CN110627820B - Diborane synthesis system and method thereof - Google Patents
Diborane synthesis system and method thereof Download PDFInfo
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- CN110627820B CN110627820B CN201910910709.8A CN201910910709A CN110627820B CN 110627820 B CN110627820 B CN 110627820B CN 201910910709 A CN201910910709 A CN 201910910709A CN 110627820 B CN110627820 B CN 110627820B
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- C07—ORGANIC CHEMISTRY
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- C07F5/00—Compounds containing elements of Groups 3 or 13 of the Periodic System
- C07F5/02—Boron compounds
- C07F5/027—Organoboranes and organoborohydrides
Abstract
The invention provides a diborane synthesis system and a method thereof, which comprises a reaction kettle, wherein the reaction kettle is provided with an air inlet, a first air outlet and a first charging opening, second charge door and discharge gate, air inlet pipe connection has nitrogen cylinder and gas mixing device, discharge gate pipe connection has the feed inlet of reactor, the reactor is equipped with the discharge gate, dropwise add device and second gas outlet, discharge gate pipe connection has the processing pond, dropwise add device pipe connection has the acid chest, second gas outlet pipe connection has the adsorption tower, adsorption tower top pipe connection has first cold hydrazine, first cold hydrazine pipe connection has first gas collecting tank and liquid collecting tank, be equipped with heating device in the liquid collecting tank, gas outlet pipe connection has the cold hydrazine of second, the cold hydrazine pipe connection of second has the gaseous collecting tank of second, the cold hydrazine of second and liquid collecting tank pipe connection, liquid collecting tank pipe connection has the filling device. The invention has the advantages of high reaction speed, high purification efficiency and the like.
Description
Technical Field
The invention relates to the field of industrial gas production, in particular to a diborane synthesis system and a method thereof.
Background
Diborane is a gas with a boiling point of-92.5 ℃, has the characteristic of strong ignitability, can be used as a propellant of fuel and rocket, is mainly used as a dopant for diffusion and oxidation in semiconductor manufacture in the electronic industry, is widely applied to industries such as semiconductor Integrated Circuits (IC), Liquid Crystal Displays (LCD), semiconductor light-emitting devices (LED) and solar cells (PV), can be used as a mixed gas when a boron-phosphorus-silicon glass insulating film is formed, and can be diluted by using gases such as nitrogen, helium, hydrogen and the like when used as the mixed gas, and can be used after being converted into a stable processed form by using high-grade borane, amine accessories and the like.
In recent years, with the gradual reduction of energy resources such as global petroleum and the like, environmental pollution, the influence of greenhouse effect on climate, the development of clean energy and energy-saving technology in various countries in the world is vigorous, low-carbon economy is focused, under the background, solar cells, semiconductor light-emitting devices and energy-saving technology in China are focused, and under the background, the solar cells, the semiconductor light-emitting devices and related industries in China are rapidly developed, the diborane market for the electronic industry is very wide, the existing diborane preparation device is unreasonable in design, difficult to use, low in extraction purity and high in purification difficulty.
Disclosure of Invention
The invention aims to provide a diborane synthesis system and a method thereof, which have the advantages of high reaction speed, high extraction purity and more adaptability to users.
In order to solve the technical problems, the invention adopts the technical scheme that: the utility model provides a diborane synthesis system, includes reation kettle, reation kettle is equipped with air inlet, first gas outlet, first charge door, second charge door and discharge gate, air inlet pipe connection has nitrogen cylinder and gas mixing arrangement, discharge gate pipe connection has the feed inlet of reactor, the reactor is equipped with discharge gate, dropwise add device and second gas outlet, dropwise add device pipe connection has the acid chest, second gas outlet pipe connection has the adsorption tower, adsorption tower top end pipe connection has first cold hydrazine, first cold hydrazine pipe connection has first gas collecting tank and liquid collecting tank, be equipped with heating device in the liquid collecting tank, gas outlet pipe connection has the cold hydrazine of second, the cold hydrazine of second with liquid collecting tank pipe connection, liquid collecting tank pipe connection has the filling device.
