CN216756367U - 2-hydroxyl tetrahydrofuran continuous production device - Google Patents
2-hydroxyl tetrahydrofuran continuous production device Download PDFInfo
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- CN216756367U CN216756367U CN202220106023.0U CN202220106023U CN216756367U CN 216756367 U CN216756367 U CN 216756367U CN 202220106023 U CN202220106023 U CN 202220106023U CN 216756367 U CN216756367 U CN 216756367U
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- storage tank
- fixed bed
- bed reactor
- outlet end
- continuous production
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- JNODDICFTDYODH-UHFFFAOYSA-N 2-hydroxytetrahydrofuran Chemical compound OC1CCCO1 JNODDICFTDYODH-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 238000010924 continuous production Methods 0.000 title claims abstract description 15
- 238000003860 storage Methods 0.000 claims abstract description 56
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 claims abstract description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000008367 deionised water Substances 0.000 claims abstract description 12
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 12
- 239000007791 liquid phase Substances 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 239000012071 phase Substances 0.000 claims abstract description 6
- 239000011949 solid catalyst Substances 0.000 claims abstract description 5
- 229910001868 water Inorganic materials 0.000 claims description 6
- OZCRKDNRAAKDAN-UHFFFAOYSA-N but-1-ene-1,4-diol Chemical compound O[CH][CH]CCO OZCRKDNRAAKDAN-UHFFFAOYSA-N 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N tetrahydrofuran Substances C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims 1
- 239000003054 catalyst Substances 0.000 abstract description 9
- 239000001257 hydrogen Substances 0.000 abstract description 6
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 5
- 239000007788 liquid Substances 0.000 abstract description 5
- 239000007789 gas Substances 0.000 abstract description 4
- 238000006317 isomerization reaction Methods 0.000 abstract description 3
- 230000005526 G1 to G0 transition Effects 0.000 abstract description 2
- 239000002253 acid Substances 0.000 abstract description 2
- 230000009471 action Effects 0.000 abstract description 2
- 238000005984 hydrogenation reaction Methods 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000000259 anti-tumor effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 238000012824 chemical production Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 229940127554 medical product Drugs 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000007363 ring formation reaction Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
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Abstract
The utility model relates to a continuous production device of 2-hydroxytetrahydrofuran, which comprises a fixed bed reactor, a deionized water storage tank, a 1, 4-butylene glycol storage tank, a mixing tank and an H2A storage tank and a rectifying tower; the outlet ends of the deionized water storage tank and the 1, 4-butylene glycol storage tank are connected to the inlet of the mixing tankA mouth end; the outlet end of the mixing tank is connected with the first inlet end of the fixed bed reactor, H2The outlet end of the storage tank is connected to the second inlet end of the fixed bed reactor; the fixed bed reactor is filled with a solid catalyst, the bottom of the fixed bed reactor is provided with a liquid phase outlet end and a gas phase outlet end, and the liquid phase outlet end is connected with the rectifying tower. The catalyst is a stationary phase raw material and adopts a feeding mode of feeding from top to bottom and H2The catalyst is a continuous phase and can easily pass through a liquid film on the surface of the catalyst to reach the surface of the catalyst, so that the 1, 4-butylene glycol only undergoes double bond isomerization under the action of monatomic hydrogen and surface acid centers to generate 2-hydroxytetrahydrofuran, and the generation of a hydrogenation product 1, 4-butanediol is inhibited.
Description
Technical Field
The utility model relates to chemical production equipment, in particular to a continuous production device for 2-hydroxytetrahydrofuran.
Background
1, 4-butylene glycol is used as a raw material, 2-hydroxytetrahydrofuran converted by C = C position isomerization and spontaneous cyclization condensation is a key raw material with extremely high added value, and can be extended downstream to synthesize various anti-tumor, anti-depression, blood sugar reduction and other medical products, and high-quality GBL obtained by oxidation of the raw material has huge demand as an electrolyte of a Li ion battery. With the rapid development of important industries related to national civilians, such as the pharmaceutical industry and the battery industry in the important field of the 2025 strategic emerging industry in China, the 2-hydroxytetrahydrofuran industry has a vigorous development trend. The existing 2-hydroxyl tetrahydrofuran production adopts a kettle type batch reactor, has low production efficiency and is difficult to produce on a large scale.
Disclosure of Invention
The utility model aims to provide a continuous production device of 2-hydroxytetrahydrofuran to improve the efficiency of producing the 2-hydroxytetrahydrofuran.
In order to solve the technical problems, the utility model adopts the technical scheme that:
a continuous production device of 2-hydroxyl tetrahydrofuran comprises a fixed bed reactor, a deionized water storage tank, a 1, 4-butylene glycol storage tank, a mixing tank and an H2A storage tank and a rectifying tower;
the outlet ends of the deionized water storage tank and the 1, 4-butylene glycol storage tank are connected to the inlet end of the mixing tank; the outlet end of the mixing tank is connected with the first inlet end of the fixed bed reactor, H2The outlet end of the storage tank is connected to the second inlet end of the fixed bed reactor; the fixed bed reactor is filled with a solid catalyst, the bottom of the fixed bed reactor is provided with a liquid phase outlet end and a gas phase outlet end, and the liquid phase outlet end is connected with the rectifying tower.
