CN104649230A - Method for preparing sodium hydride powder - Google Patents

Method for preparing sodium hydride powder Download PDF

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Publication number
CN104649230A
CN104649230A CN201510108603.8A CN201510108603A CN104649230A CN 104649230 A CN104649230 A CN 104649230A CN 201510108603 A CN201510108603 A CN 201510108603A CN 104649230 A CN104649230 A CN 104649230A
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sodium hydride
hydrogen
atomizer
sodium
production technology
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CN201510108603.8A
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CN104649230B (en
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赵燕
郑琦宏
于洁
张盼盼
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Ningxia Shenglan Chemical Environmental Protection Technology Co ltd
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Ningbo University
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Abstract

The invention relates to a method for preparing sodium hydride powder. The method for preparing the sodium hydride powder comprises the following steps: (1) heating hydrogen with the purity higher than 99.9% to 200-350 DEG C; (2) melting metallic sodium, and filtering to remove insoluble impurities, and heating to 150-350 DEG C; (3) introducing molten metallic sodium and hydrogen into an atomizer, wherein the atomizer is arranged at the upper part of a closed reactor, hydrogen is respectively introduced into an inner channel and an outer channel of the atomizer, the molten metallic sodium is introduced into an intermediate channel of the atomizer; and (4) carrying out quick reaction on hydrogen and atomized metallic sodium fogdrops in an external space of a nozzle of the atomizer to generate sodium hydride powder. The method for preparing the sodium hydride powder has the beneficial effects that firstly the problem that sodium hydride is polluted by an organic solvent in the traditional technique is solved, the purity of sodium hydride prepared by adopting the method provided by the invention can reach up to 98% or more, and no organic matter is contained; and secondly, the grain size of the sodium hydride powder is small and can reach up to 30-50 microns.

