottom of the rectifying tower is 2 liters, and a heat source is from a bath kettle.
6. The experimental device for preparing high-purity boron trichloride according to claim 1, which is characterized in that: the bath kettle is filled with hot water, the electric heating mode is adopted for heating, and a temperature measuring probe is placed in the bath kettle.
7. The experimental device for preparing high-purity boron trichloride according to claim 1, which is characterized in that: the elevated tank is a glass device, and the interface is in a flange structure.
8. The experimental device for preparing high-purity boron trichloride according to claim 1, which is characterized in that: the raw material steel cylinder is a 47L boron trichloride steel cylinder, and 50kg of liquid boron trichloride is filled in the cylinder.
9. The experimental device for preparing high-purity boron trichloride according to claim 1, which is characterized in that: the first adsorber is of an electric heating jacket structure, the volume of the first adsorber is 1000ml, and the adsorbent is activated carbon.
10. The experimental device for preparing high-purity boron trichloride according to claim 1, which is characterized in that: the second adsorber is a normal-temperature adsorber with the volume of 1000ml and the adsorbent is 13X molecular sieve.
11. The experimental device for preparing high-purity boron trichloride according to claim 1, which is characterized in that: the neutralizer is filled with sodium hydroxide lye.
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Address after: No. 09, Yuanda Road, Shitan Industrial Park, Shizi Town, Quanjiao County, Chuzhou City, Anhui Province 239500 Patentee after: Anhui APK Electronic Material Co.,Ltd. Address before: 239500 east side of Chaoyang Road, Shitan Industrial Park, Shizi Town, Quanjiao County, Chuzhou City, Anhui Province Patentee before: ANHUI AIPEIKE ELECTRONIC MATERIALS CO.,LTD. |