CN220657537U - Production device for preparing octacarbonyl cobalt - Google Patents
Production device for preparing octacarbonyl cobalt Download PDFInfo
- Publication number
- CN220657537U CN220657537U CN202322294205.2U CN202322294205U CN220657537U CN 220657537 U CN220657537 U CN 220657537U CN 202322294205 U CN202322294205 U CN 202322294205U CN 220657537 U CN220657537 U CN 220657537U
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- CN
- China
- Prior art keywords
- octacarbonyl
- cobalt
- autoclave
- air inlet
- kettle
- Prior art date
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- 229910017052 cobalt Inorganic materials 0.000 title claims abstract description 33
- 239000010941 cobalt Substances 0.000 title claims abstract description 33
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 22
- 238000001914 filtration Methods 0.000 claims abstract description 35
- 238000002425 crystallisation Methods 0.000 claims abstract description 34
- 230000008025 crystallization Effects 0.000 claims abstract description 34
- 239000000706 filtrate Substances 0.000 claims abstract description 29
- 238000001035 drying Methods 0.000 claims abstract description 19
- 239000007788 liquid Substances 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims description 15
- 239000000463 material Substances 0.000 abstract description 11
- 238000003786 synthesis reaction Methods 0.000 abstract description 8
- 230000015572 biosynthetic process Effects 0.000 abstract description 6
- 238000003860 storage Methods 0.000 abstract description 5
- 239000002699 waste material Substances 0.000 abstract description 4
- 238000012858 packaging process Methods 0.000 abstract description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 16
- 229910052757 nitrogen Inorganic materials 0.000 description 8
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 6
- 238000004806 packaging method and process Methods 0.000 description 4
- 229910021503 Cobalt(II) hydroxide Inorganic materials 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- ASKVAEGIVYSGNY-UHFFFAOYSA-L cobalt(ii) hydroxide Chemical compound [OH-].[OH-].[Co+2] ASKVAEGIVYSGNY-UHFFFAOYSA-L 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- UKVIEHSSVKSQBA-UHFFFAOYSA-N methane;palladium Chemical compound C.[Pd] UKVIEHSSVKSQBA-UHFFFAOYSA-N 0.000 description 3
- 239000003208 petroleum Substances 0.000 description 3
- 230000000712 assembly Effects 0.000 description 2
- 238000000429 assembly Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000002902 organometallic compounds Chemical class 0.000 description 1
- -1 oxo aldehydes Chemical class 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000011085 pressure filtration Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The utility model relates to the technical field of organic synthesis equipment, in particular to a production device for preparing octacarbonyl cobalt. The production device for preparing the octacarbonyl cobalt comprises a storage bin, wherein an autoclave is communicated below the storage bin, a crystallization kettle and a filtrate tank are connected to the autoclave, a filtering and drying assembly is connected to the crystallization kettle, and a liquid outlet of the filtering and drying assembly is communicated with the filtrate tank, so that the integrated design of the synthesis, filtering and packaging processes of octacarbonyl cobalt is realized, the contact with air is avoided, and the operation of people is facilitated; meanwhile, the filtrate can be recycled, so that the waste of materials is effectively avoided.
Description
Technical Field
The utility model relates to the technical field of organic synthesis equipment, in particular to a production device for preparing octacarbonyl cobalt.
Background
Cobalt octacarbonyl with the chemical general formula of Co 2 (CO) 8 . Cobalt octacarbonyl is an important organometallic compound and has very wide application in the field of oxo synthesis, and can be used for preparing catalysts for oxo aldehydes, alcohols, acids or esters.
At present, the preparation method of the octacarbonyl cobalt comprises the steps of adding CoCO into petroleum ether or toluene solvent respectively 3 、Co(OH) 2 Or Co 2 O 3 Synthesizing the mixture in the synthesis gas of hydrogen and carbon monoxide at the pressure of 3-20 Mpa and the temperature of 90-150 ℃, and then filtering, centrifuging, packaging and the like. The devices involved in these steps are typically separate from each other due to Co 2 (CO) 8 The device can be quickly failed when contacted with air and is easy to spontaneously ignite, so that no device for integrating the reaction, filtration, centrifugation, packaging and other processes is designed at present.
