CN113582192A - Boron trichloride purification device - Google Patents
Boron trichloride purification device Download PDFInfo
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- CN113582192A CN113582192A CN202110827964.3A CN202110827964A CN113582192A CN 113582192 A CN113582192 A CN 113582192A CN 202110827964 A CN202110827964 A CN 202110827964A CN 113582192 A CN113582192 A CN 113582192A
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- Prior art keywords
- boron trichloride
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- fixedly connected
- purification device
- finished product
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- FAQYAMRNWDIXMY-UHFFFAOYSA-N trichloroborane Chemical compound ClB(Cl)Cl FAQYAMRNWDIXMY-UHFFFAOYSA-N 0.000 title claims abstract description 84
- 238000000746 purification Methods 0.000 title claims abstract description 28
- 239000007789 gas Substances 0.000 claims abstract description 30
- 238000011084 recovery Methods 0.000 claims abstract description 28
- 238000001179 sorption measurement Methods 0.000 claims abstract description 28
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 15
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- 239000003463 adsorbent Substances 0.000 claims description 6
- 238000005485 electric heating Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 5
- 239000002808 molecular sieve Substances 0.000 claims description 4
- 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 4
- 238000001816 cooling Methods 0.000 claims description 3
- 238000007872 degassing Methods 0.000 claims 1
- 229910001873 dinitrogen Inorganic materials 0.000 claims 1
- 238000004821 distillation Methods 0.000 claims 1
- 238000007710 freezing Methods 0.000 claims 1
- 230000008014 freezing Effects 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 239000003507 refrigerant Substances 0.000 claims 1
- 230000008929 regeneration Effects 0.000 claims 1
- 238000011069 regeneration method Methods 0.000 claims 1
- 239000012535 impurity Substances 0.000 abstract description 10
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000000465 moulding Methods 0.000 abstract 1
- 229910000831 Steel Inorganic materials 0.000 description 5
- 239000010959 steel Substances 0.000 description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- 239000012530 fluid Substances 0.000 description 4
- 239000001307 helium Substances 0.000 description 4
- 229910052734 helium Inorganic materials 0.000 description 4
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 239000003921 oil Substances 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 229910052796 boron Inorganic materials 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000005049 silicon tetrachloride Substances 0.000 description 2
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 description 2
- 239000005052 trichlorosilane Substances 0.000 description 2
- YGYAWVDWMABLBF-UHFFFAOYSA-N Phosgene Chemical compound ClC(Cl)=O YGYAWVDWMABLBF-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B35/00—Boron; Compounds thereof
- C01B35/06—Boron halogen compounds
- C01B35/061—Halides
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Separation Of Gases By Adsorption (AREA)
Abstract
本发明公开了一种三氯化硼提纯装置，涉及三氯化硼技术领域。本发明包括原料汇流排、三氯化硼吸附系统、过滤器、精馏塔、液化器、成品储存机构、回收储存机构、回收充装机构、成品充装机构、去尾气系统、热氮气接入口和不凝汽排放机构。本发明通过各个配件的配合，能够较好的对三氯化硼进行提纯，得到高纯度的三氯化硼，且能够自动对不合格的三氯化硼进行回收，降低了生产成本，提纯过程一次成型，保证了提纯工艺的连续性，并避免三氯化硼受到外部杂质的影响，保证了三氯化硼的纯度，且易于操作、效率较高、适合大批量推广。
The invention discloses a boron trichloride purification device, which relates to the technical field of boron trichloride. The invention includes a raw material busbar, a boron trichloride adsorption system, a filter, a rectifying tower, a liquefier, a finished product storage mechanism, a recovery storage mechanism, a recovery filling mechanism, a finished product filling mechanism, a tail gas removal system, and a hot nitrogen inlet. and non-condensable emission mechanism. Through the cooperation of various accessories, the present invention can better purify boron trichloride to obtain high-purity boron trichloride, and can automatically recover unqualified boron trichloride, thereby reducing the production cost and the purification process. One-time molding ensures the continuity of the purification process, avoids the influence of external impurities on boron trichloride, ensures the purity of boron trichloride, is easy to operate, has high efficiency, and is suitable for mass promotion.
Description
Technical Field
The invention belongs to the technical field of boron trichloride, and particularly relates to a boron trichloride purification device.
Background
Boron trichloride is a dangerous chemical, is mainly used as a doping source or an organic synthesis catalyst of semiconductor silicon, and can also be used for preparing high-purity boron or organic boron.
