CN210945432U - Synthesizer of 1, 3-butanediol - Google Patents
Synthesizer of 1, 3-butanediol Download PDFInfo
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- CN210945432U CN210945432U CN201921861778.6U CN201921861778U CN210945432U CN 210945432 U CN210945432 U CN 210945432U CN 201921861778 U CN201921861778 U CN 201921861778U CN 210945432 U CN210945432 U CN 210945432U
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Abstract
The utility model discloses a 1, 3-butanediol synthesizer, acetaldehyde aqueous solution carries out condensation reaction in the reaction rectifying column of load alkaline anion resin, acetaldehyde that is fractionated from the top of the tower returns the head tank recycle, 3-hydroxy butyraldehyde that the column bottom is fractionated directly gets into the tower reactor and carries out hydrogenation; carrying out hydrogenation reaction on 3-hydroxybutyraldehyde and hydrogen in a tower reactor, recycling the hydrogen at the tower top, and feeding the 1, 3-butanediol crude product obtained at the tower bottom into a vacuum refining system; the 1, 3-butanediol crude product enters a light component removal tower to remove light components, then enters a heavy component removal tower, and a 1, 3-butanediol product with the purity of more than 99.6 percent and no peculiar smell is obtained at the tower top. The utility model has the characteristics of short, the energy consumption is low, pollute less, can realize serialization production of flow.
Description
Technical Field
The utility model relates to a chemical industry reaction separation technical field specifically is a synthesizer of 1, 3-butanediol.
Background
1, 3-butanediol has good hygroscopicity and water solubility, no odor and low toxicity, so that the butanediol-containing water-soluble organic silicon dioxide is widely applied to cosmetics, medicines and high-grade building material products. However, the current domestic 1, 3-butanediol product almost completely depends on foreign import, and has no own industrialized device at home. With the popularization of the application range of the 1, 3-butanediol, the domestic research on the 1, 3-butanediol is increasing. At present, acetaldehyde is mostly used as a raw material in the research of a synthetic route of 1, 3-butanediol, and a specific route is that the acetaldehyde is condensed to generate 3-hydroxybutyraldehyde, and then the 3-hydroxybutyraldehyde is hydrogenated to generate the 1, 3-butanediol. The route is also the route for producing the 1, 3-butanediol at present abroad.
For example, the research of the liquid-phase aldol condensation reaction of acetaldehyde by the university of Tongji for many years, and a series of optimization researches are carried out on the reaction temperature, the pH value and the alkaline condition of the system.
At present, the patent also reports various methods for preparing hydroxyaldehydes and 1, 3-butanediol: canadian patent CN107849522A provides a non-naturally occurring microorganism having a 1,3-BDO pathway; chinese patent CN105585448A proposes that water is used as a solvent to optimize an acetaldehyde condensation reaction to obtain 3-hydroxybutyraldehyde, and then the 3-hydroxybutyraldehyde is injected into an autoclave to react to obtain 1, 3-butanediol; chinese patent CN206396080U provides a 1, 3-butanediol condensation reaction apparatus, which comprises a condensation reactor, a hydrogenation reactor and a first rectification tower. Patent 105037119A proposes a plate-type reactive distillation column for acetaldehyde condensation. Chinese patent CN109422624A shows that the yield and purity of 1, 3-butanediol prepared by the mainstream production process of 1, 3-butanediol are not ideal and have pungent smell, so that the production process of 1, 3-butanediol is optimized by adopting a fixed bed reactor and a supported nickel hydrogenation catalyst. Although the fixed bed reactor has less back mixing than the tank reactor, the back mixing still exists and the flow is complex. In addition, the acetaldehyde condensation section of the above patents has a large amount of salt generated and is difficult to handle.
SUMMERY OF THE UTILITY MODEL
The utility model provides a synthetic device of 1, 3-butanediol for solve above-mentioned technical problem.
The utility model discloses a realize according to following technical scheme.
A1, 3-butanediol synthesis device comprises a condensation reaction system, a hydrogenation reaction system and a vacuum refining system which are sequentially connected through pipelines; the condensation reaction system adopts a reaction rectifying tower loaded with alkaline anion resin; the hydrogenation reaction system adopts a tower type hydrogenation reactor; the vacuum refining system comprises a light component removal tower and a heavy component removal tower.
