CN106467457B - Method for continuously producing 5-chloro-2-pentanone - Google Patents
Method for continuously producing 5-chloro-2-pentanone Download PDFInfo
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- CN106467457B CN106467457B CN201610756869.8A CN201610756869A CN106467457B CN 106467457 B CN106467457 B CN 106467457B CN 201610756869 A CN201610756869 A CN 201610756869A CN 106467457 B CN106467457 B CN 106467457B
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- 238000000034 method Methods 0.000 title claims abstract description 68
- XVRIEWDDMODMGA-UHFFFAOYSA-N 5-chloropentan-2-one Chemical compound CC(=O)CCCCl XVRIEWDDMODMGA-UHFFFAOYSA-N 0.000 title claims abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 65
- 238000010533 azeotropic distillation Methods 0.000 claims abstract description 62
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 59
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims abstract description 43
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims abstract description 43
- 239000007789 gas Substances 0.000 claims abstract description 37
- 239000000463 material Substances 0.000 claims abstract description 36
- 238000006243 chemical reaction Methods 0.000 claims abstract description 30
- JSHPTIGHEWEXRW-UHFFFAOYSA-N 5-hydroxypentan-2-one Chemical compound CC(=O)CCCO JSHPTIGHEWEXRW-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000005660 chlorination reaction Methods 0.000 claims abstract description 23
- 230000018044 dehydration Effects 0.000 claims abstract description 16
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 16
- 238000005191 phase separation Methods 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 230000035484 reaction time Effects 0.000 claims abstract description 8
- BGTOWKSIORTVQH-UHFFFAOYSA-N cyclopentanone Chemical compound O=C1CCCC1 BGTOWKSIORTVQH-UHFFFAOYSA-N 0.000 claims description 18
- 239000012024 dehydrating agents Substances 0.000 claims description 17
- 238000000926 separation method Methods 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 13
- 239000000047 product Substances 0.000 claims description 11
- 239000012043 crude product Substances 0.000 claims description 10
- 238000007872 degassing Methods 0.000 claims description 8
- 238000009826 distribution Methods 0.000 claims description 8
- 239000010410 layer Substances 0.000 claims description 8
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 7
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 7
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 239000002808 molecular sieve Substances 0.000 claims description 7
- 239000012044 organic layer Substances 0.000 claims description 7
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 7
- 238000010025 steaming Methods 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 2
- 239000000945 filler Substances 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 14
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 8
- 239000002351 wastewater Substances 0.000 description 8
- 238000005265 energy consumption Methods 0.000 description 5
- 239000010865 sewage Substances 0.000 description 5
- 238000011049 filling Methods 0.000 description 4
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 3
- VQKFNUFAXTZWDK-UHFFFAOYSA-N 2-Methylfuran Chemical compound CC1=CC=CO1 VQKFNUFAXTZWDK-UHFFFAOYSA-N 0.000 description 2
- 239000012295 chemical reaction liquid Substances 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 239000000543 intermediate Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- FYSNRJHAOHDILO-UHFFFAOYSA-N thionyl chloride Chemical compound ClS(Cl)=O FYSNRJHAOHDILO-UHFFFAOYSA-N 0.000 description 2
- HVCFCNAITDHQFX-UHFFFAOYSA-N 1-cyclopropylethanone Chemical compound CC(=O)C1CC1 HVCFCNAITDHQFX-UHFFFAOYSA-N 0.000 description 1
- OMQHDIHZSDEIFH-UHFFFAOYSA-N 3-Acetyldihydro-2(3H)-furanone Chemical compound CC(=O)C1CCOC1=O OMQHDIHZSDEIFH-UHFFFAOYSA-N 0.000 description 1
- BGCWDXXJMUHZHE-UHFFFAOYSA-N 5-methyl-2,3-dihydrofuran Chemical compound CC1=CCCO1 BGCWDXXJMUHZHE-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 125000001309 chloro group Chemical group Cl* 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- NPTDXPDGUHAFKC-UHFFFAOYSA-N ethynylcyclopropane Chemical group C#CC1CC1 NPTDXPDGUHAFKC-UHFFFAOYSA-N 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- UHZYTMXLRWXGPK-UHFFFAOYSA-N phosphorus pentachloride Chemical compound ClP(Cl)(Cl)(Cl)Cl UHZYTMXLRWXGPK-UHFFFAOYSA-N 0.000 description 1
- FAIAAWCVCHQXDN-UHFFFAOYSA-N phosphorus trichloride Chemical compound ClP(Cl)Cl FAIAAWCVCHQXDN-UHFFFAOYSA-N 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000007142 ring opening reaction Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/61—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by reactions not involving the formation of >C = O groups