Disclosure of Invention
The invention aims to provide a boron trichloride purification device, which solves the existing problems: the purity of boron trichloride purified by the existing purification device is low, the production cost is high, the operation process is complex, and the purification efficiency is low.
In order to solve the technical problems, the invention is realized by the following technical scheme:
the invention relates to a boron trichloride purification device which comprises a raw material busbar, a boron trichloride adsorption system, a filter, a rectifying tower, a liquefier, a finished product storage mechanism, a recovery filling mechanism, a finished product filling mechanism, a tail gas removing system, a hot nitrogen inlet and a non-condensed steam discharge mechanism, wherein the output end of the raw material busbar is fixedly connected with the input end of the boron trichloride adsorption system, and the hot nitrogen inlet is fixedly connected with the other input end of the boron trichloride adsorption system;
the two boron trichloride adsorption systems are divided into two output ends, wherein the output end of one boron trichloride adsorption system is fixedly connected with the input end of the filter, and the output end of the other boron trichloride adsorption system is fixedly connected with the input end of the tail gas removal system;
the output end of the filter is fixedly connected with the input end of the rectifying tower, the output end of the top of the rectifying tower is fixedly connected with the input end of the liquefier, and the output end of the bottom of the rectifying tower is fixedly connected with the input end of the recovery storage mechanism;
the liquefiers are provided with two output ends, wherein the output end of one liquefier is connected with the non-condensed steam discharge mechanism and the regenerated gas output end of the boron trichloride adsorption system in parallel, and the finished product output end of the other liquefier is connected with the finished product storage mechanism and the recovery storage mechanism in parallel;
the output end of the finished product storage mechanism is fixedly connected with the input end of the finished product filling mechanism, and the output end of the recycling storage mechanism is fixedly connected with the input end of the recycling filling mechanism.
Further, the raw material busbar comprises a first electronic scale, a first gas storage steel cylinder is arranged at the upper end of the first electronic scale, and an electric heating belt is arranged at the output end of the first gas storage steel cylinder.
Further, the first gas storage steel cylinder has an internal gas pressure of 0.2MPa at an ambient temperature of 30 ℃.
Further, the heating temperature of the electric heating belt is 60-80 ℃.
Further, the precision of the filter is 0.1 micron.
Further, an adsorbent is arranged inside the adsorber, and the adsorbent at least consists of one or more of activated carbon and molecular sieve.
Further, boron trichloride adsorption system is including high-temperature furnace, coil pipe cooler and two adsorbers, high-temperature furnace, coil pipe cooler and two adsorbers establish ties in proper order, just high-temperature furnace and two adsorbers all are equipped with an output tube that establishes ties in proper order, output tube and the tail gas system fixed connection that goes.
Furthermore, a cold source of the coil cooler is refrigerating fluid at the temperature of-10 ℃.
Further, a condenser is arranged at the top of the rectifying tower, and a reboiler is arranged at the bottom of the rectifying tower.
Furthermore, a heat source of a reboiler at the bottom of the rectifying tower is heat conduction oil, and a cold source of a condenser at the top of the rectifying tower is refrigerating fluid.
The invention has the following beneficial effects:
according to the invention, through the matching of all the accessories, boron trichloride can be well purified to obtain high-purity boron trichloride, unqualified boron trichloride can be automatically recovered, the production cost is reduced, the purification process is formed at one time, the continuity of the purification process is ensured, the boron trichloride is prevented from being influenced by external impurities, the purity of the boron trichloride is ensured, the operation is easy, the efficiency is high, and the method is suitable for large-scale popularization.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a system diagram of a boron trichloride purification apparatus of the present invention;
FIG. 2 is a system diagram of a raw material bus of a boron trichloride purification apparatus according to the present invention;
FIG. 3 is a system diagram of a boron trichloride adsorption system of a boron trichloride purification apparatus of the present invention.
