CN210438664U - Reaction system for continuously preparing 1, 2-pentanediol - Google Patents
Reaction system for continuously preparing 1, 2-pentanediol Download PDFInfo
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- CN210438664U CN210438664U CN201921230583.1U CN201921230583U CN210438664U CN 210438664 U CN210438664 U CN 210438664U CN 201921230583 U CN201921230583 U CN 201921230583U CN 210438664 U CN210438664 U CN 210438664U
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- alcoholysis
- hydrolysis
- reaction system
- feed inlet
- discharge hole
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- WCVRQHFDJLLWFE-UHFFFAOYSA-N pentane-1,2-diol Chemical compound CCCC(O)CO WCVRQHFDJLLWFE-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 31
- 238000006136 alcoholysis reaction Methods 0.000 claims abstract description 58
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 36
- 230000007062 hydrolysis Effects 0.000 claims abstract description 33
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 27
- 238000000605 extraction Methods 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000004821 distillation Methods 0.000 claims abstract description 13
- 239000003054 catalyst Substances 0.000 claims abstract description 8
- 239000011973 solid acid Substances 0.000 claims abstract description 8
- 238000010924 continuous production Methods 0.000 claims abstract description 6
- 239000010410 layer Substances 0.000 claims abstract description 5
- 239000012044 organic layer Substances 0.000 claims abstract description 5
- 238000001914 filtration Methods 0.000 claims description 8
- 238000009834 vaporization Methods 0.000 claims description 8
- 230000008016 vaporization Effects 0.000 claims description 8
- 239000007795 chemical reaction product Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 238000000034 method Methods 0.000 description 9
- 239000007921 spray Substances 0.000 description 7
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 239000013067 intermediate product Substances 0.000 description 6
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 5
- SCKXCAADGDQQCS-UHFFFAOYSA-N Performic acid Chemical compound OOC=O SCKXCAADGDQQCS-UHFFFAOYSA-N 0.000 description 4
- 238000003912 environmental pollution Methods 0.000 description 4
- YWAKXRMUMFPDSH-UHFFFAOYSA-N pentene Chemical compound CCCC=C YWAKXRMUMFPDSH-UHFFFAOYSA-N 0.000 description 4
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- 239000004280 Sodium formate Substances 0.000 description 3
- 235000019253 formic acid Nutrition 0.000 description 3
- 238000006386 neutralization reaction Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- HLBBKKJFGFRGMU-UHFFFAOYSA-M sodium formate Chemical compound [Na+].[O-]C=O HLBBKKJFGFRGMU-UHFFFAOYSA-M 0.000 description 3
- 235000019254 sodium formate Nutrition 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- KFSLWBXXFJQRDL-UHFFFAOYSA-N Peracetic acid Chemical compound CC(=O)OO KFSLWBXXFJQRDL-UHFFFAOYSA-N 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 150000002009 diols Chemical class 0.000 description 2
- 239000007800 oxidant agent Substances 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- SYURNNNQIFDVCA-UHFFFAOYSA-N 2-propyloxirane Chemical compound CCCC1CO1 SYURNNNQIFDVCA-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 239000005822 Propiconazole Substances 0.000 description 1
- 238000005904 alkaline hydrolysis reaction Methods 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 239000003899 bactericide agent Substances 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- STJLVHWMYQXCPB-UHFFFAOYSA-N propiconazole Chemical compound O1C(CCC)COC1(C=1C(=CC(Cl)=CC=1)Cl)CN1N=CN=C1 STJLVHWMYQXCPB-UHFFFAOYSA-N 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The utility model discloses a reaction system for continuously preparing 1, 2-pentanediol. The reaction system comprises: the device comprises a reactor, a hydrolysis device, an alcoholysis device, an extraction device, a distillation device and a rectification device, wherein a discharge hole of the reactor is connected with a feed inlet of the hydrolysis device, a water inlet and a solid acid catalyst feeding hole are further formed in the top of the hydrolysis device, a discharge hole of the hydrolysis device is connected with the feed inlet of the alcoholysis device, an alcoholysis agent feed inlet is further formed in the top of the alcoholysis device, a discharge hole of the alcoholysis device is connected with a feed inlet of the extraction device, an organic layer discharge hole of the extraction device is connected with a feed inlet of the distillation device, a water layer discharge hole of the extraction device is connected with a water inlet of the hydrolysis device, and a discharge hole of the distillation device is connected with a feed inlet of the. The reaction system can realize the continuous production of the 1, 2-pentanediol, and has high production efficiency.