- C07C45/63—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by reactions not involving the formation of >C = O groups by introduction of halogen; by substitution of halogen atoms by other halogen atoms
Abstract
A method for continuously producing 5-chloro-2-pentanone, belonging to the technical field of organic synthesis process. The method is characterized in that: comprises the working procedures of chlorination reaction, azeotropic distillation, oil-water phase separation and dehydration; in the chlorination reaction procedure, hydrogen chloride gas enters from the bottom of the reactor (1), 3-acetyl propanol enters from the top of the reactor (1), the reaction temperature in the reactor (1) is 48-55 ℃, the reaction pressure is 0.3-0.5 MPa, and the material mixing reaction time is 165-180 min; after the materials are fully mixed and reacted, the materials at the bottom of the reactor (1) are conveyed into an azeotropic distillation tower (3). The invention takes hydrogen chloride gas as the chlorination raw material, the hydrogen chloride gas enters from the bottom of the reactor, 3-acetyl propanol enters from the top of the reactor, the hydrogen chloride gas and the 3-acetyl propanol are fully mixed in the counter-current process and then fall into the bottom of the reactor together for chlorination reaction.
Description
Technical Field
A method for continuously producing 5-chloro-2-pentanone, belonging to the technical field of organic synthesis process.
Background
5-chloro-2-pentanone is an organic synthesis intermediate, is widely used as an important raw material for producing substances such as cyclopropyl methyl ketone, cyclopropyl acetylene and the like, and is widely used for synthesizing intermediates for producing medicines, pesticides and the like. In the prior art, acetyl butyrolactone is used as a raw material to perform chlorination reaction with hydrochloric acid to prepare 5-chloro-2-pentanone. Or hydrogenating 2-methylfuran to produce 2-methyl-4, 5-dihydrofuran, and then performing ring opening and chlorination with hydrochloric acid to produce 5-chloro-2-pentanone. However, in the prior art, hydrochloric acid is used as a chlorine substitute source, wherein the hydrochloric acid is rich in 70% of water, and has the phenomena of generation of a large amount of high-chlorine wastewater after chlorination, high post-treatment difficulty, poor economy of chlorine atoms, unstable product quality and the like. In a more traditional process, thionyl chloride, phosphorus trichloride, phosphorus pentachloride and the like are taken as chlorination reagents, and the phenomena of more side reactions, difficulty in treatment of waste water, waste gas and the like are caused; these problems are urgently needed to be solved.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: overcomes the defects of the prior art and provides a method for continuously producing 5-chloro-2-pentanone, which reduces the consumption of raw materials.
The technical scheme adopted by the invention for solving the technical problems is as follows: the method for continuously producing the 5-chloro-2-pentanone is characterized by comprising the following steps: the production system comprises a reactor, an azeotropic distillation tower, a condenser, a layering tank, a water diversion tank, a dehydration tower and a finished product degassing kettle, wherein material inlets are respectively formed in the top and the bottom of the reactor, and the preparation steps comprise chlorination reaction, azeotropic distillation, oil-water phase separation and dehydration;
in the chlorination reaction procedure, hydrogen chloride gas enters from the bottom of a reactor, 3-acetyl propanol enters from the top of the reactor, the reaction temperature in the reactor is 48-55 ℃, the reaction pressure is 0.3-0.5 MPa, and the material mixing reaction time is 165-180 min; after the materials are fully mixed and reacted, the materials at the bottom of the reactor are conveyed into an azeotropic distillation tower;
in the azeotropic distillation process, the mixture containing the material and the water from the reactor is distilled by an azeotropic distillation tower; condensing the distillate at the top of the azeotropic distillation tower through a condenser, and then feeding the distillate into a water separation tank to perform an oil-water phase separation process; and the lower organic layer of the water diversion tank enters a dehydrating tower filled with dehydrating agent for dehydrating.
