CN113968839A - Preparation method of ketone compound - Google Patents
Preparation method of ketone compound Download PDFInfo
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- CN113968839A CN113968839A CN202111085842.8A CN202111085842A CN113968839A CN 113968839 A CN113968839 A CN 113968839A CN 202111085842 A CN202111085842 A CN 202111085842A CN 113968839 A CN113968839 A CN 113968839A
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- plate
- cooling
- ketone
- outer side
- water tank
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- 238000002360 preparation method Methods 0.000 title claims description 10
- -1 ketone compound Chemical class 0.000 title claims description 5
- 238000001816 cooling Methods 0.000 claims abstract description 104
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 61
- 150000002576 ketones Chemical class 0.000 claims abstract description 35
- 238000000034 method Methods 0.000 claims abstract description 16
- 238000004519 manufacturing process Methods 0.000 claims abstract description 10
- 230000000149 penetrating effect Effects 0.000 claims abstract 2
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 63
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 33
- 238000003756 stirring Methods 0.000 claims description 26
- 238000006243 chemical reaction Methods 0.000 claims description 24
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 21
- 238000010438 heat treatment Methods 0.000 claims description 20
- 238000002425 crystallisation Methods 0.000 claims description 17
- 230000008025 crystallization Effects 0.000 claims description 17
- 238000009833 condensation Methods 0.000 claims description 15
- 230000005494 condensation Effects 0.000 claims description 15
- RMVRSNDYEFQCLF-UHFFFAOYSA-N thiophenol Chemical compound SC1=CC=CC=C1 RMVRSNDYEFQCLF-UHFFFAOYSA-N 0.000 claims description 15
- 239000000047 product Substances 0.000 claims description 11
- WNZQDUSMALZDQF-UHFFFAOYSA-N 2-benzofuran-1(3H)-one Chemical compound C1=CC=C2C(=O)OCC2=C1 WNZQDUSMALZDQF-UHFFFAOYSA-N 0.000 claims description 10
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- WQDUMFSSJAZKTM-UHFFFAOYSA-N Sodium methoxide Chemical compound [Na+].[O-]C WQDUMFSSJAZKTM-UHFFFAOYSA-N 0.000 claims description 10
- 150000001875 compounds Chemical class 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 10
- 238000012360 testing method Methods 0.000 claims description 10
- 239000012043 crude product Substances 0.000 claims description 8
- 229920000137 polyphosphoric acid Polymers 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 7
- 238000001704 evaporation Methods 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 5
- 238000003916 acid precipitation Methods 0.000 claims description 5
- 229910052799 carbon Inorganic materials 0.000 claims description 5
- 239000000706 filtrate Substances 0.000 claims description 5
- 230000007062 hydrolysis Effects 0.000 claims description 5
- 238000006460 hydrolysis reaction Methods 0.000 claims description 5
- 238000004806 packaging method and process Methods 0.000 claims description 5
- 239000003208 petroleum Substances 0.000 claims description 5
- 238000007670 refining Methods 0.000 claims description 5
- 238000006798 ring closing metathesis reaction Methods 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 239000002994 raw material Substances 0.000 abstract description 12
- 239000013078 crystal Substances 0.000 abstract description 8
- 238000004321 preservation Methods 0.000 description 16
- 239000000243 solution Substances 0.000 description 9
- 230000000694 effects Effects 0.000 description 7
- 239000005457 ice water Substances 0.000 description 6
- 238000010992 reflux Methods 0.000 description 6
- 239000000758 substrate Substances 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000007599 discharging Methods 0.000 description 3
- 238000009434 installation Methods 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 230000007935 neutral effect Effects 0.000 description 3
- 238000005070 sampling Methods 0.000 description 3
- 238000010025 steaming Methods 0.000 description 3
- 238000000967 suction filtration Methods 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 239000000498 cooling water Substances 0.000 description 2
- 239000012047 saturated solution Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D335/00—Heterocyclic compounds containing six-membered rings having one sulfur atom as the only ring hetero atom
- C07D335/04—Heterocyclic compounds containing six-membered rings having one sulfur atom as the only ring hetero atom condensed with carbocyclic rings or ring systems
- C07D335/10—Dibenzothiopyrans; Hydrogenated dibenzothiopyrans
- C07D335/12—Thioxanthenes
- C07D335/14—Thioxanthenes with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached in position 9
- C07D335/16—Oxygen atoms, e.g. thioxanthones
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0004—Crystallisation cooling by heat exchange
- B01D9/0013—Crystallisation cooling by heat exchange by indirect heat exchange
