CN111137861A - Preparation process of sodium borohydride - Google Patents
Preparation process of sodium borohydride Download PDFInfo
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- CN111137861A CN111137861A CN201911421872.4A CN201911421872A CN111137861A CN 111137861 A CN111137861 A CN 111137861A CN 201911421872 A CN201911421872 A CN 201911421872A CN 111137861 A CN111137861 A CN 111137861A
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- raw materials
- sodium borohydride
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- reaction kettles
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B6/00—Hydrides of metals including fully or partially hydrided metals, alloys or intermetallic compounds ; Compounds containing at least one metal-hydrogen bond, e.g. (GeH3)2S, SiH GeH; Monoborane or diborane; Addition complexes thereof
- C01B6/06—Hydrides of aluminium, gallium, indium, thallium, germanium, tin, lead, arsenic, antimony, bismuth or polonium; Monoborane; Diborane; Addition complexes thereof
- C01B6/10—Monoborane; Diborane; Addition complexes thereof
- C01B6/13—Addition complexes of monoborane or diborane, e.g. with phosphine, arsine or hydrazine
- C01B6/15—Metal borohydrides; Addition complexes thereof
- C01B6/19—Preparation from other compounds of boron
- C01B6/21—Preparation of borohydrides of alkali metals, alkaline earth metals, magnesium or beryllium; Addition complexes thereof, e.g. LiBH4.2N2H4, NaB2H7
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention discloses a preparation process of sodium borohydride, which comprises the following raw materials and preparation steps as well as two reaction kettles, wherein the raw materials are as follows: including boric acid and methanol; the preparation steps are as follows: the method comprises the steps of raw material mixing, raw material extraction, water-liquid phase separation and mother liquor extraction, wherein the two reaction kettles are communicated through a circulating reflux pipeline, and compared with the prior art, the method has the following beneficial effects: according to the preparation process of the sodium borohydride, two reaction kettles are adopted during use, when the reaction kettles need to be replaced, raw materials can circularly flow back in the two reaction kettles in the process of preparing the sodium borohydride, the number of the reaction kettles needed for use is reduced, equipment investment is low, energy consumption is reduced, the possibility of error in the batching process due to more workers is reduced due to less operators, the product quality is stable, and the processing cost of the sodium borohydride is greatly reduced.
Description
Technical Field
The invention discloses a preparation process of sodium borohydride, belonging to the technical field of sodium borohydride preparation.
Background
Sodium borohydride is stable at normal temperature and pressure. The sodium borohydride alkaline solution is brownish yellow, one of the most commonly used reducing agents is stable to moisture and oxygen in the air, the operation and the treatment are easy, and the sodium borohydride alkaline solution is suitable for industrial scale.
The existing sodium borohydride preparation process needs a plurality of reaction kettles to be used simultaneously when in operation, needs a plurality of people to operate the sodium borohydride preparation process simultaneously, and enables the batching process technology not to be easily mastered due to more personnel when in multi-person operation, thereby enabling the quality of products to be unstable and causing the processing cost of the sodium borohydride to be higher.
Disclosure of Invention
The invention aims to solve the technical problems that in the existing sodium borohydride preparation process, a plurality of reaction kettles are required to be used simultaneously, a plurality of people are required to operate the sodium borohydride preparation process simultaneously, and the processing cost of the sodium borohydride is high due to unstable product quality because the batching process is difficult to master because more people are required during the operation of the plurality of people, and the preparation process of the sodium borohydride is provided, so that the problems are solved.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation process of sodium borohydride comprises the following steps of raw materials and preparation steps as well as two reaction kettles, wherein the raw materials are as follows: including boric acid and methanol; the preparation steps are as follows: comprises mixing raw materials, extracting raw materials, separating water and liquid phases, and extracting mother liquor.
Preferably, the two reaction kettles are communicated through a circulating reflux pipeline.
Preferably, the mixed raw materials are prepared by putting boric acid and methanol into one of the reaction kettles through a feeding device, and starting a mixing structure to mix the boric acid and the methanol.