Furthermore, the discharge hole is connected with a treatment pool through a pipeline.
Further, the second cold hydrazine pipeline is connected with a second gas collecting tank.
Further, the liquid collecting tank and the second gas collecting tank are connected with the gas mixing device through pipelines.
A method for synthesizing diborane comprising the steps of:
the method comprises the following steps: introducing inert gas into the reaction kettle for internal environment replacement, ventilating for 10-15min, adding dimethyl ether polyethylene glycol, stirring, adding solid sodium borohydride into the reaction kettle, and continuing stirring to uniformly mix the sodium borohydride and the dimethyl ether polyethylene glycol;
step two: introducing mixed gas of diborane and nitrogen into the reaction kettle in the first step according to the mass ratio of 2:3, wherein the introducing speed of diborane gas is 50g/min, and generating an intermediate;
step three: introducing the intermediate in the second step into a reactor, slowly dropwise adding sulfuric acid into the reactor under the condition of stirring, and collecting reaction gas to obtain diborane crude gas A;
step four: introducing the reaction gas into an adsorption tower, and absorbing sulfide impurities in the reaction gas to obtain diborane crude gas B;
step five: introducing diborane crude gas B in the fourth step into a first cold hydrazine for precooling, and removing small molecular gas in the first cold hydrazine by using a vacuum pump, wherein the small molecular gas is hydrogen in the second step to obtain liquid diborane;
step six: and (4) carrying out endothermic gasification on the liquid diborane in the step five at the temperature of 25-40 ℃ to obtain diborane gas.
Further, the mass ratio of the sodium borohydride to the diborane is 2: 1.
Further, the precooling temperature of the first cold hydrazine in the fifth step is-100 ℃.
And further, introducing the mixed waste gas in the second step into a second cold hydrazine for separation.
Further, the temperature of the reaction kettle is set to be 0-40 ℃.
Further, in the sixth step, the product is mixed with hydrogen in different proportions to prepare diborane mixed gas with a molar concentration of 5-40, and then filling is carried out.
Compared with the prior art, the invention has the advantages and positive effects that:
1. according to the method, the intermediate product is generated by sodium borohydride and diborane, and the intermediate product reacts with the acid to generate diborane, so that the generation of impurities in the production process can be effectively reduced, the overall performance of the whole device is greatly improved, and the requirements of users can be met.
2. According to the invention, impurities in the production process can be effectively removed through the first cold hydrazine, the second cold hydrazine and the adsorption tower, so that 5N-grade diborane can be produced, the overall performance of the whole device is greatly improved, and the requirements of users can be met.
3. The invention can store hydrogen and nitrogen separately, can effectively reduce the input of raw materials, can realize continuous large-scale production, greatly improves the overall performance of the whole device, and can better meet the requirements of users.
Drawings
FIG. 1 is a schematic diagram of the flue gas desulfurization system of the present invention.
In the figure: the device comprises a reaction kettle-1, a nitrogen gas bottle-2, a gas mixing device-3, a reactor-4, a dripping device-5, an acid pool-6, an adsorption tower-7, a first cold hydrazine-8, a first gas collecting tank-9, a liquid collecting tank-10, a heating device-11, a second cold hydrazine-12, a filling device-13, a treatment pool-14 and a second gas collecting tank-15.
Detailed Description
For a better understanding of the present invention, reference is made to the following detailed description and accompanying drawings that illustrate the invention.