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/005—Selection of auxiliary, e.g. for control of crystallisation nuclei, of crystal growth, of adherence to walls; Arrangements for introduction thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D2009/0086—Processes or apparatus therefor
Abstract
The invention discloses a method for preparing a ketone, which relates to the technical field of production of the ketone, and comprises a bottom plate, wherein support plates are respectively arranged on the upper end surface of the bottom plate close to two sides, bearing plates are arranged at the upper ends of the support plates, a cooling barrel is arranged between the two groups of bearing plates, a cooling mechanism is arranged above the cooling barrel, a collecting mechanism is arranged on the upper end surface of the bottom plate and between the two groups of support plates, a funnel is arranged on the bottom surface of the cooling barrel, a water tank is arranged on one side of the bottom plate, the cooling mechanism comprises a vertical plate, a vertical groove is formed in the outer side surface of the vertical plate in a penetrating manner, a sliding block is arranged in the vertical groove, an electric telescopic rod is arranged between the inner side wall of the vertical groove and the outer side surface of the sliding block, a transverse plate is arranged between the two groups of sliding blocks, and a cooling fan is arranged on the bottom surface of the transverse plate; the invention can accelerate the cooling speed of the raw materials and is convenient for workers to collect crystals.
Description
Technical Field
The invention relates to the technical field of ketone substrate production, in particular to a preparation method of a ketone substrate.
Background
The ketone base material needs to be cooled and crystallized on a raw material during the production, and the cooling crystallization is a method for crystallizing a saturated solution, a solute is precipitated from the solution in the form of crystals by a method of reducing the temperature, and the method is suitable for the substances with obviously increased solubility along with the increase of the temperature, and the saturated solution is reduced in temperature under the condition of relatively high temperature, so that the crystals are precipitated.
Through search, chinese patent No. CN202021942533.9 discloses a crystallization cooling device, which can adjust the position of the cooling device according to the melting material and melting parameter, so as to meet the crystallization requirements under different materials and melting parameters, and achieve the preparation of products with different grain sizes.
Disclosure of Invention
The present invention is directed to a method for preparing ketone compound, which solves the above problems of the prior art.
In order to achieve the above purpose, the invention provides the following technical scheme:
a method of making a ketone, the method comprising:
step S001: by acid precipitation of condensation
Putting sodium methoxide and thiophenol into a reaction kettle, stirring, cooling to room temperature, putting phthalide into the reaction kettle in portions, and evaporating methanol under reduced pressure; adding water to dissolve the mixture, and then dropwise adding hydrochloric acid to adjust the pH value of the solution to 1-2; then adding toluene, heating to dissolve to 65-75 ℃, and removing a lower acid water layer to obtain a condensation compound;
step S002: ring closure hydrolysis
Putting polyphosphoric acid into a reaction kettle, stirring, pouring a preheated condensation compound, heating to 115-120 ℃ after adding, recovering toluene under reduced pressure, and immediately separating out black granular solid through a cooling crystallization device after the test is qualified to crystallize the black granular solid into a ketone crude product;
step S003: refining
Respectively putting toluene and crude ketone products into a reaction kettle, stirring, and standing for 30 minutes for layering; adding activated carbon, stirring, filtering to remove carbon, cooling and crystallizing the filtrate by a cooling and crystallizing device, rinsing with petroleum ether after filtering, drying in vacuum, taking out after testing is qualified, drying and packaging to obtain a finished product;
the cooling crystallization device comprises a bottom plate, wherein supporting plates are arranged on the upper end surface of the bottom plate close to the two sides, bearing plates are arranged on the upper ends of the supporting plates, a cooling barrel is arranged between the two groups of bearing plates, a cooling mechanism is arranged above the cooling barrel, a collecting mechanism is arranged on the upper end surface of the bottom plate and between the two groups of supporting plates, a funnel is arranged on the bottom surface of the cooling barrel, and a water tank is arranged on one side of the bottom plate.
