CN208995418U - A kind of acetic synthesis separation and recovery of catalyst device - Google Patents
A kind of acetic synthesis separation and recovery of catalyst device Download PDFInfo
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- CN208995418U CN208995418U CN201821648157.5U CN201821648157U CN208995418U CN 208995418 U CN208995418 U CN 208995418U CN 201821648157 U CN201821648157 U CN 201821648157U CN 208995418 U CN208995418 U CN 208995418U
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Abstract
A kind of acetic synthesis separation and recovery of catalyst device, including pre-separation tower, cooler, the first separator, stripper, reboiler, lightness-removing column, first cold cooler, eventually cold cooler, the second separator, quantizer.The utility model is designed by modularization, function division, expensive rhodium catalyst, co-catalyst iodomethane and thick acetic acid substep is realized to efficiently separate, unit product consumption and cost are effectively reduced, the clean and environmental protection index and economic benefit of Processes for Producing Acetic Acid are improved.
Description
Technical field
The utility model belongs to separation technology field, in particular to a kind of separating and reclaiming device of acetic synthesis catalyst.
Background technique
In the method for synthesis acetic acid used at present, commercially it is most useful that by methanol in the presence of rhodium catalyst
The method of carbonylation manufacture acetic acid, the rhodium catalyst include that (it is dissolved or dispersed in liquid reaction medium or is supported on lazy rhodium
On property solid), halogen-containing co-catalyst (such as iodomethane) and methyl acetate.
Iodomethane in the separable recycling rhodium catalyst of traditional catalyst and lighter component separation and recovery system, while with dilute
Acetic acid form is by partial moisture from recycling.For acetic acid (117.7 DEG C of normal boiling point), methyl acetate, first alcohol and water are all
It is lighter component, propionic acid is heavy component, and hydrogen iodide can ionize in water, thus its volatility is related with water content, 96~
In 99% aqueous acetic acid, volatility differs several orders of magnitude.
Above-mentioned separation and recovery system includes lightness-removing column, first cold cooler, eventually cold cooler, condensate separator, quantizer,
It is sent to from the evaporator in methanol carbonylization manufacture acetic acid technique and is entrained with a small amount of rhodium catalyst in the gas phase of lightness-removing column, passed through
The washing of lightness-removing column lower tray, returns to reaction kettle after sending evaporator back to by lightness-removing column tower reactor.The separation and recovery system arranges separation
Recovering effect is poor, and major catalyst rhodium part moves back other systems, can not recycle, and consumes higher.Co-catalyst iodine first
Alkane primary recovery only has 87%, must be equipped with the absorption system of bulky complex for further recycling iodomethane further to recycle
Co-catalyst.It is more that whole flow process is related to step, and process is complicated, and energy consumption is higher, and equipment investment is big, less economical.
Summary of the invention
The purpose of this utility model is to provide a kind of acetic synthesis separation and recovery of catalyst device, easily operated, costs
It is low, and good separating effect, improve the clean and environmental protection index and economic benefit of Processes for Producing Acetic Acid.