In view of this, the present application proposes an integrated production device for the preparation of cobalt octacarbonyl, which can avoid contact with air.
Disclosure of Invention
The utility model aims to at least solve one of the technical problems in the prior art and provides a production device for preparing octacarbonyl cobalt.
In order to achieve the above purpose, the technical scheme adopted by the utility model is as follows: the utility model provides a apparatus for producing for be used for preparing octacarbonyl cobalt, includes the feed bin, feed bin below intercommunication has autoclave, be connected with crystallization kettle and filtrate jar on the autoclave, be connected with the filtration drying module on the crystallization kettle, the liquid outlet of filtration drying module with the filtrate jar is linked together.
Further, a crystallization kettle is located below the autoclave, and the filtrate tank is located on the autoclave.
Further, at least three first air inlet pipelines are arranged above the autoclave, and the first air inlet pipelines comprise N 2 Air inlet pipeline, CO air inlet pipeline and H 2 One or more of the air intake lines.
Further, a second air inlet pipeline is arranged above the crystallization kettle, and the second air inlet pipeline is N 2 An air inlet pipeline.
Further, filter dry subassembly and include filtering the cauldron, the third air inlet line is installed to filtering the cauldron top, it is equipped with the discharge gate to filter the cauldron below.
Further, the third air inlet pipeline is N 2 An air inlet pipeline.
Further, the liquid outlet is positioned at the side part of the filter kettle.
Further, the filtering kettle is positioned below the crystallization kettle.
Further, stirring components are arranged on the autoclave, the crystallization kettle and the filtering kettle, the stirring components comprise motors, stirring rods are arranged at the output ends of the motors, and stirring blades are arranged on the stirring rods.
Furthermore, a plurality of valves for controlling the flow of gas or liquid are arranged among the autoclave, the crystallization kettle, the filtering and drying assembly and the filtrate tank.
Compared with the prior art, the technical scheme of the application has the following beneficial effects:
the production device for preparing the octacarbonyl cobalt comprises a storage bin, wherein an autoclave is communicated below the storage bin, a crystallization kettle and a filtrate tank are connected to the autoclave, a filtering and drying assembly is connected to the crystallization kettle, and a liquid outlet of the filtering and drying assembly is communicated with the filtrate tank, so that the integrated design of the synthesis, filtering and packaging processes of octacarbonyl cobalt is realized, the contact with air is avoided, and the operation of people is facilitated; meanwhile, the filtrate can be recycled, so that the waste of materials is effectively avoided.
Drawings
FIG. 1 is a schematic structural diagram of a production apparatus for producing cobalt octacarbonyl in a preferred embodiment of the present utility model.
Reference numerals: 1. a storage bin; 2. a filtrate tank; 3. an autoclave; 4. a crystallization kettle; 5. a filtering kettle; 6. a first air intake line; 7. a second air intake line; 8. a third air intake line; 9. and (5) a stirring assembly.
Detailed Description
The following description of the embodiments of the present utility model will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all embodiments of the utility model.
Referring to fig. 1, the production device for preparing octacarbonyl cobalt according to the preferred embodiment of the utility model comprises a bin 1, wherein an autoclave 3 is communicated below the bin 1, a crystallization kettle 4 and a filtrate tank 2 are connected to the autoclave 3, a filter drying component is connected to the crystallization kettle 4, and a liquid outlet of the filter drying component is communicated with the filtrate tank 2, so that the integrated design of the synthesis, filtration and packaging processes of octacarbonyl cobalt is realized, contact with air is avoided, and convenience is brought to people; meanwhile, the filtrate can be recycled, so that the waste of materials is effectively avoided.
As a preferred embodiment of the utility model, it may also have the following additional technical features: a crystallization kettle 4 is located below the autoclave 3, and the filtrate tank 2 is located on the autoclave 3. Thereby facilitating the input of raw materials.