As a further scheme of the invention, the cooling mechanism comprises a vertical plate, a vertical groove penetrates through the outer side surface of the vertical plate, a sliding block is arranged in the vertical groove, and an electric telescopic rod is arranged between the inner side wall of the vertical groove and the outer side surface of the sliding block.
By adopting the technical scheme, the following technical effects can be achieved: the combination use of slider and perpendicular groove is convenient for.
As a further scheme of the invention, a transverse plate is arranged between the two groups of sliding blocks, a cooling fan is arranged on the bottom surface of the transverse plate, a first motor is arranged on the upper end surface of the transverse plate close to the middle position, and the transverse plate is movably arranged with the vertical plate through an electric telescopic rod and a sliding block matched with a vertical groove.
By adopting the technical scheme, the following technical effects can be achieved: the transverse plate can move between the two sets of vertical plates conveniently.
As a further scheme of the invention, the collecting mechanism comprises a collecting box, L-shaped limiting plates are arranged at two side angle positions of the collecting box on the upper end surface of the bottom plate, and connecting plates are arranged at the other two side angle positions of the collecting box on the upper end surface of the bottom plate.
By adopting the technical scheme, the following technical effects can be achieved: realize spacing one side of collecting the box.
As a further scheme of the invention, a rotating shaft is arranged on the outer side surface of the connecting plate close to the middle position, a rotating plate is sleeved outside the rotating shaft, a round plate is fixedly arranged at one end of the rotating shaft, and an attachment strap is arranged on the outer side surface of the collecting box and close to the bottom surface of the rotating plate.
By adopting the technical scheme, the following technical effects can be achieved: realize spacing collecting box opposite side.
As a further scheme of the invention, the inner side wall of the L-shaped limiting plate is tightly attached to the outer side surface of the collecting box, one end of the rotating plate is movably arranged with the connecting plate through a rotating shaft, and one side of the rotating plate is tightly attached to the outer side surface of the collecting box.
By adopting the technical scheme, the following technical effects can be achieved: the combination use of the rotating plate and the collecting box is convenient.
As a further scheme of the invention, a cooling pipe is wound on the outer side surface of the cooling barrel, a water pump is arranged in the water tank, one end of the cooling pipe penetrates through the water tank and is connected with the output end of the water pump, the other end of the cooling pipe penetrates through the water tank and is arranged in the water tank, and water is filled in the water tank.
By adopting the technical scheme, the following technical effects can be achieved: the water inside the water tank flows circularly on the outer side surface of the cooling barrel through the cooling pipe.
As a further scheme of the invention, a round baffle is arranged in the funnel and close to the upper end, the outer side surface of the round baffle is tightly attached to the inner side wall of the funnel, an L-shaped plate is arranged on the outer side surface of the funnel, a rotating shaft is arranged on the inner side wall of the L-shaped plate, one end of the rotating shaft penetrates through the funnel and is connected with the outer side surface of the round baffle, a second motor is arranged on the outer side surface of the L-shaped plate, and the output end of the second motor penetrates through the L-shaped plate and is connected with one end of the rotating shaft.
By adopting the technical scheme, the technical effect that the round baffle plate is convenient to rotate and is arranged in the funnel can be achieved.
In the technical scheme, the preparation method of the ketone compound provided by the invention has the beneficial effects that:
1. start electric telescopic handle, make it shorten, the vertical slot downstream that drives the slider along, the diaphragm is followed two sets of slider downstream, it is close to the upper end position to drive thermantidote downstream to cooling barrel inside, open the thermantidote through motor this moment, the raw materials to cooling barrel inside is bloied and is cooled off, start water tank internally mounted's water pump simultaneously, make the inside rivers of water tank flow to inside the cooling barrel, and flow in the cooling barrel outside through the cooling tube, flow to inside the water tank again through cooling tube one end at last, repeat above-mentioned process, can make the inside hydrologic cycle of water tank flow, cool down the cooling barrel, thereby cool down to its inside raw materials that holds, through the above-mentioned operation, can cool off the raw materials well, accelerate the cooling rate of raw materials.