Description
Technical Field
The utility model belongs to the technical field of 1, 2-pentanediol preparation, concretely relates to a reaction system for continuously preparing 1, 2-pentanediol.
Background
1, 2-pentanediol is a colorless transparent liquid, and is dissolved in organic solvents such as alcohol, ether and ethyl acetate. The 1, 2-pentanediol is widely applied in the world, is used as a key intermediate of propiconazole serving as a bactericide and a cosmetic formula, and is also an important raw material for producing products such as polyester fibers, surfactants, medicines and the like. Pentane-1, 2-diol is a straight chain diol, with significant polarity and non-polarity, giving it properties different from those of other diols, and this particular charge distribution explains its unique characteristics and versatility.
Document 1 discloses a method for preparing 1, 2-pentanediol, in which n-pentene, formic acid and hydrogen peroxide are used as raw materials, the formic acid and the hydrogen peroxide react at a certain molar ratio under a low temperature condition to prepare peroxyformic acid, and the n-pentene generates 1, 2-cyclopentane under the action of a strong oxidant, namely peroxyformic acid, and then is hydrolyzed under a strong alkaline condition to obtain 1, 2-pentanediol. Wherein, formic acid and hydrogen peroxide generate strong oxidant peroxyformic acid under the condition of low temperature, and compared with flammable and explosive peroxyacetic acid, the peroxyformic acid has higher safety. The method is used for preparing the 1, 2-pentanediol, the product purity is 99 percent, and the yield is 72 percent. However, the preparation method has some defects, such as the strong alkali sodium hydroxide used in the hydrolysis process seriously corrodes reaction equipment, a large amount of heat is released, sodium formate is generated in the reaction process, the cost for separating the sodium formate is high, and in addition, the residual sodium formate in the extracted organic phase can promote the decomposition of the 1, 2-pentanediol during rectification. Document 2 also discloses a method for preparing 1, 2-pentanediol, in which calcium hydroxide is used to replace sodium hydroxide for neutralization hydrolysis, and through a series of processes of neutralization, hydrolysis, filtration, concentration, extraction, filtration, concentration and rectification, the total yield of 1, 2-pentanediol is 92.8%, and the purity is 99.5%. However, this method still has the same problems as in document 1.
Therefore, it is known that the research on the method for producing 1, 2-pentanediol in the prior art is not sufficient, and it is necessary to develop a production method with less environmental pollution and high safety of reaction operation, and a reaction system suitable for the production method.
Document 1: patent CN 1552684A;
document 2: improvement of hydrolysis neutralization process in production of 1, 2-pentanediol in zhanzhen kikai, dune yi jia, koelreun et al fine and specialty chemicals, 2004, 12 (24): 18-19.
Disclosure of Invention
Problem to be solved by utility model
In order to overcome the problems of complex operation and great environmental pollution of the preparation method of the 1, 2-pentanediol in the prior art, the utility model provides a reaction system for continuously preparing the 1, 2-pentanediol, the reaction system can implement a new preparation method of the 1, 2-pentanediol with small environmental pollution and high yield, on one hand, each step of reaction is thorough, the total yield is improved, on the other hand, the continuous production can be realized, and the production efficiency is greatly improved.
Means for solving the problems
The utility model provides a reaction system for preparing 1, 2-pentanediol in succession, reaction system includes: the device comprises a reactor, a hydrolysis device, an alcoholysis device, an extraction device, a distillation device and a rectification device, wherein a discharge hole of the reactor is connected with a feed inlet at the top of the hydrolysis device, a water inlet and a solid acid catalyst feeding hole are further formed in the top of the hydrolysis device, a discharge hole at the bottom of the hydrolysis device is connected with a feed inlet at the top of the alcoholysis device, an alcoholysis agent feed inlet is further formed in the top of the alcoholysis device, a discharge hole at the bottom of the alcoholysis device is connected with a feed inlet of the extraction device, a discharge hole at an organic layer of the extraction device is connected with a feed inlet of the distillation device, a discharge hole at a water layer of the extraction device is connected with a water inlet of the hydrolysis device, and a discharge hole.