Example 1:
as shown in figure 1, a diborane synthesis system comprises a reaction kettle 1, wherein the reaction kettle 1 is provided with an air inlet, a first air outlet, a first feed inlet, a second feed inlet and a discharge outlet, the air inlet is connected with a nitrogen cylinder 2 and a gas mixing device 3 through pipelines, the discharge outlet is connected with a feed inlet of a reactor 4 through a pipeline, the reactor 4 is provided with a discharge outlet, a dripping device 5 and a second air outlet, the discharge outlet is connected with a treatment pool 14 through a pipeline, the dripping device 5 is connected with an acid pool 6 through a pipeline, the second air outlet is connected with an adsorption tower 7 through a pipeline, the top end of the adsorption tower 7 is connected with a first cold hydrazine 8 through a pipeline, the first cold hydrazine 8 is connected with a first gas collection tank 9 and a liquid collection tank 10 through a pipeline, a heating device 11 is arranged in the liquid collection tank 10, the air outlet is connected with a second cold hydrazine 12 through a pipeline, the second cold hydrazine 12 is connected with a second gas collection tank 15, and the second cold hydrazine 12 is connected with the liquid collection tank 10 through a pipeline, the liquid collecting tank 10 is connected with a filling device 13 through a pipeline, and the liquid collecting tank 10 and the second gas collecting tank 15 are both connected with the gas mixing device 3 through a pipeline.
A method for synthesizing diborane comprising the steps of:
the method comprises the following steps: introducing inert gas into the reaction kettle 1 for internal environment replacement, setting the temperature of the reaction kettle 1 to be 0 ℃, ventilating for 10min, adding dimethyl ether polyethylene glycol, stirring, adding solid sodium borohydride into the reaction kettle 1, and continuously stirring to uniformly mix the sodium borohydride and the dimethyl ether polyethylene glycol;
step two: introducing mixed gas of diborane and nitrogen according to the mass ratio of 2:3 into the reaction kettle 1 in the first step, wherein the introduction speed of the diborane gas is 50g/min, the mass ratio of sodium borohydride to diborane is 2:1, generating an intermediate and mixed waste gas, and introducing the mixed waste gas into a second cold hydrazine 12 for separation;
step three: introducing the intermediate in the step two into a reactor 4, slowly dropwise adding sulfuric acid into the reactor 4 under the condition of stirring, and collecting reaction gas to obtain diborane crude gas A;
step four: introducing the reaction gas into an adsorption tower 7, and absorbing sulfide impurities in the reaction gas to obtain diborane crude gas B;
step five: introducing diborane crude gas B in the fourth step into a first cold hydrazine 8 pre-cooled to-100 ℃, and removing small molecular gas in the first cold hydrazine 8 by using a vacuum pump, wherein the small molecular gas is hydrogen in the second step to obtain liquid diborane;
step six: and (5) performing endothermic gasification on the liquid diborane in the step five at 25 ℃ to obtain diborane gas, mixing the diborane gas with hydrogen in different proportions to prepare diborane mixed gas with the molar concentration of 5, and filling.
In the embodiment of the invention, the production method of firstly mixing diborane and sodium borohydride in a certain proportion to generate an intermediate, and then reacting the intermediate with acid to generate diborane again is utilized, so that the generation of other byproducts can be effectively reduced. The improvement according to the production mode can have the characteristic of less byproducts, and the product is collected by adding cold hydrazine, and diborane, nitrogen and the like are recycled to improve the synthesis efficiency of diborane gas. Specifically, the method for producing the diborane by the sodium borohydride and the diborane and reacting the intermediate product with the acid can effectively reduce the generation of impurities in the production process, greatly improve the overall performance of the whole device and meet the requirements of users; in addition, the impurities in the production process can be effectively removed through the first cold hydrazine, the second cold hydrazine and the adsorption tower, so that 5N-grade diborane can be produced, the overall performance of the whole device is greatly improved, and the requirements of users can be met; the invention can store hydrogen and nitrogen separately, can effectively reduce the input of raw materials, can realize continuous large-scale production, greatly improves the overall performance of the whole device, and can better meet the requirements of users.
Example 2:
diborane synthesis system, as in example 1.