In this embodiment, at least three first air inlet pipelines 6 are arranged above the autoclave 3, and the first air inlet pipelines 6 comprise N 2 Air inlet pipeline, CO air inlet pipeline and H 2 One or more of the air intake lines. Thereby ensuring that no reaction is performed in the whole reaction processAir is available, and the cobalt octacarbonyl is effectively prevented from being contacted with the air.
In this embodiment, a second air inlet pipe 7 is installed above the crystallization kettle 4, and the second air inlet pipe 7 is N 2 An air inlet pipeline. Thus, the cobalt octacarbonyl can be prevented from contacting with air.
In this embodiment, the filter drying assembly includes a filter tank 5, a third air inlet pipeline 8 is installed above the filter tank 5, and the third air inlet pipeline 8 is N 2 An air intake line; a discharge hole is arranged below the filtering kettle and is positioned at the side part of the filtering kettle 5. Thereby facilitating the passage of the cobalt octacarbonyl in the filter kettle through N 2 Drying is carried out, and meanwhile, the filtrate can be recycled, so that the waste of materials is avoided.
In this embodiment, the filter tank 5 is located below the crystallization tank 4. Thereby, the solution after crystallization is easily filtered.
In this embodiment, stirring assemblies 9 are all installed on autoclave 3, crystallization kettle 4, filtration cauldron 5, stirring assemblies 9 include the motor, the puddler is installed to the output of motor, install the stirring leaf on the puddler. Therefore, the materials can be fully and uniformly mixed in the synthesis, crystallization and filtration processes.
In this embodiment, a plurality of valves for controlling the flow of gas or liquid are installed among the autoclave 3, the crystallization kettle 4, the filtration and drying assembly and the filtrate tank 2. Thereby facilitating control of the production process of the cobalt octacarbonyl.
The production device of the application is utilized to prepare octacarbonyl cobalt, and the operation is specifically as follows: to the silo 1, 6kg of cobalt hydroxide was added, and to the filtrate tank 2, 90L of petroleum ether and 0.15kg of palladium carbon were added. The whole system is replaced by nitrogen, the connecting valve of the feed bin 1 and the autoclave 3 and the connecting valve of the filtrate tank 2 and the autoclave 3 are opened, materials are put into the autoclave 3, after the replacement for 3 times by CO, the materials are pressurized to 6MPa by using hydrogen and CO, the temperature is raised to 180 ℃, after the reaction is finished, the materials are transferred into the crystallization kettle 4 through a pressure difference and a filter at the bottom of the autoclave 3, and redundant cobalt hydroxide and palladium carbon in the autoclave 3 are used mechanically.
Cooling to-60 ℃ in the crystallization 4, stirring and crystallizing for 7 hours, transferring the obtained crystallization liquid into a filtering kettle 5, carrying out pressure filtration through nitrogen, and transferring filtrate into a filtrate tank 2 through nitrogen for reuse. And after the press filtration is finished, introducing nitrogen for drying, and packaging after drying. 15.6kg of octacarbonyl cobalt is obtained in a single batch, the purity is 98 percent, and the yield is 71 percent
The working principle of the utility model is as follows: by adding cobalt hydroxide into the stock bin 1, petroleum ether and palladium carbon are added into the filtrate tank 2. The whole system is replaced by nitrogen, the connecting valve of the feed bin 1 and the autoclave 3 and the connecting valve of the filtrate tank 2 and the autoclave 3 are opened, materials are put into the autoclave 3, after CO is replaced for 3 times, hydrogen and CO are used for pressurizing to 6MPa, the temperature rising reaction is started, after the reaction is finished, the materials are transferred into the crystallization kettle 4 through a pressure difference and a filter at the bottom of the autoclave 3, the crystallization kettle 4 is cooled and crystallized, the obtained crystallization liquid is transferred into the filtering kettle 5 for filter pressing through nitrogen, and the filtrate is transferred into the filtrate tank 2 for use through nitrogen. And after the press filtration is finished, nitrogen drying is carried out, and discharging and packaging are carried out.
The above additional technical features can be freely combined and superimposed by a person skilled in the art without conflict.