Description

A kind of sodium hydride raw powder's production technology
Technical field
The invention belongs to Inorganic synthese technical field, relate to a kind of raw powder's production technology, be specifically related to a kind of sodium hydride raw powder's production technology.
Background technology
Sodium hydride is a kind of widely used reductive agent, and common commerical prod is dispersed in (normally kerosene or paraffin) in inert solvent with 25% ~ 50% ratio, also can obtain the product of sodium hydride content 65% through press filtration.This product owing to affecting the application in downstream containing organic solvent, especially when to derived product require higher.In addition, the sodium hydride granularity that this method obtains is comparatively large, active poor.
Chinese patent application (application number: the preparation and the purification process that 02814666.2) disclose a kind of sodium hydride, wherein describe a kind of preparation method of sodium hydride, the sodium hydride granularity that the method obtains less than 20 microns.This method introduces organism in preparation process, in reaction process with metal hydroxidess such as sodium hydroxide for solvent, comprise the impurity such as sodium carbonate unavoidably in therefore obtained sodium hydride.
Summary of the invention
Goal of the invention: the present invention is directed to above-mentioned prior art Problems existing and make improvement, namely the invention discloses a kind of sodium hydride raw powder's production technology.
Technical scheme: a kind of sodium hydride raw powder's production technology, comprises the following steps:
(1), by purity higher than 99.9% hydrogen be warming up to 200 ~ 350 DEG C;
(2), sodium Metal 99.5 melt filteration removed infusibility impurity and be warming up to 150 ~ 350 DEG C;
(3), by sodium Metal 99.5 melt, hydrogen pass into atomizer, atomizer is located at the top of airtight reactor simultaneously, and hydrogen passes into interior passageway and the exterior passage way of atomizer, and sodium Metal 99.5 melt passes into the center-aisle of atomizer;
(4), at the space outerpace of the spout of atomizer, the sodium Metal 99.5 droplet rapid reaction of hydrogen and atomization generates sodium hydride powder.
A kind of preferred version as sodium hydride raw powder's production technology a kind of in the present invention: unreacted hydrogen can again use as raw material after removing sodium hydride by the cyclonic separator of inside reactor after hydrogen gas compressor compression.
A kind of preferred version as sodium hydride raw powder's production technology a kind of in the present invention: adopt metal sintered filter to filter in step (2), the aperture of the filter pore of metal sintered filter is 0.1 micron.
A kind of preferred version as sodium hydride raw powder's production technology a kind of in the present invention: the molar flow entering the hydrogen of shower nozzle in step (3) is 50 ~ 100 times of the molar flow of the sodium Metal 99.5 melt entering shower nozzle.
A kind of preferred version as sodium hydride raw powder's production technology a kind of in the present invention: enter the mol ratio of the hydrogen of interior passageway and the hydrogen of exterior passage way in step (3) for (1 ~ 2): (2 ~ 1).
A kind of preferred version as sodium hydride raw powder's production technology a kind of in the present invention: atomizer is the outer hybrid shower nozzle of triple channel fluid.
Beneficial effect: a kind of sodium hydride raw powder's production technology disclosed by the invention has following beneficial effect:
1, solve sodium hydride in traditional technology and be subject to a difficult problem for organic solvent pollution, the purity of the sodium hydride adopting the present invention to prepare can reach more than 98%, and not containing any organism.
2, the particle diameter of sodium hydride powder is little, can reach 30 ~ 50 microns.
Accompanying drawing explanation
Fig. 1 is the structural representation of atomizer;
Fig. 2 is the schematic flow sheet of a kind of sodium hydride raw powder's production technology disclosed by the invention;
Wherein:
10-exterior passage way 20-center-aisle
30-interior passageway
Embodiment:
Below the specific embodiment of the present invention is described in detail.
Specific embodiment 1
As shown in Figure 2, a kind of sodium hydride raw powder's production technology, comprises the following steps:
(1), by purity higher than 99.9% hydrogen be warming up to 200 DEG C;
(2), sodium Metal 99.5 melt filteration removed infusibility impurity and be warming up to 350 DEG C;
(3), by sodium Metal 99.5 melt, hydrogen pass into atomizer, atomizer is located at the top of airtight reactor simultaneously, and hydrogen passes into interior passageway 30 and the exterior passage way 10 of atomizer, and sodium Metal 99.5 melt passes into the center-aisle 20 of atomizer;