In the drawings, the components represented by the respective reference numerals are listed below:
1. a raw material bus bar; 101. a first electronic scale; 102. a first gas storage steel cylinder; 103. an electrical heating belt; 2. a boron trichloride adsorption system; 201. a high temperature furnace; 202. a coil cooler; 203. an adsorber; 3. a filter; 4. a rectifying tower; 5. a liquefier; 6. a finished product storage mechanism; 7. a recovery storage mechanism; 8. a recycling and filling mechanism; 9. a finished product filling mechanism; 10. a tail gas removal system; 11. hot nitrogen inlet.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1, the invention is a boron trichloride purification device, which includes a raw material busbar 1, a boron trichloride adsorption system 2, a filter 3, a rectifying tower 4, a liquefier 5, a finished product storage mechanism 6, a recovery storage mechanism 7, a recovery filling mechanism 8, a finished product filling mechanism 9, a tail gas removal system 10, a hot nitrogen inlet 11 and a non-condensed steam discharge mechanism 12, wherein an output end of the raw material busbar 1 is fixedly connected with an input end of the boron trichloride adsorption system 2, and the hot nitrogen inlet 11 is fixedly connected with another input end of the boron trichloride adsorption system 2;
here, referring to fig. 2, the raw material bus bar 1 includes a first electronic scale 101, a first gas cylinder 102 is disposed at an upper end of the first electronic scale 101, and an electric heating strip 103 is disposed at an output end of the first gas cylinder 102;
and the first gas storage cylinder 102 has an internal gas pressure of 0.2MPa and a heating temperature of 60-80 ℃ at an ambient temperature of 30 ℃.
Referring to fig. 1, the boron trichloride adsorption system 2 is divided into two output ends, wherein the output end of one boron trichloride adsorption system 2 is fixedly connected with the input end of the filter 3, and the output end of the other boron trichloride adsorption system 2 is fixedly connected with the input end of the tail gas removing system 10;
here, the precision of the filter 3 is 0.1 micron;
in detail, please refer to fig. 3, the boron trichloride adsorption system 2 includes a high temperature furnace 201, a coil cooler 202 and two adsorbers 203, the high temperature furnace 201, the coil cooler 202 and the two adsorbers 203 are sequentially connected in series, and the high temperature furnace 201 and the two adsorbers 203 are respectively provided with an output pipe which is sequentially connected in series, and the output pipe is fixedly connected with the tail gas removal system 10;
specifically, the cold source of the coil cooler 202 is refrigerating fluid with the temperature of-10 ℃, and the cooling temperature is-10 ℃;
the inside of the adsorber 203 is provided with an adsorbent, and the adsorbent at least consists of one or more of activated carbon and molecular sieve;
referring to fig. 1, the output end of the filter 3 is fixedly connected with the input end of the rectifying tower 4, the output end of the top of the rectifying tower 4 is fixedly connected with the input end of the liquefier 5, and the output end of the bottom of the rectifying tower 4 is fixedly connected with the input end of the recovery storage mechanism 7;
the top of the rectifying tower 4 is provided with a condenser, the condenser penetrates through the rectifying tower 4 and is connected with the liquefier 5, the condensing temperature is-15 ℃, the bottom of the rectifying tower 4 is provided with a reboiler, the heating temperature is 60-80 ℃, and the heat-conducting oil heating device is mature prior art and is not described in detail in the technical scheme;
here, the heat source of the reboiler at the bottom of the rectifying tower 4 is heat conducting oil, and the cold source of the condenser at the top is refrigerating fluid;
the liquefiers 5 are provided with two output ends, wherein the output end of one liquefier 5 is connected with the non-condensed steam discharge mechanism 12 and the regenerated gas output end of the boron trichloride adsorption system 2 in parallel, and the finished product output end of the other liquefier 5 is connected with the finished product storage mechanism 6 and the recovery storage mechanism 7 in parallel;
the finished product storage mechanism 6 and the recovery storage mechanism 7 are arranged at a position 1.5M away from the ground;
the output end of the finished product storage mechanism 6 is fixedly connected with the input end of the finished product filling mechanism 9, and the output end of the recovery storage mechanism 7 is fixedly connected with the input end of the recovery filling mechanism 8.