It will be understood that the utility model has been described in terms of several embodiments, and that various changes and equivalents may be made to these features and embodiments by those skilled in the art without departing from the spirit and scope of the utility model. In addition, many modifications may be made to adapt a particular situation or material to the teachings of the utility model without departing from the essential scope thereof. Therefore, it is intended that the utility model not be limited to the particular embodiment disclosed, but that the utility model will include all embodiments falling within the scope of the appended claims.
Claims (10)
1. A production device for preparing octacarbonyl cobalt, which is characterized in that: including the feed bin, feed bin below intercommunication has autoclave, be connected with crystallization kettle and filtrate jar on the autoclave, be connected with filtration drying assembly on the crystallization kettle, filtration drying assembly's liquid outlet with the filtrate jar is linked together.
2. The production apparatus for producing octacarbonyl cobalt according to claim 1, wherein: the crystallization kettle is located below the autoclave, and the filtrate tank is located on the autoclave.
3. The production apparatus for producing octacarbonyl cobalt according to claim 1, wherein: at least three first air inlet pipelines are arranged above the autoclave, and each first air inlet pipeline comprises N 2 Air inlet pipeline, CO air inlet pipeline and H 2 One or more of the air intake lines.
4. The production apparatus for producing octacarbonyl cobalt according to claim 1, wherein: a second air inlet pipeline is arranged above the crystallization kettle, and the second air inlet pipeline is N 2 An air inlet pipeline.
5. The production apparatus for producing octacarbonyl cobalt according to claim 1, wherein: the filtering and drying assembly comprises a filtering kettle, a third air inlet pipeline is arranged above the filtering kettle, and a discharge hole is arranged below the filtering kettle.
6. The production apparatus for producing cobalt octacarbonyl according to claim 5, wherein: the third air inlet pipeline is N 2 An air inlet pipeline.
7. The production apparatus for producing cobalt octacarbonyl according to claim 5, wherein: the liquid outlet is positioned at the side part of the filter kettle.
8. The production apparatus for producing cobalt octacarbonyl according to claim 5, wherein: the filtering kettle is positioned below the crystallization kettle.
9. The production apparatus for producing cobalt octacarbonyl according to claim 5, wherein: stirring components are arranged on the autoclave, the crystallization kettle and the filtering kettle, the stirring components comprise motors, stirring rods are arranged at the output ends of the motors, and stirring blades are arranged on the stirring rods.
10. The production apparatus for producing octacarbonyl cobalt according to claim 1, wherein: and a plurality of valves for controlling the flow of gas or liquid are arranged among the autoclave, the crystallization kettle, the filtering and drying assembly and the filtrate tank.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202322294205.2U CN220657537U (en) | 2023-08-25 | 2023-08-25 | Production device for preparing octacarbonyl cobalt |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202322294205.2U CN220657537U (en) | 2023-08-25 | 2023-08-25 | Production device for preparing octacarbonyl cobalt |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN220657537U true CN220657537U (en) | 2024-03-26 |
Family
ID=90340035
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202322294205.2U Active CN220657537U (en) | 2023-08-25 | 2023-08-25 | Production device for preparing octacarbonyl cobalt |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN220657537U (en) |
-
2023
- 2023-08-25 CN CN202322294205.2U patent/CN220657537U/en active Active
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| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CP03 | Change of name, title or address |
Address after: Room 421, 4th Floor, Office Building, Hongxing Wodengka Quangang Petrochemical Technology Innovation Park, No. 499 Yifeng West Road, Sanzhu Village, Qianhuang Town, Quangang District, Quanzhou City, Fujian Province, 362800 Patentee after: Fujian Chunming New Materials Technology Co.,Ltd. Country or region after: China Address before: Room 421, 4th Floor, Office Building, Hongxing Wodengka Quangang Petrochemical Technology Innovation Park, No. 499 Yifeng West Road, Sanzhu Village, Qianhuang Town, Quangang District, Quanzhou City, Fujian Province, 362800 Patentee before: Fujian Qingyan Biotechnology Co.,Ltd. Country or region before: China |