A method for synthesizing diborane comprising the steps of:
the method comprises the following steps: introducing inert gas into the reaction kettle 1 for internal environment replacement, setting the temperature of the reaction kettle 1 to be 20 ℃, ventilating for 12min, adding dimethyl ether polyethylene glycol, stirring, adding solid sodium borohydride into the reaction kettle 1, and continuously stirring to uniformly mix the sodium borohydride and the dimethyl ether polyethylene glycol;
step two: introducing mixed gas of diborane and nitrogen according to the mass ratio of 2:3 into the reaction kettle 1 in the first step, wherein the introduction speed of the diborane gas is 50g/min, the mass ratio of sodium borohydride to diborane is 2:1, generating an intermediate and mixed waste gas, and introducing the mixed waste gas into a second cold hydrazine 12 for separation;
step three: introducing the intermediate in the step two into a reactor 4, slowly dropwise adding sulfuric acid into the reactor 4 under the condition of stirring, and collecting reaction gas to obtain diborane crude gas A;
step four: introducing the reaction gas into an adsorption tower 7, and absorbing sulfide impurities in the reaction gas to obtain diborane crude gas B;
step five: introducing diborane crude gas B in the fourth step into a first cold hydrazine 8 pre-cooled to-100 ℃, and removing small molecular gas in the first cold hydrazine 8 by using a vacuum pump, wherein the small molecular gas is hydrogen in the second step to obtain liquid diborane;
step six: and (5) performing endothermic gasification on the liquid diborane in the step five at 32 ℃ to obtain diborane gas, mixing the diborane gas with hydrogen in different proportions to prepare diborane mixed gas with the molar concentration of 27, and filling.
Example 3:
diborane synthesis system, as in example 1.
A method for synthesizing diborane comprising the steps of:
the method comprises the following steps: introducing inert gas into the reaction kettle 1 for internal environment replacement, setting the temperature of the reaction kettle 1 to be 40 ℃, ventilating for 15min, adding dimethyl ether polyethylene glycol, stirring, adding solid sodium borohydride into the reaction kettle 1, and continuously stirring to uniformly mix the sodium borohydride and the dimethyl ether polyethylene glycol;
step two: introducing mixed gas of diborane and nitrogen according to the mass ratio of 2:3 into the reaction kettle 1 in the first step, wherein the introduction speed of the diborane gas is 50g/min, the mass ratio of sodium borohydride to diborane is 2:1, generating an intermediate and mixed waste gas, and introducing the mixed waste gas into a second cold hydrazine 12 for separation;
step three: introducing the intermediate in the step two into a reactor 4, slowly dropwise adding sulfuric acid into the reactor 4 under the condition of stirring, and collecting reaction gas to obtain diborane crude gas A;
step four: introducing the reaction gas into an adsorption tower 7, and absorbing sulfide impurities in the reaction gas to obtain diborane crude gas B;
step five: introducing diborane crude gas B in the fourth step into a first cold hydrazine 8 pre-cooled to-100 ℃, and removing small molecular gas in the first cold hydrazine 8 by using a vacuum pump, wherein the small molecular gas is hydrogen in the second step to obtain liquid diborane;
step six: and D, performing endothermic gasification on the liquid diborane in the step V at 40 ℃ to obtain diborane gas, mixing the diborane gas with hydrogen in different proportions to prepare diborane mixed gas with the molar concentration of 40, and filling.
The embodiments of the present invention have been described in detail, but the description is only for the preferred embodiments of the present invention and should not be construed as limiting the scope of the present invention. All equivalent changes and modifications made within the scope of the present invention should be covered by the present patent.
Claims (8)
1. A diborane synthesis system, comprising: comprises a reaction kettle (1), wherein the reaction kettle (1) is provided with an air inlet, a first air outlet, a first feed inlet, a second feed inlet and a discharge outlet, the air inlet is connected with a nitrogen cylinder (2) and a gas mixing device (3) through a pipeline, the discharge outlet is connected with a feed inlet of a reactor (4) through a pipeline, the reactor (4) is provided with a discharge outlet, a dripping device (5) and a second air outlet, the dripping device (5) is connected with an acid pool (6) through a pipeline, the second air outlet is connected with an adsorption tower (7) through a pipeline, the top end of the adsorption tower (7) is connected with a first cold hydrazine (8) through a pipeline, the first cold hydrazine (8) is connected with a first gas collecting tank (9) and a liquid collecting tank (10) through a pipeline, a heating device (11) is arranged in the liquid collecting tank (10), the first air outlet is connected with a second cold hydrazine (12) through a pipeline, the second cold trap (12) is connected with the liquid collecting tank (10) through a pipeline, and the liquid collecting tank (10) is connected with a filling device (13) through a pipeline; the second cold trap (12) is connected with a second gas collecting tank (15) through a pipeline; the liquid collecting tank (10) and the second gas collecting tank (15) are connected with the gas mixing device (3) through pipelines.
