CN212893907U - Sodium hydride safety production equipment - Google Patents
Sodium hydride safety production equipment Download PDFInfo
- Publication number
- CN212893907U CN212893907U CN202021090998.6U CN202021090998U CN212893907U CN 212893907 U CN212893907 U CN 212893907U CN 202021090998 U CN202021090998 U CN 202021090998U CN 212893907 U CN212893907 U CN 212893907U
- Authority
- CN
- China
- Prior art keywords
- kettle
- paraffin oil
- communicated
- metering tank
- inner cavity
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The utility model discloses sodium hydride safety production equipment, which comprises a fresh paraffin oil metering tank, a metal sodium melting kettle, a hydrogenation kettle, a recovered paraffin oil metering tank, a cooling kettle, a closed filter, a mother liquor collecting tank and a lead-out pump; a liquid outlet of the fresh paraffin oil metering tank is communicated with an inner cavity of the sodium metal melting kettle, a metal inlet is arranged on the sodium metal melting kettle, and a liquid outlet of the sodium metal melting kettle is communicated with an inner cavity of the hydrogenation kettle; the hydrogenation kettle is provided with a hydrogen inlet; the liquid outlet of the recovered paraffin oil metering tank is provided with two branches, wherein one branch is communicated with the inner cavity of the recovered paraffin oil metering tank, and the other branch is communicated with the inner cavity of the cooling kettle; the liquid outlet of the hydrogenation kettle is communicated with the inner cavity of the cooling kettle; and a liquid guide outlet of the cooling kettle is communicated with a liquid inlet of the reuse paraffin oil metering tank sequentially through the closed filter, the mother liquid collecting tank and the guide pump. The utility model discloses how to simplify and throw the material process, reach safety in production purpose technical problem.
Description
Technical Field
The utility model relates to a sodium hydride safety production equipment.
Background
Sodium hydride, chemical formula NaH, is an inorganic salt. In organic synthesis, sodium hydride is mainly used as a strong base. Sodium hydride is a typical representative of salt-type hydrides, i.e., it is composed of Na + and H-, unlike molecular-type hydrides of borane, methane, ammonia and water. Sodium hydride is insoluble in organic solvents and soluble in molten metal sodium, so almost all of the reactions associated with sodium hydride occur on solid surfaces.
Sodium hydride can be formed by combining hydrogen and sodium at elevated temperatures. Pure sodium hydride is colorless, however, sodium hydride is generally produced in a somewhat gray color. Like lithium hydride, potassium hydride, rubidium hydride, and cesium hydride, sodium hydride adopts a sodium chloride type structure, with each Na + surrounded by six H "to form an octahedron.
Sodium hydride is a strong base that is widely used in organic synthesis. It can abstract protons from many compounds to produce the corresponding sodium compound. Typical examples are: alcohols, phenols, pyrazoles, and thiols, and the like.
Sodium hydride is most commonly used for deprotonation of 1, 3-dicarbonyl compounds, maleates and similar compounds, and the corresponding sodium compound can be alkylated to produce a wide variety of organic compounds. The corresponding reactions are seen in Dieckmann condensation, Stobbe condensation, Darzens condensation and Claisen condensation. Dimethyl sulfoxide is a commonly used solvent.
Sodium hydride is also used in the synthesis of thioylides to effect conversion of ketones to epoxides. Sodium hydride allows the synthesis of dithioiodophorosphinates, a field of particular interest in acetylacetone complexes. Sodium hydride is less useful as a reducing agent because the negative hydrogen is too small to overlap well with other orbitals. However, sodium hydride can reduce Si-Si bonds and S-S bonds.