The invention takes hydrogen chloride gas as the chlorination raw material, the hydrogen chloride gas enters from the bottom of the reactor, 3-acetyl propanol enters from the top of the reactor, the hydrogen chloride gas and the 3-acetyl propanol are fully mixed in the counter-current process and then fall into the bottom of the reactor together for chlorination reaction. The reaction of gas and liquid generally needs the continuous introduction of gas, and can not carry out long-time common reaction, the invention designs that hydrogen chloride gas enters from the bottom, 3-acetyl propanol enters from the top, the two can be fully contacted and mixed in the filling section of the reactor, and then lower reaction temperature is kept, and the escape of the hydrogen chloride gas is prevented as much as possible; and then the azeotropic distillation process, the oil-water phase separation process and the dehydration process are carried out, the invention realizes the one-time feeding of the gas reaction raw materials, the continuous reaction can be realized, the product with stable quality can be obtained, and the higher yield is achieved. .
Preferably, the residual liquid at the bottom of the azeotropic distillation tower is distilled under vacuum to recover the crude product with low content of the cyclopentanone. And (3) pumping the residual liquid at the bottom of the azeotropic tower to a storage tank for centralized collection, and then distilling under high vacuum to recover a low-content crude product of the cyclopentanone. For a small amount of residual liquid at the bottom of the azeotropic distillation tower, the method is used for distilling and recovering under a certain vacuum condition, the boiling point temperature difference of materials is enlarged by utilizing the vacuum condition, the operation is convenient, and a small amount of cyclopentanone can be recovered.
The dehydrating agent in the dehydrating tower is anhydrous sodium sulfate, anhydrous magnesium sulfate or a molecular sieve. The dehydrating agent in the dehydrating tower can absorb a small amount of moisture in the materials, and the quality of the 5-chloro-2-pentanone is ensured.
Preferably, the dehydrating agent in the dehydrating tower is anhydrous calcium chloride.
Preferably, the water solution rich in hydrogen chloride at the upper layer of the water separation tank is conveyed back to the top of the reactor. The water solution rich in hydrogen chloride separated by the water separation tank directly returns to the top of the reactor, the water solution rich in hydrogen chloride falls down together with the 3-acetyl propanol, and the rising hydrogen chloride gas is absorbed in the packing layer, so that the utilization rate of the hydrogen chloride is increased.
Preferably, the working pressure of the azeotropic distillation tower is-0.09 MPa to-0.08 MPa, and the working temperature is 90 ℃ to 95 ℃. The distillation efficiency of the azeotropic distillation tower needs to be adapted to the reaction rate in the reactor, and in order to adapt to the reaction rate, the reaction conditions are controlled to be-0.09 MPa to-0.08 MPa and 90-95 ℃ so that the reaction product, water and contained hydrogen chloride can be distilled out together, and then the water and the hydrogen chloride are separated through an oil-water phase separation process, so that the overall process rate is improved.
Preferably, the reactor used in the chlorination reaction process is a tower reactor or a kettle reactor with a steaming section of tower. For providing a sufficiently long gas-liquid contact section.
The production system comprises a reactor, an azeotropic distillation tower, a condenser, a layering tank, a water diversion tank, a dehydration tower and a finished product degassing kettle, wherein the top and the bottom of the reactor are respectively provided with a material inlet. The bottom pipeline of the reactor is connected to the middle filling area of the azeotropic distillation tower, the top of the azeotropic distillation tower is sequentially connected with a condenser, a layering tank and a water diversion tank, the bottom of the water diversion tank is connected to the middle section of the dehydration tower, the middle upper part of the water diversion tank is connected to the top of the reactor through a return pipeline, and the upper part of the dehydration tower is connected with a finished product degassing kettle. The device of the invention realizes the direct reaction of gas and liquid, does not need to use hydrochloric acid with high water content, and reduces the fertilizer emission.
Compared with the prior art, the method for continuously producing 5-chloro-2-pentanone has the beneficial effects that: the invention takes hydrogen chloride gas as the chlorination raw material, the hydrogen chloride gas enters from the bottom of the reactor, 3-acetyl propanol enters from the top of the reactor, the hydrogen chloride gas and the 3-acetyl propanol are fully mixed in the counter-current process and then fall into the bottom of the reactor together for chlorination reaction. The reaction of gas and liquid generally needs continuous introduction of gas, and cannot carry out long-time common reaction, the hydrogen chloride gas and the 3-acetyl propanol can be fully contacted and mixed in a filling section of a reactor, then the reaction temperature is kept low, and the escape of the hydrogen chloride gas is prevented as much as possible. Then the azeotropic distillation process, the oil-water phase separation process and the dehydration process are carried out. The raw material of the process adopts hydrogen chloride gas to replace 30 percent hydrochloric acid, and a continuous process is adopted. The invention can reduce the energy consumption by more than 60 percent, and the sewage in the whole process is reduced by 80 percent.
