CN214634626U - System for be used for cyclohexyl hydrogen peroxide to decompose and separate - Google Patents
System for be used for cyclohexyl hydrogen peroxide to decompose and separate Download PDFInfo
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- CN214634626U CN214634626U CN202120520479.7U CN202120520479U CN214634626U CN 214634626 U CN214634626 U CN 214634626U CN 202120520479 U CN202120520479 U CN 202120520479U CN 214634626 U CN214634626 U CN 214634626U
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Abstract
The utility model discloses a system for decomposing and separating cyclohexyl hydrogen peroxide, which comprises a membrane filter, wherein one end of the membrane filter is connected with a decomposition liquid source, and the other end of the membrane filter is connected with a mixer; the mixer is connected with a cooler, and the cooler is connected with an inlet end at the bottom of the decomposition tower; the liquid outlet end at the top of the decomposition tower is connected with a waste alkali separation mechanism; one end of an oil phase outlet of the waste alkali separation mechanism is connected with the alkane recovery device, and one end of an alkali liquor outlet of the waste alkali separation mechanism is connected with the waste alkali collecting tank; the upper part of the waste alkali collecting tank is connected with the inlet end of the waste alkali separating mechanism through a light phase delivery pump; the lower part of the waste alkali collecting tank is connected with a waste alkali treatment device through a waste alkali delivery pump. The system solves the problems of insufficient mixing and incomplete separation of the decomposition liquid and the alkaline water after the decomposition reaction in the prior art, and has the purposes of higher yield of heterogeneous decomposition, higher mixed mass transfer efficiency and longer production operation period of the device.
Description
Technical Field
The utility model belongs to the technical field of cyclohexyl hydrogen peroxide decomposes and separates, in particular to a system that is used for cyclohexyl hydrogen peroxide to decompose and separate.
Background
At present, the heterogeneous decomposition process technology is mature, and is still the main decomposition method in the current world oxidation method cyclohexanone production device. The process is that cyclohexyl hydrogen peroxide (CHHP) is mixed and contacted with an alkaline aqueous solution containing a small amount of cobalt acetate in a decomposition tower, so that the cyclohexyl hydrogen peroxide in a cyclohexane oil phase is extracted by an alkaline aqueous phase, and under the action of an alkaline condition and a cobalt acetate catalyst, the CHHP is directionally decomposed to generate cyclohexanone and cyclohexanol; after the reaction is finished, the cyclohexanone and the cyclohexanol in the alkaline water phase are back-extracted to the oil phase by the cyclohexane in the decomposition liquid due to different relative solubilities, and the decomposition reaction is finished. And (3) carrying out phase separation on the decomposed liquid and the alkaline water phase in a waste alkaline separator, feeding the separated decomposed liquid into a subsequent working section, returning one part of alkaline water to the decomposition tower for cyclic utilization, and discharging the other part of alkaline water serving as waste alkaline water out of the system.
In the running process of a system, decomposition liquid and an alkaline water phase need to be fully mixed to ensure complete reaction, otherwise, the yield of the system is reduced, and a decomposition tower is gradually blocked in the running process to cause uneven mixing; after the decomposition reaction is finished, the decomposition liquid needs to be thoroughly separated from the alkaline water phase, otherwise, the decomposition liquid carrying the alkaline water phase enters an alkane recovery system to cause the blockage of a heat exchanger of the alkane recovery system, the long-period stable operation of the device is seriously influenced, and certain potential safety hazards can be brought by frequent starting and stopping of the device.
Disclosure of Invention
The utility model aims to solve the technical problem that a system for cyclohexyl hydrogen peroxide decomposes and separates is provided, and this system has solved prior art and has mixed inadequately, and after the decomposition reaction, decomposition liquid and the not thorough problem of buck phase separation have heterogeneous decomposition yield higher, mix the purpose that mass transfer efficiency is higher, the production operation cycle of device has been prolonged.