2. The collection box that will collect in the mechanism is placed at bottom plate upper end specific surface, and make its both sides angle hug closely L type limiting plate inside wall, then lead to the rotatory rotor plate of pivot of installation on the connecting plate, make its one side hug closely and collect box front end surface, can prescribe a limit to well and collect the position of box, make it be difficult for moving, make the crystallization drop to it in better, start motor two of installation on the L template and make the axis of rotation rotate, drive round baffle and rotate 90 in the funnel is inside, the crystallization falls to the collection box in the collection mechanism through the funnel inside this moment, can collect the crystallization, through the process, the staff of being convenient for collects the crystallization.
Drawings
In order to more clearly illustrate the embodiments of the present application or technical solutions in the prior art, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments described in the present invention, and other drawings can be obtained by those skilled in the art according to the drawings.
FIG. 1 is a schematic diagram of an overall structure provided in an embodiment of the present invention;
FIG. 2 is a schematic structural diagram of a cooling mechanism according to an embodiment of the present invention;
fig. 3 is a schematic structural diagram of a bottom plate and a collecting mechanism according to an embodiment of the present invention.
Fig. 4 is a schematic structural view of a funnel and an L-shaped plate according to an embodiment of the present invention.
Description of reference numerals:
1. a base plate; 2. a support plate; 3. a cooling barrel; 4. a cooling tube; 6. a water tank; 7. a vertical plate; 8. a transverse plate; 9. a cooling fan; 10. a vertical slot; 11. a slider; 12. an electric telescopic rod; 13. a funnel; 14. a collection box; 15. a circular baffle plate; 16. an L-shaped plate; 17. a connecting plate; 18. a rotating plate; 19. a circular plate; 20. an L-shaped limiting plate; 21. a cooling mechanism; 22. and a collecting mechanism.
Detailed Description
In order to make the technical solutions of the present invention better understood, those skilled in the art will now describe the present invention in further detail with reference to the accompanying drawings.
Example 1:
a method of making a ketone, the method comprising:
step S001: by acid precipitation of condensation
Putting sodium methoxide and thiophenol into a reaction kettle, stirring, cooling water by a reflux condenser, naturally heating, then heating to 50 ℃, carrying out heat preservation reaction for 30 minutes, cooling to room temperature after heat preservation, adding phthalide in portions, heating to reflux, carrying out heat preservation for 2 hours at 65 ℃, recovering methanol at normal pressure after heat preservation, and evaporating methanol under reduced pressure after methanol is basically evaporated; after the steaming is finished, cooling to 50 ℃, adding 1000g of water for dissolving, dropwise adding hydrochloric acid to adjust the pH value of the solution to 2, stirring for 30 minutes, and repeatedly measuring the pH value to be unchanged; then 600g of toluene is added, the temperature is raised, the mixture is heated and dissolved to 75 ℃, a lower acid water layer is removed to obtain a condensation compound, and the water layer is separated as clear as possible for standby;
feeding amount:
step S002: ring closure hydrolysis
Putting polyphosphoric acid into a clean and dry reaction kettle, stirring, pouring a preheated condensation compound, heating, decompressing and recovering toluene after the addition is finished, starting heat preservation reaction for 1 hour after the toluene is completely evaporated when the internal temperature reaches 120 ℃, sampling and analyzing, immediately cooling to below 50 ℃ through a cooling crystallization device after the test is qualified, quickly adding ice water at 5 ℃ into the cooling crystallization device, separating out black granular solid, crystallizing to obtain a ketone crude product, performing suction filtration and water washing until the pH of an aqueous solution is neutral, draining, and discharging to obtain the ketone crude product; the weight is about 235g for standby;
feed amount
Condensate step S001 obtaining a condensate
Polyphosphoric acid (1: 1) 800g
1200g of ice water.
Step S003: refining
Respectively putting toluene and crude ketone products into a 2000ml reaction kettle, stirring, heating to 70-73 ℃, stirring for dissolving for 30 minutes, and standing for 30 minutes for layering; adding activated carbon at the temperature, stirring and preserving heat for 30 minutes, filtering to remove carbon, cooling and crystallizing filtrate by a cooling and crystallizing device, rinsing by a small amount of petroleum ether after filtering, drying in vacuum, taking out after testing is qualified, drying and packaging to obtain a finished product; the yield thereof was found to be 81.5%.