Further, the top of the reactive distillation tower is connected with a condenser at the top of the reactive distillation tower through a pipeline, and the lower part of the reactive distillation tower is connected with a reboiler of the reactive distillation tower and a tower type hydrogenation reactor through a pipeline; the tower top condenser of the reactive distillation tower is connected with a reflux tank of the reactive distillation tower through a pipeline, and the reflux tank of the reactive distillation tower is connected with the reactive distillation tower through a pipeline;
the tower top of the tower type hydrogenation reactor is connected with the lower part of the tower type hydrogenation reactor through a pipeline, and the tower kettle of the tower type hydrogenation reactor is connected with the light component removal tower through a pipeline;
the top of the light component removal tower is connected with a condenser at the top of the light component removal tower through a pipeline, and the lower part of the light component removal tower is connected with a reboiler of the light component removal tower and a heavy component removal tower through pipelines; the condenser at the top of the light component removal tower is connected with a light component removal tower reflux tank through a pipeline, and the light component removal tower reflux tank is connected with the light component removal tower through a pipeline;
the top of the heavy component removal tower is connected with a tower top condenser of the heavy component removal tower through a pipeline, and the lower part of the heavy component removal tower is connected with a reboiler of the heavy component removal tower through a pipeline; the tower top condenser of the de-heavy tower is connected with a reflux tank of the de-heavy tower through a pipeline, and the reflux tank of the de-heavy tower is connected with the de-heavy tower through a pipeline;
and the tops of the light component removal tower and the heavy component removal tower are respectively connected with a light component removal tower vacuum-pumping pipeline and a heavy component removal tower vacuum-pumping pipeline.
Furthermore, the operating temperature of the reactive distillation tower is-5-50 ℃.
Further, the operating pressure of the tower type hydrogenation reactor is 2.0-6.0 MpaA absolute pressure, and the operating temperature is 50-120 ℃.
Further, the operating pressure of the light component removal tower is 0.03-0.08 MpaA.
Further, the operation pressure of the de-heavy tower is 0.0002-0.005 MpaA.
The utility model discloses following beneficial effect has been obtained.
The utility model discloses an adopt reaction rectifying column, tower reactor and the refined system in vacuum of load alkaline anion resin, obtain high-quality 1, 3-butanediol product, the purity is greater than 99.6% and free from extraneous odour. The method has the characteristics of short flow, low energy consumption, less pollution and continuous production. Therefore, the method has great implementation value, social benefit, environmental benefit and economic benefit.
Drawings
FIG. 1 is a schematic diagram of the process for synthesizing and refining 1, 3-butanediol of the present invention.
Wherein, 1, acetaldehyde aqueous solution; 2. reacting light components at the top of the rectifying tower; 3. condensing the light components on the top of the reaction rectifying tower; 4. refluxing liquid phase in the reactive distillation tower; 5. recycling acetaldehyde; 6. heavy components in the tower kettle of the reactive distillation tower; 7. a heavy component vaporized by a reboiler; 8.3-hydroxybutyraldehyde; 9. circulating hydrogen; 10. fresh hydrogen gas; 11. total hydrogen; 12. crude 1, 3-butanediol; 13. light components at the top of the light component removal tower; 14. condensing light components at the top of the lightness-removing tower; 15. refluxing liquid phase in the light component removal tower; 16. light components; 17. heavy components in the tower kettle of the light component removal tower; 18. heavy components in a tower kettle of the light component removal tower gasified by a reboiler; 19. removing light components of the 1, 3-butanediol crude product; 20. removing light components at the top of the heavy tower; 21. the condensed components of the de-weighting tower; 22. refluxing the liquid phase in the de-heavy tower; 1, 3-butanediol product; 24. heavy components in a tower kettle of the de-heavy tower; 25. heavy components in a heavy component removal tower gasified by a reboiler; 26. a heavies stream; 27. a reactive distillation column; 28. a condenser at the top of the reaction rectifying tower; 29. a reflux tank of the reaction rectifying tower; 30. a reboiler at the tower bottom of the reactive distillation tower; 31. a tower hydrogenation reactor; 32. a light component removal tower; 33. a condenser at the top of the light component removal tower; 34. a light component removal tower reflux tank; 35. a light component removal tower reboiler; 36. a de-weighting tower; 37. a tower top condenser of the de-heavy tower; 38. a reflux tank of the de-weighting tower; 39. a de-heaving column reboiler; 40. vacuumizing a pipeline of the light component removal tower; 41. and (4) vacuumizing a pipeline of the de-weighting tower.