In order to solve the technical problem, the utility model discloses the technical scheme who adopts is: a system for decomposition and separation of cyclohexyl hydroperoxide comprises a membrane filter, one end of the membrane filter is connected with a decomposition liquid source, and the other end of the membrane filter is connected with a mixer; the mixer is connected with a cooler, and the cooler is connected with an inlet end at the bottom of the decomposition tower; the liquid outlet end at the top of the decomposition tower is connected with a waste alkali separation mechanism; one end of an oil phase outlet of the waste alkali separation mechanism is connected with the alkane recovery device, and one end of an alkali liquor outlet of the waste alkali separation mechanism is connected with the waste alkali collecting tank; the upper part of the waste alkali collecting tank is connected with the inlet end of the waste alkali separating mechanism through a light phase delivery pump; the lower part of the waste alkali collecting tank is connected with a waste alkali treatment device through a waste alkali delivery pump.
Preferably, the liquid inlet end of the mixer is provided with an alkali liquor conveying pipeline which comprises an alkali liquor conveying pump and an alkali liquor storage tank.
Preferably, both ends of the cooler are respectively connected with a circulating water recovery system and a circulating water upper water system.
Preferably, the waste alkali separation mechanism comprises a plurality of waste alkali separators, light phase ends of the plurality of waste alkali separators are arranged in series, and heavy phase ends are connected to the waste alkali collecting tank in parallel; the number of spent caustic separators is preferably three.
Furthermore, a back flushing port is arranged at the top of the decomposition tower, and a sewage draining port is arranged at the bottom of the decomposition tower; the back flushing port is connected to the circulating water recovery system through a pipeline and a three-way valve.
Preferably, the waste alkali separation mechanism comprises a hydrocyclone in series connection with the waste alkali separator, an oil phase outlet of the hydrocyclone is connected with the alkane recovery device, and a heavy phase outlet is connected with the waste alkali collecting tank.
Preferably, a plurality of layers of decomposition areas are arranged inside the decomposition tower, and flat ring packing is arranged in the decomposition areas.
Preferably, the top and the bottom of the inner wall of the waste alkali separator are connected with a plurality of vertical partition plates in a staggered manner; the bottom of the waste alkali collecting tank is connected with a vertical clapboard.
Preferably, the outlet end of the waste alkali conveying pump is connected to the alkali liquor conveying pipeline through a pipeline.
The utility model has the advantages that:
1. a pre-mixing mixer is arranged in front of the decomposition tower, and the yield of heterogeneous decomposition is further improved through pre-mixing reaction of the decomposition liquid and the alkali water phase;
2. the decomposition tower is provided with a multi-layer packing area, and flat ring packing is adopted as the packing, so that the mixed mass transfer efficiency is improved;
3. by arranging a plurality of waste liquid separators and hydrocyclone separators, decomposed decomposition liquid and alkaline water are fully separated, the shutdown blockage removal frequency of the heat exchanger of the alkane recovery system is reduced, and the production operation period of the device is prolonged.
Drawings
FIG. 1 is a schematic diagram of the system connection of the present invention;
the reference numbers in the figures are: the system comprises a membrane filter 1, a mixer 2, a cooler 3, a decomposition tower 4, a first waste alkali separator 5, a second waste alkali separator 6, a third waste alkali separator 7, a hydrocyclone 8, a waste alkali collecting tank 9, a light phase delivery pump 10, a waste alkali delivery pump 11, an alkali liquor delivery pump 12, a decomposition liquid source 13, an alkali water storage tank 14, a waste alkali treatment device 15, an alkane recovery device 16, a circulating water recovery system 17 and a circulating water upper water system 18.