Feed amount
Crude ketone substrate 235g
470g of toluene
12g of activated carbon.
The chemical reaction process comprises the following steps:
example 2:
a method of making a ketone, the method comprising:
step S001: by acid precipitation of condensation
Putting sodium methoxide and thiophenol into a reaction kettle, stirring, cooling water by a reflux condenser, naturally heating, then heating to 45 ℃, carrying out heat preservation reaction for 30 minutes, cooling to room temperature after heat preservation, adding phthalide in portions, heating to reflux, carrying out heat preservation for 2 hours at 60 ℃, recovering methanol at normal pressure after heat preservation, and evaporating methanol under reduced pressure after methanol is basically evaporated; after the steaming is finished, cooling to 50 ℃, adding 1000g of water for dissolving, dropwise adding hydrochloric acid to adjust the pH value of the solution to 2, stirring for 30 minutes, and repeatedly measuring the pH value to be unchanged; then 600g of toluene is added, the temperature is raised, the mixture is heated and dissolved to 75 ℃, a lower acid water layer is removed to obtain a condensation compound, and the water layer is separated as clear as possible for standby;
feeding amount:
step S002: ring closure hydrolysis
Putting polyphosphoric acid into a clean and dry reaction kettle, stirring, pouring a preheated condensation compound, heating, decompressing and recovering toluene after the addition is finished, starting heat preservation reaction for 1 hour after the toluene is completely evaporated when the internal temperature reaches 120 ℃, sampling and analyzing, immediately cooling to below 50 ℃ through a cooling crystallization device after the test is qualified, quickly adding ice water at 0 ℃ into the cooling crystallization device, separating out black granular solid, crystallizing to obtain a ketone crude product, performing suction filtration and water washing until the pH of an aqueous solution is neutral, draining, and discharging to obtain the ketone crude product; the weight is about 235g for standby;
feed amount
Condensate step S001 obtaining a condensate
Polyphosphoric acid (1: 1) 800g
1200g of ice water.
Step S003: refining
Respectively putting toluene and crude ketone products into a 2000ml reaction kettle, stirring, heating to 70 ℃, stirring for dissolving for 30 minutes, and standing for 30 minutes for layering; adding activated carbon at the temperature, stirring and preserving heat for 30 minutes, filtering to remove carbon, cooling and crystallizing filtrate by a cooling and crystallizing device, rinsing by a small amount of petroleum ether after filtering, drying in vacuum, taking out after testing is qualified, drying and packaging to obtain a finished product; the yield is 82.3%;
feed amount
Crude ketone substrate 235g
473g of toluene
11g of activated carbon.
Example 3:
a method of making a ketone, the method comprising:
step S001: by acid precipitation of condensation
Putting sodium methoxide and thiophenol into a reaction kettle, stirring, starting a reflux condenser to cool water, naturally heating, then heating to 40-50 ℃, carrying out heat preservation reaction for 30 minutes, cooling to room temperature after heat preservation, adding phthalide in portions, heating to reflux after heat preservation, carrying out heat preservation for 2 hours at 60-65 ℃, recovering methanol at normal pressure after heat preservation, and after methanol is basically evaporated, evaporating methanol under reduced pressure; after the steaming is finished, cooling to 45-50 ℃, adding 1000g of water for dissolving, dropwise adding hydrochloric acid to adjust the pH value of the solution to 1-2, stirring for 30 minutes, and repeatedly measuring the pH value to be unchanged; then adding 600g of toluene, heating and dissolving to 65-75 ℃, removing a lower acid water layer to obtain a condensation compound, and separating the water layer as clear as possible for later use;
feeding amount:
step S002: ring closure hydrolysis
Putting polyphosphoric acid into a clean and dry reaction kettle, stirring, pouring a preheated condensation compound, after the addition is finished, heating, decompressing and recovering toluene, when the internal temperature reaches 115-120 ℃, completely evaporating the toluene, starting a heat preservation reaction for 1 hour, sampling and analyzing, immediately cooling to below 50 ℃ through a cooling crystallization device after the test is qualified, quickly adding ice water at 0-5 ℃ into the cooling crystallization device, separating out black granular solid, crystallizing to obtain a ketone crude product, performing suction filtration, washing with water until the pH of an aqueous solution is neutral, draining, and discharging to obtain the ketone crude product; the weight is about 230g for standby;
feed amount
Condensate step S001 obtaining a condensate
Polyphosphoric acid (1: 1) 810g
Ice Water 1200g
Step S003: refining
Respectively putting toluene and crude ketone products into a 2000ml reaction kettle, stirring, heating to 70-73 ℃, stirring for dissolving for 30 minutes, and standing for 30 minutes for layering; adding activated carbon at the temperature, stirring and preserving heat for 30 minutes, filtering to remove carbon, cooling and crystallizing filtrate by a cooling and crystallizing device, rinsing by a small amount of petroleum ether after filtering, drying in vacuum, taking out after testing is qualified, drying and packaging to obtain a finished product; the yield is 80.6%;
feed amount
Crude ketone base 230g
470g of toluene
12g of activated carbon.