Detailed Description
The present invention will be described in detail with reference to the accompanying drawings and examples.
As shown in fig. 1, a 1, 3-butanediol synthesis apparatus comprises a condensation reaction system, a hydrogenation reaction system and a vacuum refining system which are connected in sequence by pipelines; the condensation reaction system adopts a reaction rectifying tower 27 loaded with basic anion resin; the hydrogenation reaction system adopts a tower type hydrogenation reactor 31; the vacuum refining system includes a light ends removal column 32 and a heavy ends removal column 36.
The top of the reaction rectifying tower 27 is connected with a reaction rectifying tower top condenser 28 through a pipeline, and the lower part of the reaction rectifying tower 27 is connected with a reaction rectifying tower reboiler 30 and a tower type hydrogenation reactor 31 through pipelines; the reaction rectifying tower top condenser 28 is connected with a reaction rectifying tower reflux tank 29 through a pipeline, and the reaction rectifying tower reflux tank 29 is connected with the reaction rectifying tower 27 through a pipeline;
the top of the tower hydrogenation reactor 31 is connected with the lower part of the tower hydrogenation reactor 31 through a pipeline, and the bottom of the tower hydrogenation reactor 31 is connected with the light component removal tower 32 through a pipeline;
the top of the light component removal tower 32 is connected with a condenser 33 at the top of the light component removal tower through a pipeline, and the lower part of the light component removal tower 32 is connected with a reboiler 35 and a heavy component removal tower 36 through pipelines; the top condenser 33 of the light component removal tower is connected with a light component removal tower reflux tank 34 through a pipeline, and the light component removal tower reflux tank 34 is connected with the light component removal tower 32 through a pipeline;
the top of the de-heavy column 36 is connected with a de-heavy column overhead condenser 37 through a pipeline, and the lower part of the de-heavy column 36 is connected with a de-heavy column reboiler 39 through a pipeline; the heavy component removal tower top condenser 37 is connected with a heavy component removal tower reflux tank 38 through a pipeline, and the heavy component removal tower reflux tank 38 is connected with the heavy component removal tower 36 through a pipeline;
the tops of the light component removal tower 32 and the heavy component removal tower 36 are respectively connected with a light component removal tower vacuum-pumping pipeline 40 and a heavy component removal tower vacuum-pumping pipeline 41.
The operating temperature of the reactive distillation tower 27 is-5 to 50 ℃.
The operation pressure of the tower hydrogenation reactor 31 is 2.0-6.0 MpaA absolute pressure, and the operation temperature is 50-120 ℃.
The operating pressure of the light component removal tower 32 is 0.03-0.08 MpaA.
The operation pressure of the de-heavy tower 36 is 0.0002-0.005 MpaA.
A method for synthesizing 1, 3-butanediol comprises the following steps:
s1, feeding an acetaldehyde aqueous solution 1 into a reaction rectifying tower 27, and carrying out condensation reaction under the catalytic action of an alkaline anionic resin catalyst loaded in the tower; the light component 2 at the top of the reactive distillation tower which is not completely reacted is condensed into the light component 3 at the top of the reactive distillation tower which is condensed by a condenser 28 at the top of the reactive distillation tower, and then the light component enters a reflux tank 29 of the reactive distillation tower, part of the liquid phase in the reflux tank 29 of the reactive distillation tower is used as the reflux liquid phase 4 of the reactive distillation tower and flows back to the reactive distillation tower 27, and part of the liquid phase is recycled as the circulating acetaldehyde 5; the tower bottom of the reactive distillation tower 27 is a tower bottom heavy component 6 rich in 3-hydroxy butyraldehyde, one part of the heavy component is gasified by a reboiler 30 of the reactive distillation tower and then is converted into a heavy component 7 gasified by the reboiler, and the heavy component is returned to the tower, and the other part of the heavy component is used as a raw material 3-hydroxy butyraldehyde 8 of a tower hydrogenation reactor 31 and enters the tower hydrogenation reactor 31;
s2: carrying out hydrogenation reaction on 3-hydroxybutyraldehyde 8 and total hydrogen 11 in a tower type hydrogenation reactor 31, mixing circulating hydrogen 9 at the tower top with supplemented fresh hydrogen 10, and then feeding the mixture into the tower type hydrogenation reactor 31, and obtaining a reaction product crude 1, 3-butanediol 12 at the tower bottom; the crude 1, 3-butanediol 12 of the reaction product enters a lightness-removing tower 32;