Drawings
FIG. 1 is a schematic view of a production system of a method for continuously producing 5-chloro-2-pentanone according to the present invention.
Wherein, the device comprises a reactor 1, a reactor 2, a reaction liquid discharge pump 3, an azeotropic distillation tower 4, a rich hydrochloric acid recovery pump 5, a condenser 6, a layering tank 7, a water separation tank 8, a crude product discharge pump 9, a dehydration tower 10 and a finished product degassing kettle.
Detailed Description
Referring to figure 1: the invention relates to a production system of a method for continuously producing 5-chloro-2-pentanone, which comprises the following steps: the device comprises a reactor 1, an azeotropic distillation tower 3, a condenser 5, a layering tank 6, a water diversion tank 7, a dehydration tower 9 and a finished product degassing kettle 10, wherein a 3-acetyl propanol inlet pipe is arranged at the top of the reactor 1, a hydrogen chloride gas adding pipe is arranged at the bottom of the reactor 1, the bottom of the reactor 1 is connected to a middle filling area of the azeotropic distillation tower 3 through a pipeline provided with a reaction liquid discharging pump 2, the top of the azeotropic distillation tower 3 is sequentially connected with the condenser 5, the layering tank 6 and the water diversion tank 7, the bottom of the water diversion tank 7 is connected to the middle section of the dehydration tower 9 through a pipeline provided with a crude product discharging pump 8, the middle upper part of the water diversion tank 7 is connected to the top of the reactor 1 through a return pipeline provided with a rich hydrochloric acid recovery pump 4, and the upper part of.
The method for continuously producing 5-chloro-2-pentanone according to the present invention is further described below with reference to specific examples, of which example 1 is the most preferred example.
Example 1
The reactor 1 used in the chlorination reaction procedure is a tower reactor or a kettle reactor with a steaming section of tower; hydrogen chloride gas enters from the bottom of the reactor 1 at a speed of 38kg/h, 2000kg of 3-acetyl propanol enters from the top of the reactor 1 at a speed of 200kg/h, the reaction temperature in the reactor 1 is 50 ℃, the reaction pressure is 0.4MPa, and the material mixing reaction time is 172 min; after the materials are fully mixed and reacted, the materials at the bottom of the reactor 1 are conveyed into an azeotropic distillation tower 3;
in the azeotropic distillation process, the mixture containing the material and the water from the reactor 1 is distilled by an azeotropic distillation tower 3; the working pressure of the azeotropic distillation tower 3 is-0.08 MPa, the working temperature is 92 ℃, distillate at the top of the azeotropic distillation tower 3 is condensed by a condenser 5 and then enters a water separation tank 7 for oil-water phase separation, and the water solution rich in hydrogen chloride at the upper layer of the water separation tank 7 is conveyed back to the top of the reactor 1; distilling the residual liquid at the bottom of the azeotropic distillation tower 3 under vacuum to recover a low-content cyclopentanone crude product, feeding the lower organic layer of the water distribution tank 7 into a dehydrating tower 9 filled with a dehydrating agent for dehydrating, wherein the dehydrating agent in the dehydrating tower 9 is anhydrous calcium chloride, anhydrous sodium sulfate, anhydrous magnesium sulfate or a molecular sieve;
the unit consumption of 3-acetyl propanol raw materials for producing 1 ton of 97.5 percent 5-chloro-2-pentanone is lower than 0.87t, the hydrogen chloride gas is 0.32t, the steam is 1.2t, the produced wastewater is 0.2t, the energy consumption is reduced by 61 percent in the embodiment, and the sewage is reduced by 82 percent in the whole process.