Example 4:
referring to fig. 1 to 4, the present invention provides a technical solution: a ketone preparation method comprises a bottom plate 1, wherein supporting plates 2 are respectively arranged on the upper end surface of the bottom plate 1 close to two sides, bearing plates are arranged at the upper ends of the supporting plates 2, a cooling barrel 3 is arranged between the two groups of bearing plates, a cooling mechanism 21 is arranged above the cooling barrel 3, a collecting mechanism 22 is arranged on the upper end surface of the bottom plate 1 and between the two groups of supporting plates 2, a funnel 13 is arranged on the bottom surface of the cooling barrel 3, and a water tank 6 is arranged on one side of the bottom plate 1.
Please refer to fig. 1-2, the cooling mechanism 21 includes a vertical plate 7, a vertical groove 10 is provided on the outer side surface of the vertical plate 7, a slider 11 is installed inside the vertical groove 10, an electric telescopic rod 12 is installed between the inner side wall of the vertical groove 10 and the outer side surface of the slider 11, a transverse plate 8 is installed between the two sets of sliders 11, a cooling fan 9 is arranged on the bottom surface of the transverse plate 8, a first motor is installed on the upper end surface of the transverse plate 8 near the middle position, the transverse plate 8 passes through the electric telescopic rod 12, the slider 11 is matched with the vertical groove 10 and the vertical plate 7 for movable installation, a cooling pipe 4 is wound on the outer side surface of the cooling barrel 3, the water tank 6 is internally installed with a water pump, one end of the cooling pipe 4 is connected with the output end of the water pump after passing through the water tank 6, the other end of the water tank is arranged inside the water tank 6, and the water tank 6 is filled with water.
Specifically, when in use, the raw materials are poured into the cooling barrel 3, then the electric telescopic rod 12 in the cooling mechanism 21 is started to shorten, the sliding blocks 11 are driven to move downwards along the vertical grooves 10 formed in the vertical plates 7, the transverse plate 8 moves downwards along the two groups of sliding blocks 11 to drive the cooling fan 9 to move downwards to a position close to the upper end inside the cooling barrel 3, at the moment, the cooling fan 9 is started through the first motor to blow and cool the raw materials inside the cooling barrel 3, meanwhile, the water pump installed inside the water tank 6 is started to enable the water inside the water tank 6 to flow into the cooling pipe 4 and flow outside the cooling barrel 3 through the cooling pipe 4, and finally, the water flows into the water tank 6 again through one end of the cooling pipe 4, the processes are repeated, the water inside the water tank 6 can circularly flow to cool the cooling barrel 3, so as to cool the raw materials contained inside the cooling barrel, through the operations, the raw materials can be well cooled, and the cooling speed of the raw materials is accelerated.
Example 5:
referring to fig. 1 to 4, the present invention provides a technical solution: a ketone preparation method comprises a bottom plate 1, wherein supporting plates 2 are respectively arranged on the upper end surface of the bottom plate 1 close to two sides, bearing plates are arranged at the upper ends of the supporting plates 2, a cooling barrel 3 is arranged between the two groups of bearing plates, a cooling mechanism 21 is arranged above the cooling barrel 3, a collecting mechanism 22 is arranged on the upper end surface of the bottom plate 1 and between the two groups of supporting plates 2, a funnel 13 is arranged on the bottom surface of the cooling barrel 3, and a water tank 6 is arranged on one side of the bottom plate 1.