(4), at the space outerpace of the spout of atomizer, the sodium Metal 99.5 droplet rapid reaction of hydrogen and atomization generates sodium hydride powder.Collecting reaction product is analyzed, and product is the sodium hydride powder of 99.2%, and median size is 50 microns.
In the present embodiment, unreacted hydrogen can again use as raw material after removing sodium hydride by the cyclonic separator of inside reactor after hydrogen gas compressor compression.
In the present embodiment, adopt metal sintered filter to filter in step (2), the aperture of the filter pore of metal sintered filter is 0.1 micron.
In the present embodiment, the molar flow entering the hydrogen of shower nozzle in step (3) is 50 times of the molar flow of the sodium Metal 99.5 melt entering shower nozzle.Reaction can be made like this to carry out thoroughly and Sodium Borohydride powder can be separated by cyclonic separator efficiently from air-flow.
In the present embodiment, the mol ratio entering the hydrogen of interior passageway 30 and the hydrogen of exterior passage way 10 in step (3) is 1:2.Reaction can be made like this to carry out thoroughly.
In the present embodiment, atomizer is the outer hybrid shower nozzle (as shown in Figure 1) of triple channel fluid.
Specific embodiment 2
A kind of sodium hydride raw powder's production technology, comprises the following steps:
(1), by purity higher than 99.9% hydrogen be warming up to 350 DEG C;
(2), sodium Metal 99.5 melt filteration removed infusibility impurity and be warming up to 150 DEG C;
(3), by sodium Metal 99.5 melt, hydrogen pass into atomizer, atomizer is located at the top of airtight reactor simultaneously, and hydrogen passes into interior passageway 30 and the exterior passage way 10 of atomizer, and sodium Metal 99.5 melt passes into the center-aisle 20 of atomizer;
(4), at the space outerpace of the spout of atomizer, the sodium Metal 99.5 droplet rapid reaction of hydrogen and atomization generates sodium hydride powder.Collecting reaction product is analyzed, and product is the sodium hydride powder of 99.6%, and median size is 33 microns.
In the present embodiment, unreacted hydrogen can again use as raw material after removing sodium hydride by the cyclonic separator of inside reactor after hydrogen gas compressor compression.
In the present embodiment, adopt metal sintered filter to filter in step (2), the aperture of the filter pore of metal sintered filter is 0.1 micron.
In the present embodiment, the molar flow entering the hydrogen of shower nozzle in step (3) is 100 times of the molar flow of the sodium Metal 99.5 melt entering shower nozzle.Reaction can be made like this to carry out thoroughly and Sodium Borohydride powder can be separated by cyclonic separator efficiently from air-flow.
In the present embodiment, the mol ratio entering the hydrogen of interior passageway 30 and the hydrogen of exterior passage way 10 in step (3) is 1:1.
In the present embodiment, atomizer is the outer hybrid shower nozzle of triple channel fluid.
Specific embodiment 3
A kind of sodium hydride raw powder's production technology, comprises the following steps:
(1), by purity higher than 99.9% hydrogen be warming up to 300 DEG C;
(2), sodium Metal 99.5 melt filteration removed infusibility impurity and be warming up to 300 DEG C;
(3), by sodium Metal 99.5 melt, hydrogen pass into atomizer, atomizer is located at the top of airtight reactor simultaneously, and hydrogen passes into interior passageway 30 and the exterior passage way 10 of atomizer respectively, and sodium Metal 99.5 melt passes into the center-aisle 20 of atomizer;
(4), at the space outerpace of the spout of atomizer, the sodium Metal 99.5 droplet rapid reaction of hydrogen and atomization generates sodium hydride powder.Collecting reaction product is analyzed, and product is the sodium hydride powder of 99.5%, and median size is 45 microns.
In the present embodiment, unreacted hydrogen can again use as raw material after removing sodium hydride by the cyclonic separator of inside reactor after hydrogen gas compressor compression.
In the present embodiment, adopt metal sintered filter to filter in step (2), the aperture of the filter pore of metal sintered filter is 0.1 micron.
In the present embodiment, the molar flow entering the hydrogen of shower nozzle in step (3) is 70 times of the molar flow of the sodium Metal 99.5 melt entering shower nozzle.Reaction can be made like this to carry out thoroughly and Sodium Borohydride powder can be separated by cyclonic separator efficiently from air-flow.
In the present embodiment, the mol ratio entering the hydrogen of interior passageway 30 and the hydrogen of exterior passage way 10 in step (3) is 2:1.
In the present embodiment, atomizer is the outer hybrid shower nozzle of triple channel fluid.
Above embodiments of the present invention are elaborated.But the present invention is not limited to above-mentioned embodiment, in the ken that art those of ordinary skill possesses, can also make a variety of changes under the prerequisite not departing from present inventive concept.