The production method in the general production process comprises the following steps: adding fresh paraffin oil and recycled paraffin oil into a hydrogenation kettle, and starting heating and stirring. When the temperature in the kettle rises to 140 ℃, stopping heating and stirring, and completely replacing the air in the kettle by nitrogen. And adding weighed metal sodium, and closing a feeding port after the adding is finished. After the reaction kettle is vacuumized, nitrogen is filled into the reaction kettle for replacement to normal pressure, and the nitrogen is replaced for three times. After the nitrogen replacement is finished, the vacuum is pulled again, then the hydrogen is filled to the normal pressure, the hydrogen filling is stopped, and the hydrogen replacement is carried out twice. After the replacement gas is finished, the reaction kettle is heated and stirred. Opening a hydrogen valve, introducing hydrogen into the kettle, and keeping the pressure of the hydrogen in the kettle at 0.09 MPa. The reaction temperature is controlled to be 260-280 ℃, the reaction is carried out until no hydrogen is absorbed, and the reaction time is about 4 hours. And keeping the pressure for half an hour after the reaction is finished. Then cooling, crystallizing and filtering to obtain a filter cake which is a mixture of sodium hydride and paraffin oil and contains 60-65% of sodium hydride. The filter cake is the product, and is packaged by a plastic bag and is arranged in an iron barrel. The filtered mother liquor is recycled.
The filtered mother liquor contains a large amount of paraffin oil and sodium hydride which is not precipitated, if the filtered mother liquor is treated as residual liquid, the treatment cost is too high, great waste is caused, and common enterprises recycle the filtered mother liquor, but in the recycling process, the filtered mother liquor contains the sodium hydride product, nitrogen protection is not obtained in the heating process, and the filtered mother liquor is fed at high temperature, so that the filtered mother liquor is easy to splash and generates danger.
SUMMERY OF THE UTILITY MODEL
The utility model provides a sodium hydride safety production equipment solves and how to simplify and throws the material process, reaches safety in production purpose technical problem.
The sodium hydride safety production equipment comprises a fresh paraffin oil metering tank, a metal sodium melting kettle, a hydrogenation kettle, a recovered paraffin oil metering tank, a cooling kettle, a closed filter, a mother liquor collecting tank and a lead-out pump; a liquid outlet of the fresh paraffin oil metering tank is communicated with an inner cavity of the sodium metal melting kettle, a metal inlet is arranged on the sodium metal melting kettle, and a liquid outlet of the sodium metal melting kettle is communicated with an inner cavity of the hydrogenation kettle; the hydrogenation kettle is provided with a hydrogen inlet; the liquid outlet of the recovered paraffin oil metering tank is provided with two branches, wherein one branch is communicated with the inner cavity of the recovered paraffin oil metering tank, and the other branch is communicated with the inner cavity of the cooling kettle; the liquid outlet of the hydrogenation kettle is communicated with the inner cavity of the cooling kettle; and a liquid guide outlet of the cooling kettle is communicated with a liquid inlet of the reuse paraffin oil metering tank sequentially through the closed filter, the mother liquid collecting tank and the guide pump.
The outer side of the hydrogenation kettle is provided with a heat exchange jacket.
And a heat exchange jacket is arranged on the outer side of the cooling kettle.
The closed filter is a plate-type closed filter.
The utility model has the advantages that:
1. the volume of the sodium metal melting kettle is small, the sodium metal adding is convenient, and the whole process of the temperature rising process is protected by nitrogen, so that the production safety is guaranteed.
2. The paraffin oil is recycled and directly recycled, so that the production cost is greatly reduced, and the heating process is not dangerous.
3. The hydrogenation kettle and the cooling kettle respectively use heat conduction oil and cold conduction oil, so that the equipment safety is improved, and the production efficiency is improved.
4. The whole process is simple in process and good in safety control.
Drawings
Fig. 1 is a schematic structural diagram of the present invention;
in the figure, 1, a metal sodium melting kettle, 2, a fresh paraffin oil metering tank, 3, a hydrogenation kettle, 4, a recycled paraffin oil metering tank, 5, a cooling kettle, 6, a closed filter, 7, a mother liquid collecting pool and 8, a lead-out pump are arranged.