Referring to fig. 3-4, the collecting mechanism 22 includes a collecting box 14, L-shaped limiting plates 20 are installed at two corner positions of the collecting box 14 on the upper surface of the bottom plate 1, connecting plates 17 are installed at two corner positions of the collecting box 14 on the upper surface of the bottom plate 1, a rotating shaft is installed at a position, close to the middle position, of the outer side surface of the connecting plate 17, a rotating plate 18 is sleeved outside the rotating shaft, a circular plate 19 is fixedly installed at one end of the rotating shaft, an attachment strap is installed at a position, close to the bottom surface of the rotating plate 18, on the outer side surface of the collecting box 14, an inner side wall of the L-shaped limiting plate 20 is tightly attached to the outer side surface of the collecting box 14, one end of the rotating plate 18 is movably installed with the connecting plate 17 through the rotating shaft, and one side of the rotating plate 18 is tightly attached to the outer side surface of the collecting box 14.
A round baffle 15 is installed in the position, close to the upper end, inside the funnel 13, the outer side face of the round baffle 15 is tightly attached to the inner side wall of the funnel 13, an L-shaped plate 16 is installed on the outer side face of the funnel 13, a rotating shaft is installed on the inner side wall of the L-shaped plate 16, one end of the rotating shaft penetrates through the funnel 13 to be connected with the outer side face of the round baffle 15, a second motor is installed on the outer side face of the L-shaped plate 16, and the output end of the second motor penetrates through the L-shaped plate 16 to be connected with one end of the rotating shaft.
Specifically, the collecting box 14 in the collecting mechanism 22 is placed on the specific surface of the upper end of the bottom plate 1, two side corners of the collecting box are tightly attached to the inner side wall of the L-shaped limiting plate 20, then the rotating plate 18 is rotated through the rotating shaft arranged on the connecting plate 17, one side of the rotating plate is tightly attached to the front end surface of the collecting box 14, the position of the collecting box 14 can be well limited, the collecting box is not easy to move, crystals can well fall into the collecting box, the bottom surface of the rotating plate 18 is tightly attached to the upper end surface of the butt strap, the position of one end, far away from the rotating shaft, of the rotating plate 18 can be well limited, the rotating plate 18 and the bottom plate 1 are arranged in parallel, the circular plate 19 can prevent one end of the rotating plate 18 from rotating out from one end of the rotating shaft, after raw materials in the cooling barrel 3 are cooled to form crystals, the motor II arranged on the L-shaped plate 16 is started to rotate the rotating shaft to drive the circular baffle plate 15 to rotate 90 degrees in the hopper 13, and then the crystals fall into the collecting box 14 in the collecting mechanism 22 through the hopper 13, the crystals can be collected, and through the process, the crystals can be conveniently collected by workers.
While certain exemplary embodiments of the present invention have been described above by way of illustration only, it will be apparent to those of ordinary skill in the art that the described embodiments may be modified in various different ways without departing from the spirit and scope of the invention. Accordingly, the drawings and description are illustrative in nature and should not be construed as limiting the scope of the invention.
Claims (9)
1. A method for preparing a ketone compound, comprising:
step S001: by acid precipitation of condensation
Putting sodium methoxide and thiophenol into a reaction kettle, stirring, cooling to room temperature, putting phthalide into the reaction kettle in portions, and evaporating methanol under reduced pressure; adding water to dissolve the mixture, and then dropwise adding hydrochloric acid to adjust the pH value of the solution to 1-2; then adding toluene, heating to dissolve to 65-75 ℃, and removing a lower acid water layer to obtain a condensation compound;
step S002: ring closure hydrolysis
Putting polyphosphoric acid into a reaction kettle, stirring, pouring a preheated condensation compound, heating to 115-120 ℃ after adding, recovering toluene under reduced pressure, and immediately separating out black granular solid through a cooling crystallization device after the test is qualified to crystallize the black granular solid into a ketone crude product;
step S003: refining
Respectively putting toluene and crude ketone products into a reaction kettle, stirring, and standing for 30 minutes for layering; adding activated carbon, stirring, filtering to remove carbon, cooling and crystallizing the filtrate by a cooling and crystallizing device, rinsing with petroleum ether after filtering, drying in vacuum, taking out after testing is qualified, drying and packaging to obtain a finished product;
the cooling crystallization device comprises a bottom plate (1), wherein supporting plates (2) are installed on the upper end surface of the bottom plate (1) close to the positions of the two sides, bearing plates are installed on the upper ends of the supporting plates (2), a cooling barrel (3) is arranged between the two groups of bearing plates, a cooling mechanism (21) is arranged above the cooling barrel (3), a collecting mechanism (22) is arranged on the upper end surface of the bottom plate (1) and between the two groups of supporting plates (2), a funnel (13) is installed on the bottom surface of the cooling barrel (3), and a water tank (6) is arranged on one side of the bottom plate (1).