According to the utility model discloses a reaction system for preparing 1, 2-pentanediol in succession, the hydrolysis unit with still be equipped with filter equipment between the alcoholysis device, mix in the filter equipment filtering hydrolysis reaction product the solid acid catalyst.
According to the utility model discloses a reaction system for preparing 1, 2-pentanediol in succession, the alcoholysis device still includes alcoholysis agent vaporization device, alcoholysis agent vaporization device with alcoholysis agent feed inlet links to each other.
According to a reaction system for preparing 1, 2-pentanediol in succession, be equipped with the alcoholysis agent spray tube of spiral arrangement on the alcoholysis device inner wall, the alcoholysis agent spray tube with alcoholysis agent vapourizing unit intercommunication, evenly distributed's orifice has on the pipe wall of alcoholysis agent spray tube.
According to the utility model discloses a reaction system for preparing 1, 2-pentanediol in succession, the reactor is tubular reactor.
Effect of the utility model
The reaction system for continuously preparing the 1, 2-pentanediol changes the alkaline hydrolysis mode of the intermediate product 1, 2-epoxypentane in the traditional method, adopts the hydrolysis and alcoholysis mode, and avoids the corrosion of strong alkali to equipment and potential safety hazard possibly caused by a large amount of heat release; in addition, the reaction system can realize the continuous preparation of the 1, 2-pentanediol, and the pure water used in the hydrolysis can be recycled, so that the environmental pollution is small.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of the specification, illustrate exemplary embodiments, features, and aspects of the present invention and, together with the description, serve to explain the principles of the invention.
Fig. 1 shows a schematic structural diagram of a reaction system for continuously preparing 1, 2-pentanediol according to an embodiment of the present invention.
Description of the reference numerals
1: reactor, 11: discharge port of reactor, 2: hydrolysis apparatus, 21: feed inlet of hydrolysis apparatus, 22: water inlet, 23: solid acid catalyst input port, 24: discharge gate of hydrolysis unit, 3: alcoholysis device, 31: feed inlet of alcoholysis unit, 32: alcoholysis agent feed inlet, 33: discharge port of alcoholysis device, 34: alcoholysis agent gasification, 4: an extraction device is arranged in the extraction device,
41: feed inlet of extraction device, 42: organic layer discharge port, 43: water layer discharge port, 5: distillation apparatus, 51: a feed inlet of the distillation apparatus; 52: discharge port of distillation apparatus, 6: rectification apparatus, 61: feed inlet of the rectification apparatus, 7: and (4) a filtering device.
Detailed Description
Various exemplary embodiments, features and aspects of the present invention will be described in detail below with reference to the accompanying drawings. In the drawings, like reference numbers can indicate functionally identical or similar elements. While the various aspects of the embodiments are presented in drawings, the drawings are not necessarily drawn to scale unless specifically indicated.
The word "exemplary" is used exclusively herein to mean "serving as an example, embodiment, or illustration. Any embodiment described herein as "exemplary" is not necessarily to be construed as preferred or advantageous over other embodiments.
Furthermore, in the following detailed description, numerous specific details are set forth in order to provide a better understanding of the present invention. It will be understood by those skilled in the art that the present invention may be practiced without some of these specific details. In some instances, methods, means, elements well known to those skilled in the art have not been described in detail so as not to obscure the present invention.
Example 1
Fig. 1 shows a schematic structural diagram of a reaction system for continuously preparing 1, 2-pentanediol according to an embodiment of the present invention. As shown in fig. 1, the reaction system includes: the device comprises a reactor 1, a hydrolysis device 2, an alcoholysis device 3, an extraction device 4, a distillation device 5 and a rectification device 6, wherein a discharge port 11 of the reactor 1 is connected with a feed port 21 of the hydrolysis device 2, the top of the hydrolysis device 2 is also provided with a water inlet 22 and a solid acid catalyst feeding port 23, a discharge port 24 of the hydrolysis device 2 is connected with a feed port 31 of the alcoholysis device 3, the top of the alcoholysis device 3 is also provided with an alcoholysis agent feed port 32, a discharge port 33 of the alcoholysis device 3 is connected with a feed port 41 of the extraction device 4, an organic layer discharge port 42 of the extraction device 4 is connected with a feed port 51 of the distillation device 5, a water layer discharge port 43 of the extraction device 4 is connected with the water inlet 22 of the hydrolysis device 2, and a discharge port 52 of the.