Preferably, the raw material extraction is performed by adding an extractant into the reaction kettle, reacting the mixture of boric acid and methanol in the reaction kettle by the enhanced separation effect of the extractant, and separating each component according to the volatility of the component.
Preferably, the aqueous liquid phase separation comprises adding a small amount of sulfuric acid into the reaction kettle, and absorbing water for the internal raw materials through the water absorption effect of the sulfuric acid, so as to reduce the water in the raw materials.
Preferably, after the aqueous liquid phase separation is completed, the raw material is transferred to another reaction vessel through a circulation reflux line, and the circulation reflux line is closed after the transfer is completed.
Preferably, the mother liquor extraction is to start a corresponding reaction kettle, so that the raw materials are subjected to high-temperature reaction in the reaction kettle until the sodium borohydride reaction is finished, and then the sodium borohydride can be extracted from the reaction kettle.
Preferably, the reaction kettle can be started to perform heating reaction on the internal raw materials while performing water-liquid phase separation, so that the water in the separated raw materials is evaporated, and meanwhile, hot gas at the top of the reaction kettle is discharged through an exhaust device, so that condensed water is prevented from being generated.
Compared with the prior art, the invention has the following beneficial effects: according to the preparation process of the sodium borohydride, two reaction kettles are adopted during use, when the reaction kettles need to be replaced, raw materials can circularly flow back in the two reaction kettles in the process of preparing the sodium borohydride, the number of the reaction kettles needed for use is reduced, equipment investment is low, energy consumption is reduced, the possibility of error in the batching process due to more workers is reduced due to less operators, the product quality is stable, and the processing cost of the sodium borohydride is greatly reduced.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all 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.
A preparation process of sodium borohydride comprises the following steps of raw materials and preparation steps as well as two reaction kettles, wherein the raw materials are as follows: including boric acid and methanol; the preparation method comprises the following steps: comprises mixing raw materials, extracting raw materials, separating water and liquid phases, and extracting mother liquor.
Wherein, the two reaction kettles are communicated with each other through a circulating reflux pipeline.
The mixed raw materials are that boric acid and methanol are put into one of the reaction kettles through a feeding device, and a mixing structure is started to mix the boric acid and the methanol.
The raw material extraction is to add an extracting agent into a reaction kettle, react a boric acid and methanol mixture in the reaction kettle through the enhanced separation effect of the extracting agent, and separate components according to different component volatility.
Wherein, the water-liquid phase separation comprises the steps of adding a small amount of sulfuric acid into the reaction kettle, and absorbing water for the internal raw materials through the water absorption effect of the sulfuric acid, so as to reduce the water in the raw materials.
Wherein, after the water-liquid phase separation is finished, the raw materials are conveyed into the other reaction kettle through the circulating reflux pipeline, and the circulating reflux pipeline is closed after the conveying is finished.
The mother liquor extraction is to start a corresponding reaction kettle, so that the raw materials are subjected to high-temperature reaction in the reaction kettle until the sodium borohydride reaction processing is completed, and then the sodium borohydride can be extracted from the reaction kettle.
Wherein, can start reation kettle and heat the reaction to inside raw materials when carrying out water liquid phase separation, and then the moisture content in the raw materials that will be separated is evaporated, discharges the steam at reation kettle top through exhaust apparatus simultaneously, avoids it to produce the comdenstion water.
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 (8)
1. A preparation process of sodium borohydride is characterized by comprising required raw materials, preparation steps and two reaction kettles, wherein the required raw materials are as follows: including boric acid and methanol; the preparation steps are as follows: comprises mixing raw materials, extracting raw materials, separating water and liquid phases, and extracting mother liquor.
2. The process for preparing sodium borohydride according to claim 1, characterized in that: the two reaction kettles are communicated through a circulating reflux pipeline.
3. The process for preparing sodium borohydride according to claim 1, characterized in that: the mixed raw materials are that boric acid and methanol are put into one of the reaction kettles through a feeding device, and a mixing structure is started to mix the boric acid and the methanol.