s3, condensing the light component 13 at the top of the lightness-removing column into a condensed light component 14 at the top of the lightness-removing column through a condenser 33 at the top of the lightness-removing column, and then feeding the condensed light component 14 into a reflux tank 34 of the lightness-removing column, wherein one part of the liquid phase in the reflux tank 34 of the lightness-removing column is taken as a reflux liquid phase 15 of the lightness-removing column to reflux the lightness-removing column 32, and the other part is taken as a light component 16; the bottom of the light component removal tower 32 is a heavy component 17 of the bottom of the light component removal tower rich in 1, 3-butanediol, one part of the heavy component removal tower is gasified by a reboiler 35 of the light component removal tower to form a heavy component 18 of the bottom of the light component removal tower gasified by the reboiler and returns to the tower, and the other part of the heavy component removal tower is used as a raw product 19 of the 1, 3-butanediol with the light component removed by the feeding of the heavy component removal tower 36 and enters the heavy component removal tower 36;
s4: a heavy component removal tower top 20 at the tower top of the heavy component removal tower 36 is gas-phase 1, 3-butanediol, the gas-phase 1, 3-butanediol is condensed into a condensed heavy component removal tower 21 through a heavy component removal tower top condenser 37 and then enters a heavy component removal tower reflux tank 38, a part of liquid phase in the heavy component removal tower reflux tank 38 is returned to the heavy component removal tower 36 as a heavy component removal tower reflux liquid phase 22, and a part of liquid phase is extracted as a 1, 3-butanediol product 23; the tower bottom of the heavy component removal tower 36 is the heavy component 24 of the tower bottom of the heavy component removal tower, one part of the heavy component removal tower is gasified by a heavy component removal tower reboiler 39 and then becomes the heavy component 25 of the heavy component removal tower gasified by the reboiler to return to the tower, and the other part of the heavy component removal tower is taken out as a heavy component stream 26.
The operating temperature of the reactive distillation tower 27 is-5 to 50 ℃.
The operation pressure of the tower hydrogenation reactor 31 is 2.0-6.0 MpaA absolute pressure, and the operation temperature is 50-120 ℃.
The operating pressure of the light component removal tower 32 is 0.03-0.08 MpaA.
The operation pressure of the de-heavy tower 36 is 0.0002-0.005 MpaA.
The synthesis device of the utility model comprises a condensation reaction system, a hydrogenation reaction system and a vacuum refining system. Adopting a packing type reaction rectifying tower to realize the condensation of acetaldehyde to generate 3-hydroxybutyraldehyde; hydrogenating 3-hydroxybutyraldehyde in a tower reactor to obtain a 1, 3-butanediol crude product; and (3) feeding the 1, 3-butanediol crude product into a vacuum refining system to obtain a high-quality 1, 3-butanediol product.
The condensation reaction system adopts a reaction rectifying tower loaded with alkaline anion resin to realize the condensation reaction of acetaldehyde to generate 3-hydroxybutyraldehyde, and the acetaldehyde distilled from the tower top can be recycled; and the alkaline anion resin is used as a catalyst, so that the wastewater discharge of the device is reduced.
The hydrogenation reaction system adopts a tower reactor to realize the hydrogenation reaction of the 3-hydroxybutyraldehyde, the tower reactor can reduce the back mixing to the minimum, and the yield and the conversion rate of the reaction are improved.
The refining system is a vacuum system, namely the vacuum system is adopted to refine the 1, 3-butanediol crude product, the temperature is reduced, the decomposition of heat-sensitive substances is prevented, and the purity of the 1, 3-butanediol is improved.
The utility model provides a device and a method for synthesizing 1, 3-butanediol on the basis of a plate-type reaction rectifying tower, a kettle-type reactor and a fixed bed reactor; optimizing the condensation reaction of acetaldehyde by adopting a reaction rectifying tower; a tower reactor is adopted to optimize the hydrogenation reaction of the 3-hydroxybutyraldehyde; and then refining the 1, 3-butanediol product by adopting vacuum rectification. The utility model discloses whole flow is simple, can realize the continuity operation, reduces the energy consumption, promotes sustainable development, and has improved the quality of 1, 3-butanediol product, has enlarged the range of application, has very big economic benefits, environmental benefit and social.