Example 2
The reactor 1 used in the chlorination reaction procedure is a tower reactor or a kettle reactor with a steaming section of tower; hydrogen chloride gas enters from the bottom of the reactor 1 at the speed of 38kg/h, 2000kg of 3-acetyl propanol enters from the top of the reactor 1 at the speed of 200kg/h, the reaction temperature in the reactor 1 is 52 ℃, the reaction pressure is 0.35MPa, and the material mixing reaction time is 176 min; after the materials are fully mixed and reacted, the materials at the bottom of the reactor 1 are conveyed into an azeotropic distillation tower 3;
in the azeotropic distillation process, the mixture containing the material and the water from the reactor 1 is distilled by an azeotropic distillation tower 3; the working pressure of the azeotropic distillation tower 3 is-0.08 MPa, the working temperature is 94 ℃, distillate at the top of the azeotropic distillation tower 3 is condensed by a condenser 5 and then enters a water separation tank 7 for oil-water phase separation, and the water solution rich in hydrogen chloride at the upper layer of the water separation tank 7 is conveyed back to the top of the reactor 1; distilling the residual liquid at the bottom of the azeotropic distillation tower 3 under vacuum to recover a low-content cyclopentanone crude product, feeding the lower organic layer of the water distribution tank 7 into a dehydrating tower 9 filled with a dehydrating agent for dehydrating, wherein the dehydrating agent in the dehydrating tower 9 is anhydrous calcium chloride, anhydrous sodium sulfate, anhydrous magnesium sulfate or a molecular sieve;
the unit consumption of 3-acetyl propanol raw materials for producing 1 ton of 97.5 percent 5-chloro-2-pentanone is lower than 0.88t, the hydrogen chloride gas is 0.32t, the steam is 1.2t, and the produced wastewater is 0.2 t.
Example 3
The reactor 1 used in the chlorination reaction procedure is a tower reactor or a kettle reactor with a steaming section of tower; hydrogen chloride gas enters from the bottom of the reactor 1 at a speed of 38kg/h, 2000kg of 3-acetyl propanol enters from the top of the reactor 1 at a speed of 200kg/h, the reaction temperature in the reactor 1 is 49 ℃, the reaction pressure is 0.45MPa, and the material mixing reaction time is 168 min; after the materials are fully mixed and reacted, the materials at the bottom of the reactor 1 are conveyed into an azeotropic distillation tower 3;
in the azeotropic distillation process, the mixture containing the material and the water from the reactor 1 is distilled by an azeotropic distillation tower 3; the working pressure of the azeotropic distillation tower 3 is-0.09 MPa, the working temperature is 91 ℃, distillate at the top of the azeotropic distillation tower 3 is condensed by a condenser 5 and then enters a water separation tank 7 for oil-water phase separation, and the water solution rich in hydrogen chloride at the upper layer of the water separation tank 7 is conveyed back to the top of the reactor 1; distilling the residual liquid at the bottom of the azeotropic distillation tower 3 under vacuum to recover a low-content cyclopentanone crude product, feeding the lower organic layer of the water distribution tank 7 into a dehydrating tower 9 filled with a dehydrating agent for dehydrating, wherein the dehydrating agent in the dehydrating tower 9 is anhydrous calcium chloride, anhydrous sodium sulfate, anhydrous magnesium sulfate or a molecular sieve;
the unit consumption of 3-acetyl propanol raw materials for producing 1 ton of 97.5 percent 5-chloro-2-pentanone is lower than 0.88t, the hydrogen chloride gas is 0.32t, the steam is 1.2t, and the produced wastewater is 0.2t, compared with the existing aluminum hydroxide method, the method reduces the energy consumption by 60 percent, and the sewage in the whole process is reduced by 80 percent.