Further, comprising N2Storage tank, said N2The outlet end of the storage tank is connected to the second inlet end of the fixed bed reactor.
Further, the outlet end of the rectifying tower is respectively connected to a 2-hydroxytetrahydrofuran storage tank, a 1, 4-butanediol storage tank, a water storage tank and an unreacted raw material 1, 4-butenediol storage tank.
Furthermore, a metering pump is arranged on a connecting pipeline between the mixing tank and the fixed bed reactor.
Furthermore, a deionized water storage tank and a connecting pipeline of the 1, 4-butylene glycol storage tank and the mixing tank are respectively provided with a metering pump.
Further, H2And a flowmeter is arranged on a connecting pipeline of the storage tank and the fixed bed reactor.
Compared with the prior art, the utility model adopts a fixed bed reactor, the catalyst in the reactor is used as the stationary phase raw material and adopts a feeding mode of feeding from top to bottom, and H2The product becomes a continuous phase and can easily pass through a liquid film on the surface of the catalyst to reach the surface of the catalyst, so that the 1, 4-butylene glycol only has double bond isomerization under the action of monatomic hydrogen and surface acid centers to generate 2-hydroxytetrahydrofuran, and the generation of a hydrogenation product 1, 4-butanediol is inhibited. The process can realize continuous production of 2-hydroxytetrahydrofuran, and the reaction efficiency is greatly improved.
Drawings
The accompanying drawings are included to provide a further description of the utility model and are incorporated in and constitute a part of this application, with the exemplary embodiments and description of the utility model being given to illustrate and not limit the utility model.
FIG. 1 is a schematic connection diagram of a continuous production apparatus for 2-hydroxytetrahydrofuran according to the present invention.
In the figure, 1-fixed bed reactor, 2-deionized water storage tank, 3-1, 4-butylene glycol storage tank, 4-mixing tank and 5-H2Storage tank, 6-rectification column, 7-N2The device comprises a storage tank, 8-a metering pump, 9-a flowmeter, 10-a heating wall and 11-a pressure relief tank.
Detailed Description
In order that those skilled in the art will better understand the present invention, a more complete and complete description of the present invention is provided below in conjunction with the accompanying drawings and embodiments. In addition, the features of the embodiments and examples in the present application may be combined with each other without conflict.
As shown in FIG. 1, a continuous production apparatus for 2-hydroxytetrahydrofuran according to a typical embodiment of the present invention comprises a fixed bed reactor 1, a deionized water storage tank 2, a 1, 4-butenediol storage tank 3, a mixing tank 4, and H2A storage tank 5 and a rectifying tower 6;
the outlet ends of the deionized water storage tank 2 and the 1, 4-butylene glycol storage tank 3 are connected to the inlet end of the mixing tank 4; the outlet end of the mixing tank 4 is connected to the first inlet end of the fixed bed reactor 1, H2The outlet end of the storage tank 5 is connected to the second inlet end of the fixed bed reactor 1, and the fixed bed reactor 1 is provided with a heating wall 10 for heating materials; the fixed bed reactor 1 is filled with a solid catalyst, the bottom of the fixed bed reactor 1 is provided with a liquid phase outlet end and a gas phase outlet end, the liquid phase outlet end is connected with the rectifying tower 6, and a pressure relief tank 11 is also arranged between the liquid phase outlet end and the rectifying tower 6.
According to the embodiment, the solid catalyst is filled into the fixed BED reactor 1, hydrogen is introduced into the fixed BED reactor 1, the temperature is raised to 300-500 ℃, the catalyst is reduced for 3-10 h, the reaction temperature is reduced, the hydrogen is continuously introduced, meanwhile, the mixed material of 1, 4-butylene glycol (BED) and water is continuously input into the fixed BED reactor 1, gas-liquid separation is carried out at the bottom of the fixed BED reactor 1, the gas is emptied, and the liquid enters the rectifying tower 6.
The outlet end of the rectifying tower is respectively connected to a 2-hydroxytetrahydrofuran storage tank, a 1, 4-butanediol storage tank, a water storage tank and an unreacted raw material 1, 4-butylene glycol storage tank. Separating out 2-hydroxytetrahydrofuran, 1, 4-butanediol, water, unreacted raw material 1, 4-butenediol and heavy components generated in the reaction process.