The raw material 1-pentene in the reactor 1 is subjected to oxidation reaction to generate an intermediate product 1, 2-cyclopentane epoxide, the intermediate product 1, 2-cyclopentane epoxide flows into the hydrolysis device 2, part of the intermediate product is catalyzed and hydrolyzed, then the intermediate product flows into the alcoholysis device 3 for alcoholysis, finally the 1, 2-cyclopentane epoxide is completely decomposed, and then the intermediate product is subjected to post-treatment and purification.
The reactor 1 in the utility model is a tubular reactor, a kettle type reactor and a tower type reactor. The tubular reactor is preferred because it has high volumetric efficiency (productivity per unit volume) due to low back mixing and is particularly suitable for use in applications where high conversion or series side reactions are required.
In this embodiment, a filtering device 7 is further disposed between the hydrolysis device 2 and the alcoholysis device 3, and the filtering device 7 filters the solid acid catalyst mixed in the hydrolysis reaction product.
In this embodiment, the alcoholysis device 3 further comprises an alcoholysis agent vaporization device 34, and the alcoholysis agent vaporization device 34 is connected to the alcoholysis agent feeding port 32. Further, an alcoholysis agent spray pipe (not shown) is arranged on the inner wall of the alcoholysis device 3 in a spiral arrangement, the alcoholysis agent spray pipe is communicated with the alcoholysis agent vaporization device 34, and spray holes (not shown) are uniformly distributed on the pipe wall of the alcoholysis agent spray pipe.
The above description is only for the specific embodiments of the present invention, but the protection scope of the present invention is not limited thereto, and any person skilled in the art can easily think of the changes or substitutions within the technical scope of the present invention, and all should be covered within the protection scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (5)
1. A reaction system for the continuous production of pentane-1, 2-diol, the reaction system comprising: the device comprises a reactor, a hydrolysis device, an alcoholysis device, an extraction device, a distillation device and a rectification device, wherein a discharge hole of the reactor is connected with a feed inlet of the hydrolysis device, a water inlet and a solid acid catalyst feeding hole are further formed in the top of the hydrolysis device, a discharge hole of the hydrolysis device is connected with the feed inlet of the alcoholysis device, an alcoholysis agent feed inlet is further formed in the top of the alcoholysis device, a discharge hole of the alcoholysis device is connected with a feed inlet of the extraction device, an organic layer discharge hole of the extraction device is connected with a feed inlet of the distillation device, a water layer discharge hole of the extraction device is connected with a water inlet of the hydrolysis device, and a discharge hole of the distillation device is connected with a feed inlet of the.
2. The reaction system for the continuous production of pentane-1, 2-diol according to claim 1, further comprising a filtration device disposed between the hydrolysis device and the alcoholysis device, wherein the filtration device filters off the solid acid catalyst mixed in the hydrolysis reaction product.
3. The reaction system for the continuous production of pentane-1, 2-diol according to claim 1, wherein the alcoholysis device further comprises an alcoholysis agent vaporization device, wherein the alcoholysis agent vaporization device is coupled to the alcoholysis agent feed port.
4. The reaction system for continuously preparing 1, 2-pentanediol according to claim 3, wherein an alcoholysis agent nozzle arranged in a spiral manner is disposed on an inner wall of the alcoholysis device, the alcoholysis agent nozzle is connected to the alcoholysis agent vaporization device, and the wall of the alcoholysis agent nozzle is provided with uniformly distributed nozzles.
5. The reaction system for the continuous production of pentane-1, 2-diol according to claim 1, wherein the reactor is a tubular reactor.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201921230583.1U CN210438664U (en) | 2019-07-31 | 2019-07-31 | Reaction system for continuously preparing 1, 2-pentanediol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201921230583.1U CN210438664U (en) | 2019-07-31 | 2019-07-31 | Reaction system for continuously preparing 1, 2-pentanediol |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN210438664U true CN210438664U (en) | 2020-05-01 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201921230583.1U Expired - Fee Related CN210438664U (en) | 2019-07-31 | 2019-07-31 | Reaction system for continuously preparing 1, 2-pentanediol |
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| Country | Link |
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| CN (1) | CN210438664U (en) |
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2019
- 2019-07-31 CN CN201921230583.1U patent/CN210438664U/en not_active Expired - Fee Related
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| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20200501 |