2. A diborane synthesis system according to claim 1, wherein: the discharge hole pipeline is connected with a treatment pool (14).
3. A method for synthesizing diborane is characterized by comprising the following steps: a diborane synthesis system as defined in any one of claims 1 to 2 including the steps of:
the method comprises the following steps: introducing inert gas into the reaction kettle (1) to perform internal environment replacement, ventilating for 10-15min, adding dimethyl ether polyethylene glycol, stirring, adding solid sodium borohydride into the reaction kettle (1), and continuously stirring to uniformly mix the sodium borohydride and the dimethyl ether polyethylene glycol;
step two: introducing mixed gas of diborane and nitrogen according to the mass ratio of 2:3 into the reaction kettle (1) in the step I, wherein the introducing speed of diborane gas is 50g/min, and generating an intermediate;
step three: introducing the intermediate in the second step into a reactor (4), slowly dropwise adding sulfuric acid into the reactor (4) under the condition of stirring, and collecting reaction gas to obtain diborane crude gas A;
step four: introducing the reaction gas into an adsorption tower (7), and absorbing sulfide impurities in the reaction gas to obtain diborane crude gas B;
step five: introducing diborane crude gas B in the fourth step into a first cold hydrazine (8) for precooling, and removing small molecular gas in the first cold hydrazine (8) by using a vacuum pump, wherein the small molecular gas is hydrogen in the third step to obtain liquid diborane;
step six: and (4) carrying out endothermic gasification on the liquid diborane in the step five at the temperature of 25-40 ℃ to obtain diborane gas.
4. A diborane synthesis process according to claim 3, wherein: the mass ratio of the sodium borohydride to the diborane is 2: 1.
5. A diborane synthesis process according to claim 3, wherein: and the precooling temperature of the first cold hydrazine (8) in the fifth step is-100 ℃.
6. A diborane synthesis process according to claim 3, wherein: and introducing the mixed waste gas in the second step into the second cold hydrazine (12) for separation.
7. A diborane synthesis process according to claim 3, wherein: the temperature of the reaction kettle (1) is set to be 0-40 ℃.
8. A diborane synthesis process according to claim 3, wherein: and in the sixth step, the product is mixed with hydrogen in different proportions to prepare diborane mixed gas with the molar concentration of 5-40, and then filling is carried out.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2011162362A (en) * | 2010-02-05 | 2011-08-25 | Sumitomo Seika Chem Co Ltd | Method for producing diborane |
| JP2011162363A (en) * | 2010-02-05 | 2011-08-25 | Sumitomo Seika Chem Co Ltd | Method for producing diborane |
| CN109867262A (en) * | 2019-04-15 | 2019-06-11 | 包头市海科福鹏电子材料有限公司 | A kind of synthesis system and synthetic method of diborane |
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| JP5371050B2 (en) * | 2009-11-06 | 2013-12-18 | 住友精化株式会社 | Production method of diborane |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2011162362A (en) * | 2010-02-05 | 2011-08-25 | Sumitomo Seika Chem Co Ltd | Method for producing diborane |
| JP2011162363A (en) * | 2010-02-05 | 2011-08-25 | Sumitomo Seika Chem Co Ltd | Method for producing diborane |
| CN109867262A (en) * | 2019-04-15 | 2019-06-11 | 包头市海科福鹏电子材料有限公司 | A kind of synthesis system and synthetic method of diborane |
Non-Patent Citations (1)
| Title |
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| "乙硼烷制备和纯化方法的探讨";禹金龙 等;《低温与特气》;20180831;第36卷(第4期);第22-26页 * |
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