Example 4
The reactor 1 used in the chlorination reaction procedure is a tower reactor or a kettle reactor with a steaming section of tower; hydrogen chloride gas enters from the bottom of the reactor 1 at the speed of 38kg/h, 2000kg of 3-acetyl propanol enters from the top of the reactor 1 at the speed of 200kg/h, the reaction temperature in the reactor 1 is 48 ℃, the reaction pressure is 0.5MPa, and the material mixing reaction time is 180 min; after the materials are fully mixed and reacted, the materials at the bottom of the reactor 1 are conveyed into an azeotropic distillation tower 3;
in the azeotropic distillation process, the mixture containing the material and the water from the reactor 1 is distilled by an azeotropic distillation tower 3; the working pressure of the azeotropic distillation tower 3 is-0.09 MPa, the working temperature is 90 ℃, distillate at the top of the azeotropic distillation tower 3 is condensed by a condenser 5 and then enters a water separation tank 7 for oil-water phase separation, and an aqueous solution rich in hydrogen chloride at the upper layer of the water separation tank 7 is conveyed back to the top of the reactor 1; distilling the residual liquid at the bottom of the azeotropic distillation tower 3 under vacuum to recover a low-content cyclopentanone crude product, feeding the lower organic layer of the water distribution tank 7 into a dehydrating tower 9 filled with a dehydrating agent for dehydrating, wherein the dehydrating agent in the dehydrating tower 9 is anhydrous calcium chloride, anhydrous sodium sulfate, anhydrous magnesium sulfate or a molecular sieve;
the unit consumption of 3-acetyl propanol raw material for producing 1 ton of 97.5 percent 5-chloro-2-pentanone is lower than 0.89t, the hydrogen chloride gas is 0.33t, the steam is 1.25t, and the produced wastewater is 0.21t, compared with the existing aluminum hydroxide method, the method reduces the energy consumption by 59.5 percent, and the sewage in the whole process is reduced by 80 percent.
Example 5
The reactor 1 used in the chlorination reaction procedure is a tower reactor or a kettle reactor with a steaming section of tower; hydrogen chloride gas enters from the bottom of the reactor 1 at a speed of 38kg/h, 2000kg of 3-acetyl propanol enters from the top of the reactor 1 at a speed of 200kg/h, the reaction temperature in the reactor 1 is 55 ℃, the reaction pressure is 0.3MPa, and the material mixing reaction time is 165 min; after the materials are fully mixed and reacted, the materials at the bottom of the reactor 1 are conveyed into an azeotropic distillation tower 3;
in the azeotropic distillation process, the mixture containing the material and the water from the reactor 1 is distilled by an azeotropic distillation tower 3; the working pressure of the azeotropic distillation tower 3 is-0.08 MPa, the working temperature is 95 ℃, distillate at the top of the azeotropic distillation tower 3 is condensed by a condenser 5 and then enters a water separation tank 7 for oil-water phase separation, and the water solution rich in hydrogen chloride at the upper layer of the water separation tank 7 is conveyed back to the top of the reactor 1; distilling the residual liquid at the bottom of the azeotropic distillation tower 3 under vacuum to recover a low-content cyclopentanone crude product, feeding the lower organic layer of the water distribution tank 7 into a dehydrating tower 9 filled with a dehydrating agent for dehydrating, wherein the dehydrating agent in the dehydrating tower 9 is anhydrous calcium chloride, anhydrous sodium sulfate, anhydrous magnesium sulfate or a molecular sieve;
compared with the existing aluminum hydroxide method, the unit consumption of 3-acetyl propanol raw materials for producing 1 ton of 97.5 percent 5-chloro-2-pentanone is lower than 0.89t, the hydrogen chloride gas is 0.33t, the steam is 1.3t, and the produced wastewater is 0.22t, the energy consumption of the embodiment is reduced by 59 percent, and the sewage in the whole process is reduced by 80 percent.
Comparative example 1
The basic process flow and process conditions are the same as in example 1, except that the reaction temperature in the reactor 1 is 95 ℃, the reaction pressure is 0.4MPa, the unit consumption of 3-acetylacetone raw material for producing 1 ton of 97.5 percent 5-chloro-2-pentanone is lower than 0.96t, the hydrogen chloride gas is 0.39t, the steam is 1.8t, and the produced wastewater is 0.33 t.
Comparative example 2
The basic process flow and process conditions are the same as those in example 1, except that the working pressure of the azeotropic distillation tower 3 is-0.03 MPa, the working temperature is 75 ℃, the distillation rate is too slow to reach the vaporization temperature of 5-chloro-2-pentanone, and the process cannot be continuously carried out.
The foregoing is directed to preferred embodiments of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow. However, any simple modification, equivalent change and modification of the above embodiments according to the technical essence of the present invention are within the protection scope of the technical solution of the present invention.