One specific application of this embodiment is: when the device is used, boron trichloride in the first gas storage steel cylinder 102 is heated through the electric heating belt 103, when the boron trichloride is heated to 60-80 ℃, the boron trichloride is vaporized and then enters the high-temperature furnace 201, phosgene contained in the boron trichloride raw material is decomposed at high temperature (250 ℃), then the boron trichloride raw material is cooled to normal temperature through the coil cooler 202 and then sequentially enters the two adsorbers 203, impurities such as carbon dioxide, chlorine, trichlorosilane and silicon tetrachloride contained in the boron trichloride are adsorbed through activated carbon and molecular sieves in the adsorbers 203, and the adsorbed impurities such as carbon dioxide, chlorine, trichlorosilane and silicon tetrachloride enter the tail gas removal system 10 for treatment;
the boron trichloride adsorbed by the adsorber 203 is filtered by the filter 3, solid particles carried by the boron trichloride adsorption system 2 and particles contained in the raw material are filtered, and the filtered boron trichloride enters the rectifying tower 4;
after boron trichloride enters a rectifying tower 4 through a filter 3, stopping collecting boron trichloride when the liquid level of a reboiler at the bottom of the rectifying tower 4 reaches 3/4 liquid level, and stopping feeding;
the working temperature in the rectifying tower 4 is 35-40 ℃, the pressure is 0.1-0.2 MPa, boron trichloride and heavy component impurities with boiling points higher than that of the boron trichloride are liquefied to the bottom of the rectifying tower 4 at the condensation temperature of a condenser, and light components with boiling points lower than that of the boron trichloride are gathered at the top end in the rectifying tower 4 in the continuous heat exchange process;
after the rectification is finished, opening the recovery and storage mechanism 7, and collecting the industrial boron trichloride and heavy component impurities in the rectifying tower 4 in the recovery and storage mechanism 7;
when the heavy component impurity content in the rectifying tower 4 is qualified, the heavy component is a qualified product, the output end at the top of the rectifying tower 4 is opened, the product enters the liquefier 5, the gaseous product is liquefied into a liquid state by the liquefier 5, the finished product storage mechanism 6 is opened, and the boron trichloride finished product enters the finished product storage mechanism 6;
when the heavy component impurity content in the rectifying tower 4 is unqualified, stopping the finished product collecting process, continuing to perform rectifying treatment, and if the heavy component impurity content is unqualified all the time, opening the output end at the bottom of the rectifying tower 4, and enabling the unqualified product in the rectifying tower 4 to enter the recovery storage mechanism 7;
when the finished product filling mechanism 9 is filled, a liquid boron trichloride finished product in the finished product storage mechanism 6 at the output end of the finished product storage mechanism 6 is opened and enters the finished product filling mechanism 9 through pressure difference (a high-purity helium interface at the top of the finished product storage mechanism 6 is opened, and the pressure of the high-purity helium is 0.6-0.8 MPa) and high potential difference, so that the filling work of the finished product filling mechanism 9 is completed;
when the recovery filling mechanism 8 is filled, the output end of the recovery storage mechanism 7 is opened, and the boron trichloride gas product in the recovery storage mechanism 7 enters the recovery filling mechanism 8 through the pressure difference (meanwhile, the high-purity helium gas interface at the top of the recovery storage mechanism 7 is opened, and the pressure of the high-purity helium gas is 0.6-0.8 MPa) and the high level difference, so that the filling work of the recovery filling mechanism 8 is completed.
In conclusion, the invention can better purify boron trichloride through the matching of all accessories to obtain high-purity boron trichloride, can automatically recover unqualified boron trichloride, reduces the production cost, ensures the continuity of the purification process by one-step forming of the purification process, avoids the influence of external impurities on the boron trichloride, ensures the purity of the boron trichloride, is easy to operate, has higher efficiency and is suitable for mass popularization.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (10)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110827964.3A CN113582192A (en) | 2021-07-22 | 2021-07-22 | Boron trichloride purification device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110827964.3A CN113582192A (en) | 2021-07-22 | 2021-07-22 | Boron trichloride purification device |
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| Publication Number | Publication Date |
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| CN113582192A true CN113582192A (en) | 2021-11-02 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202110827964.3A Pending CN113582192A (en) | 2021-07-22 | 2021-07-22 | Boron trichloride purification device |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115571892A (en) * | 2022-10-25 | 2023-01-06 | 中船(邯郸)派瑞特种气体股份有限公司 | Purification method of electronic-grade boron trichloride |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105731481A (en) * | 2014-12-12 | 2016-07-06 | 广东先导稀材股份有限公司 | Method and equipment for purifying boron trichloride |
| CN211847167U (en) * | 2020-03-09 | 2020-11-03 | 安徽艾佩科电子材料有限公司 | Device for preparing high-purity boron trichloride |
-
2021
- 2021-07-22 CN CN202110827964.3A patent/CN113582192A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105731481A (en) * | 2014-12-12 | 2016-07-06 | 广东先导稀材股份有限公司 | Method and equipment for purifying boron trichloride |
| CN211847167U (en) * | 2020-03-09 | 2020-11-03 | 安徽艾佩科电子材料有限公司 | Device for preparing high-purity boron trichloride |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115571892A (en) * | 2022-10-25 | 2023-01-06 | 中船(邯郸)派瑞特种气体股份有限公司 | Purification method of electronic-grade boron trichloride |
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