4. The process for preparing sodium borohydride according to claim 1, characterized in that: the raw material extraction is to add an extracting agent into a reaction kettle, react a boric acid and methanol mixture in the reaction kettle through the enhanced separation effect of the extracting agent, and separate components according to different component volatility.
5. The process for preparing sodium borohydride according to claim 1, characterized in that: the water-liquid phase separation comprises the steps of adding a small amount of sulfuric acid into the reaction kettle, and absorbing water for the internal raw materials through the water absorption effect of the sulfuric acid, so that the water in the raw materials is reduced.
6. The process according to claim 5, wherein the reaction is carried out in the presence of a solvent selected from the group consisting of: after the water-liquid phase separation is finished, the raw materials are conveyed into the other reaction kettle through a circulating reflux pipeline, and the circulating reflux pipeline is closed after the conveying is finished.
7. The process for preparing sodium borohydride according to claim 1, characterized in that: the mother liquor extraction is to start a corresponding reaction kettle, so that the raw materials are subjected to high-temperature reaction in the reaction kettle until the sodium borohydride reaction processing is finished, and then the sodium borohydride can be extracted from the reaction kettle.
8. The process according to claim 5, wherein the reaction is carried out in the presence of a solvent selected from the group consisting of: can start reation kettle and carry out the heating reaction to inside raw materials when carrying out water liquid phase separation, and then the moisture content in the raw materials that will be separated out is evaporated, discharges the steam at reation kettle top through exhaust apparatus simultaneously, avoids it to produce the comdenstion water.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911421872.4A CN111137861A (en) | 2019-12-31 | 2019-12-31 | Preparation process of sodium borohydride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911421872.4A CN111137861A (en) | 2019-12-31 | 2019-12-31 | Preparation process of sodium borohydride |
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| Publication Number | Publication Date |
|---|---|
| CN111137861A true CN111137861A (en) | 2020-05-12 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911421872.4A Pending CN111137861A (en) | 2019-12-31 | 2019-12-31 | Preparation process of sodium borohydride |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB790164A (en) * | 1955-01-26 | 1958-02-05 | Degussa | Process for the production of sodium and potassium boron hydrides |
| US6433129B1 (en) * | 2000-11-08 | 2002-08-13 | Millennium Cell, Inc. | Compositions and processes for synthesizing borohydride compounds |
| CN101269793A (en) * | 2008-04-30 | 2008-09-24 | 复旦大学 | Method for preparing sodium borohydride |
| CN201728110U (en) * | 2010-07-15 | 2011-02-02 | 山东国邦药业股份有限公司 | Boron hydrogenation reaction kettle for producing sodium borohydride |
| CN102816178A (en) * | 2012-09-14 | 2012-12-12 | 南通鸿志化工有限公司 | Method and special device for separating trimethyl borate from carbinol mixture |
-
2019
- 2019-12-31 CN CN201911421872.4A patent/CN111137861A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB790164A (en) * | 1955-01-26 | 1958-02-05 | Degussa | Process for the production of sodium and potassium boron hydrides |
| US6433129B1 (en) * | 2000-11-08 | 2002-08-13 | Millennium Cell, Inc. | Compositions and processes for synthesizing borohydride compounds |
| CN101269793A (en) * | 2008-04-30 | 2008-09-24 | 复旦大学 | Method for preparing sodium borohydride |
| CN201728110U (en) * | 2010-07-15 | 2011-02-02 | 山东国邦药业股份有限公司 | Boron hydrogenation reaction kettle for producing sodium borohydride |
| CN102816178A (en) * | 2012-09-14 | 2012-12-12 | 南通鸿志化工有限公司 | Method and special device for separating trimethyl borate from carbinol mixture |
Non-Patent Citations (1)
| Title |
|---|
| 朱洪法等: "硼氢化钠", 《无机化工产品手册》 * |
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Application publication date: 20200512 |
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