Detailed Description
Referring to fig. 1, the sodium hydride safety production apparatus in the figure includes a sodium metal melting kettle 1, a fresh paraffin oil metering tank 2, a hydrogenation kettle 3, a recycled paraffin oil metering tank 4, a cooling kettle 5, a closed filter 6, a mother liquor collecting tank 7, and a lead-out pump 8. Metallic sodium melting kettle 1 is used for the melting of metallic sodium, fresh paraffin oil metering tank 2 is used for leading-in fresh paraffin oil, hydrogenation cauldron 3 is used for the reaction of metallic sodium and hydrogen, retrieval and utilization paraffin oil metering tank 4 is used for leading-in retrieval and utilization paraffin oil to hydrogenation cauldron 3, cooling kettle 5 is used for cooling off the reaction product, airtight filter 6 is used for filtering the reaction product, mother liquor collecting tank 7 is used for collecting the mother liquor that produces after the reaction, export pump 8 and be used for pouring the paraffin oil of retrieving back to retrieval and utilization paraffin oil metering tank 4. The components are all existing components, the innovation point of the scheme is that the design of product production is completed by the connection relation of the components, corresponding valves are designed among the components, and the existing conventional components such as a material conveying pump are added according to needs.
The connection relation of the components is as follows:
the liquid outlet of the fresh paraffin oil metering tank 2 is communicated with the inner cavity of the sodium metal melting kettle 1, so that fresh paraffin oil can be conveniently introduced. The metal sodium melting kettle 1 is provided with a metal input port so as to be convenient for inputting metal sodium. The liquid outlet of the metal sodium melting kettle 1 is communicated with the inner cavity of the hydrogenation kettle 3, so that the mixture of the molten sodium and the paraffin oil can be conveniently led in. The hydrogenation kettle 3 is provided with a hydrogen inlet for introducing hydrogen. The liquid outlet of the recovered paraffin oil metering tank 2 is provided with two branches, wherein one branch is communicated with the inner cavity of the recovered paraffin oil metering tank 4, and the other branch is communicated with the inner cavity of the cooling kettle 5; the recovered paraffin oil was then introduced into the kettle. The liquid outlet of the hydrogenation kettle 3 is communicated with the inner cavity of the cooling kettle 5, so that the synthesized sodium hydride is introduced into the cooling kettle 5 to be cooled. The liquid outlet of the cooling kettle 5 is communicated with the liquid inlet of the reuse paraffin oil metering tank 4 through a closed filter 6, a mother liquid collecting tank 7 and a discharge pump 8 in sequence, so that the reacted paraffin oil is recycled. Understanding the above connection relationships, such as communication or connection, will be understood by those skilled in the art from the description of the embodiment and the representation in fig. 1, and the embodiment expressed by the present idea will be clearly understood by those skilled in the art from the description of the embodiment and the representation in fig. 1.
The operation process and principle of the scheme are as follows:
check if the sodium metal melting kettle 1 is clean and all valves are closed. And (3) opening an emptying valve of the sodium metal melting kettle 1, putting 104.2kg of paraffin oil into the sodium metal melting kettle 1 from the fresh paraffin oil metering tank 2, and closing the valve after the material is put. Firstly, replacing air in the kettle completely with nitrogen, adding 151.6kg of sodium metal, closing a feeding port after the feeding is finished, vacuumizing the reaction kettle, filling nitrogen for replacing to normal pressure, replacing for three times, opening a jacket heat-conducting oil valve of the reaction kettle, heating and stirring, and stopping heating after the sodium metal is molten.
Checking whether the hydrogenation kettle 3 is clean and whether all valves are closed, opening a emptying valve of the hydrogenation kettle 3, putting 596.8kg of recycled paraffin oil into the hydrogenation kettle 3 from the recycled paraffin oil metering tank 4, and closing the valves after emptying. The air in the hydrogenation reactor 3 was purged with nitrogen. And opening a heat conduction oil valve of a heat exchange jacket of the hydrogenation kettle 3, heating and stirring, and then adding the mixture material in the metal sodium melting kettle 1.