In the fixed bed reactor 1, H2O as solvent, and TiO is filled in the fixed bed reactor 12、Al2O3Or a catalyst which takes a compound thereof as a carrier and is loaded with Pd, Ru or Ni, 1, 4-butylene glycol is subjected to hydroisomerization to prepare 2-hydroxytetrahydrofuran, and the mass percent of 1, 4-butylene glycol in the 1, 4-butylene glycol aqueous solution is 10-30%; the liquid hourly space velocity is 0.9-1.5/h, and the reaction temperature is30-75 ℃, preferably 60-65 ℃; the hydrogen pressure is 0.1-1 MPa, preferably 0.1-0.5 MPa. Under the reaction conditions, the conversion rate of 1, 4-butylene glycol reaches 80-98%, and the selectivity of 2-hydroxytetrahydrofuran is 60-89%.
In a preferred embodiment, the apparatus of the present invention further comprises N2Storage tank 7, said N2The outlet end of the storage tank 7 is connected to the second inlet end of the fixed bed reactor 1. Before introducing hydrogen, N is started2And a valve on a connecting pipeline of the storage tank 7 and the fixed bed reactor 1 is used for introducing nitrogen into the fixed bed reactor 1 so as to remove air in the fixed bed reactor 1.
Relatively concretely, a metering pump 8 is arranged on a connecting pipeline between the mixing tank 4 and the fixed bed reactor 1; and the connecting pipelines of the deionized water storage tank 2, the 1, 4-butylene glycol storage tank 3 and the mixing tank 4 are respectively provided with a metering pump 8. H2A flow meter 9 is arranged on a connecting pipeline between the storage tank 5 and the fixed bed reactor 1.
The scope of the utility model is not limited to the above embodiments, and various modifications and changes may be made by those skilled in the art, and any modifications, improvements and equivalents within the spirit and principle of the utility model should be included in the scope of the utility model.
Claims (6)
1. The continuous production device of the 2-hydroxyl tetrahydrofuran is characterized in that: comprises a fixed bed reactor, a deionized water storage tank, a 1, 4-butylene glycol storage tank, a mixing tank and H2A storage tank and a rectifying tower;
the outlet ends of the deionized water storage tank and the 1, 4-butylene glycol storage tank are connected to the inlet end of the mixing tank; the outlet end of the mixing tank is connected with the first inlet end of the fixed bed reactor, H2The outlet end of the storage tank is connected to the second inlet end of the fixed bed reactor; the fixed bed reactor is filled with a solid catalyst, the bottom of the fixed bed reactor is provided with a liquid phase outlet end and a gas phase outlet end, and the liquid phase outlet end is connected with the rectifying tower.
2. The method of claim 12-hydroxyl tetrahydrofuran continuous production device which is characterized in that: comprising N2Storage tank, said N2The outlet end of the storage tank is connected to the second inlet end of the fixed bed reactor.
3. The continuous production apparatus of 2-hydroxytetrahydrofuran according to claim 1 or 2, characterized in that: the outlet end of the rectifying tower is respectively connected to a 2-hydroxytetrahydrofuran storage tank, a 1, 4-butanediol storage tank, a water storage tank and an unreacted raw material 1, 4-butenediol storage tank.
4. The continuous production apparatus of 2-hydroxytetrahydrofuran according to claim 3, characterized in that: a metering pump is arranged on a connecting pipeline of the mixing tank and the fixed bed reactor.
5. The continuous production apparatus of 2-hydroxytetrahydrofuran according to claim 4, characterized in that: and metering pumps are respectively arranged on the connecting pipelines of the deionized water storage tank and the 1, 4-butylene glycol storage tank and the mixing tank.
6. The continuous production apparatus of 2-hydroxytetrahydrofuran according to claim 5, characterized in that: h2And a flowmeter is arranged on a connecting pipeline of the storage tank and the fixed bed reactor.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202220106023.0U CN216756367U (en) | 2022-01-17 | 2022-01-17 | 2-hydroxyl tetrahydrofuran continuous production device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202220106023.0U CN216756367U (en) | 2022-01-17 | 2022-01-17 | 2-hydroxyl tetrahydrofuran continuous production device |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN216756367U true CN216756367U (en) | 2022-06-17 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202220106023.0U Active CN216756367U (en) | 2022-01-17 | 2022-01-17 | 2-hydroxyl tetrahydrofuran continuous production device |
Country Status (1)
| Country | Link |
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| CN (1) | CN216756367U (en) |
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- 2022-01-17 CN CN202220106023.0U patent/CN216756367U/en active Active
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| GR01 | Patent grant | ||
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| TR01 | Transfer of patent right |
Effective date of registration: 20231207 Address after: Room 1005, 10th Floor, Dingchen Times Square, No. 5 Development Road, Xuefu Industrial Park, Shanxi Transformation and Comprehensive Reform Demonstration Zone, Taiyuan City, Shanxi Province, 030017 Patentee after: Shanxi Taike High tech Co.,Ltd. Address before: No.319, Daxue street, Yuci District, Jinzhong City, Shanxi Province Patentee before: TAIYUAN NORMAL University |