It is obvious to a person skilled in the art that the invention is not restricted to details of the above-described exemplary embodiments, but that it can be implemented in other specific forms without departing from the spirit or essential characteristics of the invention. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (6)
1. The 1, 3-butanediol synthesizing device is characterized in that: comprises a condensation reaction system, a hydrogenation reaction system and a vacuum refining system which are connected in sequence through pipelines; the condensation reaction system adopts a reaction rectifying tower (27) loaded with basic anion resin; the hydrogenation reaction system adopts a tower type hydrogenation reactor (31); the vacuum refining system includes a light ends removal column (32) and a heavy ends removal column (36).
2. The apparatus for synthesizing 1, 3-butanediol as claimed in claim 1, wherein:
the top of the reactive distillation column (27) is connected with a condenser (28) at the top of the reactive distillation column through a pipeline, and the lower part of the reactive distillation column (27) is connected with a reboiler (30) of the reactive distillation column and a tower hydrogenation reactor (31) through a pipeline; the reaction rectifying tower top condenser (28) is connected with a reaction rectifying tower reflux tank (29) through a pipeline, and the reaction rectifying tower reflux tank (29) is connected with the reaction rectifying tower (27) through a pipeline;
the top of the tower hydrogenation reactor (31) is connected with the lower part of the tower hydrogenation reactor (31) through a pipeline, and the tower kettle of the tower hydrogenation reactor (31) is connected with the light component removal tower (32) through a pipeline;
the top of the light component removal tower (32) is connected with a condenser (33) at the top of the light component removal tower through a pipeline, and the lower part of the light component removal tower (32) is connected with a reboiler (35) of the light component removal tower and a heavy component removal tower (36) through pipelines; the condenser (33) at the top of the light component removal tower is connected with a light component removal tower reflux tank (34) through a pipeline, and the light component removal tower reflux tank (34) is connected with a light component removal tower (32) through a pipeline;
the top of the de-heavy tower (36) is connected with a de-heavy tower overhead condenser (37) through a pipeline, and the lower part of the de-heavy tower (36) is connected with a de-heavy tower reboiler (39) through a pipeline; the overhead condenser (37) of the de-heavy tower is connected with a reflux tank (38) of the de-heavy tower through a pipeline, and the reflux tank (38) of the de-heavy tower is connected with the de-heavy tower (36) through a pipeline;
the top parts of the light component removing tower (32) and the heavy component removing tower (36) are respectively connected with a light component removing tower vacuum-pumping pipeline (40) and a heavy component removing tower vacuum-pumping pipeline (41).
3. The apparatus for synthesizing 1, 3-butanediol as claimed in claim 1, wherein: the operating temperature of the reactive distillation tower (27) is-5-50 ℃.
4. The apparatus for synthesizing 1, 3-butanediol as claimed in claim 1, wherein: the operating pressure of the tower hydrogenation reactor (31) is 2.0-6.0 MpaA absolute pressure, and the operating temperature is 50-120 ℃.
5. The apparatus for synthesizing 1, 3-butanediol as claimed in claim 1, wherein: the operating pressure of the light component removal tower (32) is 0.03-0.08 MpaA.
6. The apparatus for synthesizing 1, 3-butanediol as claimed in claim 1, wherein: the operation pressure of the de-heavy tower (36) is 0.0002-0.005 MpaA.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201921861778.6U CN210945432U (en) | 2019-10-31 | 2019-10-31 | Synthesizer of 1, 3-butanediol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201921861778.6U CN210945432U (en) | 2019-10-31 | 2019-10-31 | Synthesizer of 1, 3-butanediol |
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| Publication Number | Publication Date |
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| CN210945432U true CN210945432U (en) | 2020-07-07 |
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| CN201921861778.6U Active CN210945432U (en) | 2019-10-31 | 2019-10-31 | Synthesizer of 1, 3-butanediol |
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| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of utility model: A synthesis device of 1,3-butanediol Effective date of registration: 20220128 Granted publication date: 20200707 Pledgee: Bank of China Limited Tianjin Nankai sub branch Pledgor: TIANJIN HUIZHU HENGSHENG TECHNOLOGY Co.,Ltd. Registration number: Y2022110000026 |
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| PC01 | Cancellation of the registration of the contract for pledge of patent right |
Date of cancellation: 20230512 Granted publication date: 20200707 Pledgee: Bank of China Limited Tianjin Nankai sub branch Pledgor: TIANJIN HUIZHU HENGSHENG TECHNOLOGY Co.,Ltd. Registration number: Y2022110000026 |