After the feeding is finished, vacuumizing, filling hydrogen to be more than normal pressure, stopping introducing the hydrogen, replacing the hydrogen twice, carefully checking the mechanical sealing performance of a feeding hole and other related parts while replacing the air, and ensuring that the air discharging speed is slow and uniform to prevent the hydrogen pipe from being blocked due to the fact that the material enters a hydrogen pipeline. After the replacement gas was completed, the hydrogenation vessel 3 was heated and stirred. Opening a hydrogen valve, introducing about 9.8kg of hydrogen into the kettle, keeping the pressure of the hydrogen in the kettle at 0.09MPa, controlling the reaction temperature at 260-280 ℃, reacting for about 4 hours until no hydrogen is absorbed, and keeping the pressure for half an hour after the reaction is finished.
The cooling vessel 5 was checked for cleanliness and the vent reflux valve was opened. The cooling kettle 5 feed valve was opened. After the pressure of the hydrogenation kettle 3 is maintained, the stirring speed is reduced, a hydrogen valve of the reaction cylinder is closed in advance, an empty valve is opened, and hydrogen is exhausted. Opening a nitrogen valve, keeping the pressure of 0.05MPa by using nitrogen, and putting the feed liquid into a cooling kettle 5. After pressing, adding 50L of paraffin oil into the hydrogenation kettle 3 for cleaning, putting the cleaning solution into the cooling kettle 5, starting the cooling kettle 5 for stirring, introducing cold oil such as cold heat-conducting oil into the jacket, and cooling the material liquid to below 60 ℃.
And (3) checking whether the sealed filter 6 is dry and clean in advance, opening a bottom valve of the cooling kettle 5, pumping the feed liquid into the sealed filter 6, guiding the mother liquid to a mother liquid collecting tank 7 after the feed liquid is filtered by the sealed filter 6, and keeping the filter cake in the sealed filter 6. After the pumping is finished, a small amount of paraffin oil is placed in the cooling kettle 5 for washing, the paraffin oil is pumped into the closed filter 6, and the product in the closed filter 6 is dried by nitrogen. After the filter pressing is finished, the nitrogen valve of the cooling kettle 5 is closed, and the discharge valve of the cooling kettle 5 is closed. And opening the closed filter 6 for discharging, wherein the filter cake is a mixture of sodium hydride and paraffin oil, contains 60-65% of sodium hydride, and is a product, and the filter cake is packaged by a plastic bag and is arranged in an iron bucket. And the mother liquor in the mother liquor collecting tank 7 is pumped into the recycled paraffin oil metering tank 4 by a lead-out pump 8.
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the above description, in combination with the drawings in the embodiments of the present invention, clearly and completely describes the technical solutions in the embodiments of the present invention, and obviously, the described embodiments are some embodiments of the present invention, not all embodiments. The components of embodiments of the present invention, as generally described and illustrated in the figures herein, may be arranged and designed in a wide variety of different configurations.
Thus, the above detailed description of the embodiments of the invention provided in the accompanying drawings is not intended to limit the scope of the invention as claimed, but is merely representative of selected embodiments of the invention. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative efforts belong to the protection scope of the present invention.
Claims (4)
1. The sodium hydride safety production equipment is characterized in that: the system comprises a fresh paraffin oil metering tank, a sodium metal melting kettle, a hydrogenation kettle, a recovered paraffin oil metering tank, a cooling kettle, a closed filter, a mother liquor collecting pool and a lead-out pump; a liquid outlet of the fresh paraffin oil metering tank is communicated with an inner cavity of the sodium metal melting kettle, a metal inlet is arranged on the sodium metal melting kettle, and a liquid outlet of the sodium metal melting kettle is communicated with an inner cavity of the hydrogenation kettle; the hydrogenation kettle is provided with a hydrogen inlet; the liquid outlet of the recovered paraffin oil metering tank is provided with two branches, wherein one branch is communicated with the inner cavity of the recovered paraffin oil metering tank, and the other branch is communicated with the inner cavity of the cooling kettle; the liquid outlet of the hydrogenation kettle is communicated with the inner cavity of the cooling kettle; and a liquid guide outlet of the cooling kettle is communicated with a liquid inlet of the reuse paraffin oil metering tank sequentially through the closed filter, the mother liquid collecting tank and the guide pump.