Claims (6)

1. a sodium hydride raw powder's production technology, is characterized in that, comprises the following steps:
(1), by purity higher than 99.9% hydrogen be warming up to 200 ~ 350 DEG C;
(2), sodium Metal 99.5 melt filteration removed infusibility impurity and be warming up to 150 ~ 350 DEG C;
(3), by sodium Metal 99.5 melt, hydrogen pass into atomizer, atomizer is located at the top of airtight reactor simultaneously, and hydrogen passes into interior passageway and the exterior passage way of atomizer, and sodium Metal 99.5 melt passes into the center-aisle of atomizer;
(4), at the space outerpace of the spout of atomizer, the sodium Metal 99.5 droplet rapid reaction of hydrogen and atomization generates sodium hydride powder.
2. a kind of sodium hydride raw powder's production technology as claimed in claim 1, is characterized in that, unreacted hydrogen can again use as raw material after removing sodium hydride by the cyclonic separator of inside reactor after hydrogen gas compressor compression.
3. a kind of sodium hydride raw powder's production technology as claimed in claim 1, is characterized in that, adopt metal sintered filter to filter in step (2), the aperture of the filter pore of metal sintered filter is 0.1 micron.
4. a kind of sodium hydride raw powder's production technology as claimed in claim 1, is characterized in that, the molar flow entering the hydrogen of shower nozzle in step (3) is 50 ~ 100 times of the molar flow of the sodium Metal 99.5 melt entering shower nozzle.
5. a kind of sodium hydride raw powder's production technology as claimed in claim 1, is characterized in that, enters the mol ratio of the hydrogen of interior passageway and the hydrogen of exterior passage way for (1 ~ 2): (2 ~ 1) in step (3).
6. a kind of sodium hydride raw powder's production technology as claimed in claim 1, is characterized in that, atomizer is the outer hybrid shower nozzle of triple channel fluid.
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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104961098A (en) * 2015-06-15 2015-10-07 车荣睿 Preparation method of sodium hydride
WO2019095627A1 (en) * 2017-11-16 2019-05-23 上海镁源动力科技有限公司 Integrated device for preparing magnesium hydride powder and method for preparing magnesium hydride powder
CN110862068A (en) * 2018-08-28 2020-03-06 宁夏佰斯特医药化工有限公司 New process for producing sodium hydride
CN110862102A (en) * 2018-08-28 2020-03-06 宁夏佰斯特医药化工有限公司 Novel process for producing magnesium sulfate
US11813675B2 (en) 2017-11-16 2023-11-14 Shanghai Mg Power Technology Co., Ltd Integrated device for preparing magnesium hydride powder and method for preparing magnesium hydride powder

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2021567A (en) * 1931-11-06 1935-11-19 Du Pont Catalyst and process of hydrogenating organic compounds
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US3535078A (en) * 1967-03-29 1970-10-20 Ceskoslovenska Akademie Ved Process for the production of sodium hydride
CN1876289A (en) * 2006-07-12 2006-12-13 华东理工大学 Method for preparing antimony doped stannic oxide nanometer electricity-conductive powder

Patent Citations (4)

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Publication number Priority date Publication date Assignee Title
US2021567A (en) * 1931-11-06 1935-11-19 Du Pont Catalyst and process of hydrogenating organic compounds
US3222288A (en) * 1960-12-12 1965-12-07 Nat Distillers Chem Corp Process for preparing sodium hydride
US3535078A (en) * 1967-03-29 1970-10-20 Ceskoslovenska Akademie Ved Process for the production of sodium hydride
CN1876289A (en) * 2006-07-12 2006-12-13 华东理工大学 Method for preparing antimony doped stannic oxide nanometer electricity-conductive powder

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Title
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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104961098A (en) * 2015-06-15 2015-10-07 车荣睿 Preparation method of sodium hydride
WO2019095627A1 (en) * 2017-11-16 2019-05-23 上海镁源动力科技有限公司 Integrated device for preparing magnesium hydride powder and method for preparing magnesium hydride powder
US11813675B2 (en) 2017-11-16 2023-11-14 Shanghai Mg Power Technology Co., Ltd Integrated device for preparing magnesium hydride powder and method for preparing magnesium hydride powder
CN110862068A (en) * 2018-08-28 2020-03-06 宁夏佰斯特医药化工有限公司 New process for producing sodium hydride
CN110862102A (en) * 2018-08-28 2020-03-06 宁夏佰斯特医药化工有限公司 Novel process for producing magnesium sulfate

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Effective date of registration: 20191129

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Address before: 315211 Zhejiang Province, Ningbo Jiangbei District Fenghua Road No. 818

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