Claims (7)
1. A method for continuously producing 5-chloro-2-pentanone is characterized by comprising the following steps: the production system comprises a reactor (1), an azeotropic distillation tower (3), a condenser (5), a layering tank (6), a water distribution tank (7), a dehydration tower (9) and a finished product degassing kettle (10), wherein the top and the bottom of the reactor (1) are respectively provided with a material inlet, and the preparation steps comprise chlorination reaction, azeotropic distillation, oil-water phase separation and dehydration;
in the chlorination reaction procedure, hydrogen chloride gas enters from the bottom of the reactor (1), 3-acetyl propanol enters from the top of the reactor (1), the reaction temperature in the reactor (1) is 48-55 ℃, the reaction pressure is 0.3-0.5 MPa, and the material mixing reaction time is 165-180 min; after the materials are fully mixed and reacted, the materials at the bottom of the reactor (1) are conveyed into an azeotropic distillation tower (3);
in the azeotropic distillation process, the mixture containing the material and the water from the reactor (1) is distilled by an azeotropic distillation tower (3); condensing distillate at the tower top of the azeotropic distillation tower (3) by a condenser (5), then entering a layering tank (6), then entering a water distribution tank (7) for oil-water phase splitting, entering a dehydrating tower (9) filled with a dehydrating agent for dehydrating at the lower organic layer of the water distribution tank (7), and entering an upper finished product after dehydration into a finished product degassing kettle (10) for removing hydrogen chloride gas;
and distilling the residual liquid at the bottom of the azeotropic distillation tower (3) under vacuum to recover a low-content cyclopentanone crude product.
2. The method for continuously producing 5-chloro-2-pentanone according to claim 1, characterized in that: the dehydrating agent in the dehydrating tower (9) is anhydrous sodium sulfate, anhydrous magnesium sulfate or a molecular sieve.
3. The method for continuously producing 5-chloro-2-pentanone according to claim 1, characterized in that: the dehydrating agent in the dehydrating tower (9) is anhydrous calcium chloride.
4. The method for continuously producing 5-chloro-2-pentanone according to claim 1, characterized in that: the water solution rich in hydrogen chloride at the upper layer of the water separation tank (7) is conveyed back to the top of the reactor (1).
5. The method for continuously producing 5-chloro-2-pentanone according to claim 1, characterized in that: the working pressure of the azeotropic distillation tower (3) is-0.09 MPa to-0.08 MPa, and the working temperature is 90 ℃ to 95 ℃.
6. The method for continuously producing 5-chloro-2-pentanone according to claim 1, characterized in that: the reactor (1) used in the chlorination reaction procedure is a tower reactor or a kettle reactor with a steaming section of tower.
7. The method for continuously producing 5-chloro-2-pentanone according to claim 1, characterized in that: the bottom pipeline of reactor (1) be connected to the middle part filler district of azeotropic distillation tower (3), the top of the tower of azeotropic distillation tower (3) connects gradually condenser (5), layering jar (6) and knockout drum (7), the bottom of knockout drum (7) is connected to dehydration tower (9) middle section, the well upper portion of knockout drum (7) is connected to reactor (1) top through returning the pipeline, finished product degasification cauldron (10) is connected on the upper portion of dehydration tower (9).
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| WO1999044979A1 (en) * | 1998-03-03 | 1999-09-10 | Great Lakes Chemical Corporation | An aqueous method to prepare cyclopropyl methylketone from acetyl-propanol |
| CN1994996A (en) * | 2006-12-05 | 2007-07-11 | 安徽绩溪县徽煌化工有限公司 | Process for preparing cyclopropyl methyl ketone |
| CN203728742U (en) * | 2014-03-13 | 2014-07-23 | 张家港市振方化工有限公司 | Equipment for preparing chloropivaloyl pentane |
| CN104447247A (en) * | 2014-11-27 | 2015-03-25 | 苏州乔纳森新材料科技有限公司 | Synthesizing method of drug intermediate 5-chloro-2-pentanone |
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| WO1999044979A1 (en) * | 1998-03-03 | 1999-09-10 | Great Lakes Chemical Corporation | An aqueous method to prepare cyclopropyl methylketone from acetyl-propanol |
| CN1994996A (en) * | 2006-12-05 | 2007-07-11 | 安徽绩溪县徽煌化工有限公司 | Process for preparing cyclopropyl methyl ketone |
| CN203728742U (en) * | 2014-03-13 | 2014-07-23 | 张家港市振方化工有限公司 | Equipment for preparing chloropivaloyl pentane |
| CN104447247A (en) * | 2014-11-27 | 2015-03-25 | 苏州乔纳森新材料科技有限公司 | Synthesizing method of drug intermediate 5-chloro-2-pentanone |
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