2. The sodium hydride safety production apparatus according to claim 1, characterized in that: the outer side of the hydrogenation kettle is provided with a heat exchange jacket.
3. The sodium hydride safety production apparatus according to claim 1, characterized in that: and a heat exchange jacket is arranged on the outer side of the cooling kettle.
4. The sodium hydride safety production apparatus according to claim 1, characterized in that: the closed filter is a plate-type closed filter.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202021090998.6U CN212893907U (en) | 2020-06-15 | 2020-06-15 | Sodium hydride safety production equipment |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202021090998.6U CN212893907U (en) | 2020-06-15 | 2020-06-15 | Sodium hydride safety production equipment |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN212893907U true CN212893907U (en) | 2021-04-06 |
Family
ID=75277119
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202021090998.6U Active CN212893907U (en) | 2020-06-15 | 2020-06-15 | Sodium hydride safety production equipment |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN212893907U (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113457577A (en) * | 2021-07-06 | 2021-10-01 | 淄博胜赢化工有限公司 | Raw material mixing and melting device for producing p-tert-butyl catechol and use method thereof |
-
2020
- 2020-06-15 CN CN202021090998.6U patent/CN212893907U/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113457577A (en) * | 2021-07-06 | 2021-10-01 | 淄博胜赢化工有限公司 | Raw material mixing and melting device for producing p-tert-butyl catechol and use method thereof |
| CN113457577B (en) * | 2021-07-06 | 2023-06-06 | 淄博胜赢化工有限公司 | Raw material mixing and melting device for producing p-tert-butyl catechol and application method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN212893907U (en) | Sodium hydride safety production equipment | |
| CN103922285B (en) | A kind of synthetic method of lithium borohydride | |
| CN101830918B (en) | Synthetic method of polynitrogen azole zinc/cadmium framework material | |
| CN102343230A (en) | Mixer for preparing lithium-ion battery electrolyte | |
| CN101805364B (en) | Producing method of triethyl aluminium | |
| CN110204419A (en) | A kind of method of energy-saving and environment-friendly toluene derivative air oxidation synthesizing benzoic alcohol (aldehyde, acid) derivative | |
| CN101805360B (en) | Novel synthesis process of lithium alkyl | |
| CN201404802Y (en) | Synthetic reaction kettle | |
| CN104245570A (en) | Method for utilizing fluoroalkyl iodide | |
| CN113842857A (en) | System and method for preparing acylation liquid | |
| CN111363922B (en) | Vacuum distillation device and process for continuously recycling metal sodium and calcium from sodium slag | |
| CN109970030A (en) | A kind of synthesis technology of α-three aluminum hydride | |
| CN215160999U (en) | Metal hydrogen production circulation system | |
| CN105439990A (en) | Method for recovering ether solvents from Grignard reaction residues | |
| CN210814655U (en) | Tail gas treatment system of fluorescent brightener sulfur oxidation coupling reaction section | |
| CN212215517U (en) | Energy-saving reaction kettle for producing sodium borohydride | |
| CN212560390U (en) | Vacuum distillation device for continuously recovering metal sodium and calcium from sodium slag | |
| CN210826003U (en) | High-yield post-treatment system for sulfur oxidation coupling reaction of fluorescent whitening agent | |
| CN103304376A (en) | Clean production process of alkyne diol serial products | |
| CN208684412U (en) | A kind of preparation facilities of phosphine gas | |
| CN108129296B (en) | Device and method for preparing aromatic acid by direct carboxylation of carbon dioxide | |
| CN106000451B (en) | A kind of Cyclamine catalyst and preparation method thereof | |
| CN210825420U (en) | Sodium sulfide recovery system for producing fluorescent whitening agent | |
| CN218516671U (en) | Promote device of synthetic water-reducing agent macromonomer catalyst efficiency | |
| CN219002986U (en) | Automatic change reaction absorbing device of continuous production ruthenium trichloride |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| GR01 | Patent grant | ||
| GR01 | Patent grant |