Detailed Description
As shown in FIG. 1, a system for decomposition and separation of cyclohexyl hydroperoxide comprises a membrane filter 1, wherein one end of the membrane filter 1 is connected with a decomposition liquid source 13, and the other end is connected with a mixer 2; the mixer 2 is connected with a cooler 3, and the cooler 3 is connected with the inlet end at the bottom of a decomposition tower 4; the liquid outlet end at the top of the decomposing tower 4 is connected with a waste alkali separating mechanism; one end of an oil phase outlet of the waste alkali separation mechanism is connected with the alkane recovery device 16, and one end of an alkali liquor outlet of the waste alkali separation mechanism is connected with the waste alkali collecting tank 9; the upper part of the waste alkali collecting tank 9 is connected with the inlet end of the waste alkali separating mechanism through a light phase delivery pump 10; the lower part of the waste alkali collecting tank 9 is connected with a waste alkali treatment device 15 through a waste alkali delivery pump 11.
Preferably, the liquid inlet end of the mixer 2 is provided with an alkali liquor conveying pipeline which comprises an alkali liquor conveying pump 12 and an alkali liquor storage tank 14; the pore size of the membrane tube in the decomposed liquid membrane filter 11 is preferably 10 nm.
Preferably, a circulating water recovery system 17 and a circulating water upper water system 18 are connected to both ends of the cooler 3, respectively.
Preferably, the waste alkali separation mechanism comprises a plurality of waste alkali separators, light phase ends of the plurality of waste alkali separators are arranged in series, and heavy phase ends are connected in parallel to the waste alkali collecting tank 9; the number of the alkali waste separators is preferably three, and the first alkali waste separator 5, the second alkali waste separator 6 and the third alkali waste separator 7 are arranged in sequence from front to back.
Furthermore, the top of the decomposition tower 4 is provided with a back flushing port, and the bottom is provided with a sewage draining port; the back flushing port is connected to the circulating water recovery system 17 through a pipeline and a three-way valve.
Preferably, the waste alkali separation mechanism comprises a hydrocyclone 8 connected with the waste alkali separator in series, an oil phase outlet of the hydrocyclone 8 is connected with the alkane recovery device 16, and a heavy phase outlet is connected with the waste alkali collecting tank 9.
Preferably, a multi-layer decomposition area is arranged inside the decomposition tower 4, and flat ring packing is arranged in the decomposition area.
Preferably, the top and the bottom of the inner wall of the waste alkali separator are connected with a plurality of vertical partition plates in a staggered manner; the bottom of the waste alkali collecting tank 9 is connected with a vertical clapboard.
Preferably, the outlet end of the spent caustic conveying pump 11 is connected to the caustic conveying pipeline through a pipeline.
The working principle of a system for decomposition and separation of cyclohexyl hydroperoxide as described above is as follows:
cyclohexyl hydrogen peroxide from a heat exchange system enters a decomposition liquid membrane filter 1 for filtering, trace fine impurities in a decomposition liquid are separated, and the separated decomposition liquid is fully mixed with alkali water containing cobalt acetate conveyed by an alkali liquor conveying pump 12 and part of waste alkali returned by a waste alkali conveying pump 11 in a mixer 2;
cooling the mixed decomposition liquid to 90 ℃ in a cooler 3, cooling, then allowing the cooled decomposition liquid to enter a decomposition tower 4 for decomposition reaction to generate cyclohexanone and cyclohexanol, allowing the decomposed decomposition liquid and alkaline water to sequentially enter a first waste alkali separator 5, a second waste alkali separator 6 and a third waste alkali separator 7 for separation, and controlling the boundary positions of the first waste alkali separator 5, the second waste alkali separator 6 and the third waste alkali separator 7 to be 20%, 12% and 5% at one time; the separated decomposition liquid is further separated in the hydrocyclone 8, and the separated oil phase is sent to the alkane recovery unit 16.
Heavy phases in the first alkali waste separator 5, the second alkali waste separator 6, the third alkali waste separator 7 and the hydrocyclone 8 enter an alkali waste collecting tank 9 for standing separation, a light phase after standing separation is conveyed to an inlet of the first alkali waste separator 5 through a light phase conveying pump 10 for re-separation, one heavy phase alkali waste conveying pump 11 after standing separation is conveyed to an inlet of the mixer 2, and one part of the heavy phase alkali waste is conveyed to an alkali waste treatment device 15.