2. The ketone preparation method according to claim 1, wherein the cooling mechanism (21) comprises a vertical plate (7), a vertical groove (10) is formed on the outer side surface of the vertical plate (7) in a penetrating manner, a sliding block (11) is installed inside the vertical groove (10), and an electric telescopic rod (12) is installed between the inner side wall of the vertical groove (10) and the outer side surface of the sliding block (11).
3. The ketone preparation method according to claim 2, wherein a transverse plate (8) is installed between two sets of the sliding blocks (11), a cooling fan (9) is arranged on the bottom surface of the transverse plate (8), a first motor is installed on the upper end surface of the transverse plate (8) close to the middle position, and the transverse plate (8) is movably installed with a vertical plate (7) through an electric telescopic rod (12) and the sliding blocks (11) matched with a vertical groove (10).
4. A ketone member producing method according to claim 1, wherein said collecting means (22) comprises a collecting case (14), L-shaped restriction plates (20) are provided at both side positions of said collecting case (14) on the upper end surface of said base plate (1), and said connecting plates (17) are provided on the upper end surface of said base plate (1) near the other side positions of said collecting case (14).
5. A ketone member production method according to claim 4, wherein a rotary shaft is provided on the outer side of the connecting plate (17) near the center, a rotary plate (18) is provided around the rotary shaft, a circular plate (19) is fixedly provided at one end of the rotary shaft, and a butt plate is provided on the outer side of the collecting box (14) near the bottom surface of the rotary plate (18).
6. A ketone member manufacturing method according to claim 5, wherein the inner side wall of the L-shaped limiting plate (20) is closely attached to the outer side surface of the collection box (14), one end of the rotating plate (18) is movably mounted with the connecting plate (17) through a rotating shaft, and one side of the rotating plate (18) is closely attached to the outer side surface of the collection box (14).
7. The ketone preparation method according to claim 1, wherein a cooling pipe (4) is wound on the outer side surface of the cooling barrel (3), a water pump is installed inside the water tank (6), one end of the cooling pipe (4) penetrates through the water tank (6) to be connected with the output end of the water pump, the other end of the cooling pipe penetrates through the water tank (6) to be arranged inside the cooling pipe, and water is filled inside the water tank (6).
8. A method of making a ketone according to claim 1 wherein a circular baffle (15) is mounted in the interior of the hopper (13) adjacent the upper end thereof, the outer side of the circular baffle (15) being in close proximity to the inner side of the hopper (13).
9. The method for preparing the ketone material according to claim 8, wherein an L-shaped plate (16) is arranged on the outer side surface of the funnel (13), a rotating shaft is arranged on the inner side wall of the L-shaped plate (16), one end of the rotating shaft penetrates through the funnel (13) to be connected with the outer side surface of the circular baffle (15), a second motor is arranged on the outer side surface of the L-shaped plate (16), and the output end of the second motor penetrates through the L-shaped plate (16) to be connected with one end of the rotating shaft.
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| CN202111085842.8A CN113968839A (en) | 2021-09-16 | 2021-09-16 | Preparation method of ketone compound |
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| CN202111085842.8A CN113968839A (en) | 2021-09-16 | 2021-09-16 | Preparation method of ketone compound |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116271935A (en) * | 2023-03-16 | 2023-06-23 | 福建省德旭新材料有限公司 | Cooler for preparing sodium hexafluorophosphate |
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| CN213317549U (en) * | 2020-09-08 | 2021-06-01 | 烟台一诺电子材料有限公司 | Crystallization cooling device |
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Application publication date: 20220125 |