The above embodiments are merely preferred technical solutions of the present invention, and should not be considered as limitations of the present invention, and the features in the embodiments and the examples in the present application may be arbitrarily combined with each other without conflict. The protection scope of the present invention shall be defined by the claims and the technical solutions described in the claims, including the technical features of the equivalent alternatives as the protection scope. Namely, equivalent alterations and modifications within the scope of the invention are also within the scope of the invention.
Claims (8)
1. A system for cyclohexyl hydroperoxide decomposition and separation, characterized by: comprises a membrane filter (1), one end of the membrane filter (1) is connected with a decomposition liquid source (13), and the other end is connected with a mixer (2); the mixer (2) is connected with the cooler (3), and the cooler (3) is connected with the inlet end at the bottom of the decomposition tower (4); the liquid outlet end at the top of the decomposing tower (4) is connected with a waste alkali separating mechanism; one end of an oil phase outlet of the waste alkali separation mechanism is connected with an alkane recovery device (16), and one end of an alkali liquor outlet of the waste alkali separation mechanism is connected with a waste alkali collecting tank (9); the upper part of the waste alkali collecting tank (9) is connected with the inlet end of the waste alkali separating mechanism through a light phase delivery pump (10); the lower part of the waste alkali collecting tank (9) is connected with a waste alkali treatment device (15) through a waste alkali delivery pump (11).
2. The system for decomposition and separation of cyclohexyl hydroperoxide as described in claim 1, wherein: an alkali liquor conveying pipeline is arranged at the liquid inlet end of the mixer (2) and comprises an alkali liquor conveying pump (12) and an alkali liquor storage tank (14).
3. The system for decomposition and separation of cyclohexyl hydroperoxide as described in claim 1, wherein: and two ends of the cooler (3) are respectively connected with a circulating water recovery system (17) and a circulating water upper water system (18).
4. The system for decomposition and separation of cyclohexyl hydroperoxide as described in claim 1, wherein: the waste alkali separation mechanism comprises a plurality of waste alkali separators, light phase ends of the waste alkali separators are arranged in series, and heavy phase ends are connected to a waste alkali collecting tank (9) in parallel.
5. The system for decomposition and separation of cyclohexyl hydroperoxide as described in claim 1, wherein: the waste alkali separation mechanism comprises a hydrocyclone separator (8) connected with the waste alkali separator in series, an oil phase outlet of the hydrocyclone separator (8) is connected with an alkane recovery device (16), and a heavy phase outlet is connected with a waste alkali collecting tank (9).
6. The system for decomposition and separation of cyclohexyl hydroperoxide as described in claim 1, wherein: the decomposition tower (4) is internally provided with a plurality of layers of decomposition areas, and flat ring packing is arranged in the decomposition areas.
7. A system for decomposition and separation of cyclohexyl hydroperoxide as described in claim 4 wherein: the top and the bottom of the inner wall of the waste alkali separator are connected with a plurality of vertical partition plates in a staggered manner; the bottom of the waste alkali collecting tank (9) is connected with a vertical clapboard.
8. The system for decomposition and separation of cyclohexyl hydroperoxide as described in claim 1, wherein: the outlet end of the waste alkali delivery pump (11) is connected to an alkali liquor delivery pipeline through a pipeline.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN114570152A (en) * | 2022-03-28 | 2022-06-03 | 南京诺令生物科技有限公司 | Integrated device for separating and purifying low-particulate-matter gas and separating and purifying method thereof |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN114570152A (en) * | 2022-03-28 | 2022-06-03 | 南京诺令生物科技有限公司 | Integrated device for separating and purifying low-particulate-matter gas and separating and purifying method thereof |
CN114570152B (en) * | 2022-03-28 | 2023-12-19 | 南京诺令生物科技有限公司 | Integrated device for separating and purifying low-particulate gas and separation and purification method thereof |
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