To achieve the above object, provided technical solution is the utility model:
A kind of acetic synthesis separation and recovery of catalyst device comprising:
Pre-separation tower, top, bottom are respectively equipped with gaseous phase outlet, liquid-phase outlet, and lower part is equipped with gas phase entrance；It is additionally provided with
One circulation fluid entrance, the circulation fluid entry position are higher than the gas phase entry position；One circulation is set outside the pre-separation tower
Pump, the both ends of the circulating pump are separately connected pre-separation tower bottom and pre-separation tower circulation fluid entrance；
Cooler, import are connect by pipeline with the pre-separation tower gaseous phase outlet；
First separator, which is provided with feed inlet, and top, bottom further respectively have gaseous phase outlet, liquid-phase outlet；Described
The feed inlet of one separator is connected by the outlet of pipeline and cooler；
Stripper, upper part are respectively equipped with liquid phase entrance, heavy liquid inlet, and its underpart is equipped with boils liquid entrance, top, bottom again
Portion is respectively equipped with gaseous phase outlet, the outlet of thick acetic acid；The liquid phase entrance of the stripper connects first separator by pipeline
Liquid-phase outlet；
Reboiler, both ends are separately connected stripper bottom and stripper and boil liquid entrance again；
Lightness-removing column, top, bottom are respectively equipped with light phase export, heavy out, are additionally provided with the first gas phase entrance, thereon
Two gas phase entrances, light phase inlet, second gas phase entry position are lower than first gas phase entry position；The lightness-removing column
One gas phase entrance connects the gaseous phase outlet of first separator by pipeline；Second gas phase entrance of the lightness-removing column passes through pipe
Road connects the gaseous phase outlet of the stripper；
First cold cooler, eventually cold cooler are respectively equipped with material inlet, condensate outlet, fixed gas outlet, described just cold
The material inlet of cooler connects the light phase export of the lightness-removing column by pipeline, and the fixed gas outlet of the just cold cooler is logical
What piping connected the end cold cooler has material inlet；The fixed gas outlet of the end cold cooler is low with one by pipeline
Press absorption tower connection；
Second separator sets condensate inlet, material outlet, fixed gas outlet thereon；The condensation of second separator
Liquid entrance connects the condensate outlet of the end cold cooler by pipeline；The fixed gas outlet of second separator passes through pipe
Road is connected to a low-pressure absorption tower；
Quantizer is respectively equipped with condensate inlet, liquid phase entrance, desalination water inlet, light phase export, heavy out thereon；
The quantizer condensate inlet connects just cold cooler condensate outlet by pipeline；The quantizer liquid phase entrance passes through pipe
Road connects the second separator material outlet, and the quantizer desalination water inlet is connected to by pipeline with desalted water water source；Described point
Layer device heavy out passes through pipeline and heavy phase pump connection reaction kettle；The quantizer light phase export divides two-way, passes through pipe all the way
Road and a reflux pump connect the lightness-removing column light phase inlet, and another way removes spirit of vinegar pump connection reaction kettle by pipeline and one.
Further, the liquid phase entrance of the quantizer, desalination water inlet share an entrance by a common conduit.
The gas phase entrance of pre-separation tower in pipeline and the technique of methanol carbonylization manufacture acetic acid by steaming in the utility model
Device connection is sent out, a small amount of rhodium catalyst is entrained with from the gas phase that evaporator is sent to pre-separation tower, by pre-separation tower outer circulation
Pump provides circulating mother liquor and pre-separation tower lower tray washs, and pre-separation tower bottoms keeps water content > 5% in acetic acid, hydrogen iodide
It is most of also to stay in tower reactor, evaporator is then returned together.The preseparator column overhead of pre-separated tower gaseous phase outlet discharge
Material enters gas-liquid two-phase feeding the first separator progress gas-liquid two-phase separation that cooler is cooling, and cooling obtains.First separation
The gas phase that device is isolated enters lightness-removing column and carries out secondary separation, and the light phase isolated sequentially enters just cold cooler, end through top
Cold cooler, the condensation such as iodomethane and methyl acetate, methanol in light phase, wherein in condensate liquid iodomethane density it is big (20 DEG C,
2.279g/ml) and water is insoluble in, so the heavy phase is returned by heavy phase pump into heavy phase is precipitated as in quantizer after quantizer
The reaction kettle returned in the technique of methanol carbonylization manufacture acetic acid recycles.First cool condenser, eventually acetic acid in cold cooler, water and
A small amount of methyl acetate, methanol become light phase, and a part is back to lightness-removing column, stripper, and most of returned by thin acid pump is reacted
Kettle recycles.
The liquid phase that first separator is isolated enters stripper, completes acetate products by high-efficient tower plate in stripper
The thick acetic acid of concentration about 90% is taken out in separation and concentrate, stripper lower part, is sent into dehydrating tower.
It has and follows in pre-separation tower module design in acetic synthesis separation and recovery of catalyst device provided by the utility model
Ring pump, realizes the high efficiente callback of noble metal catalyst, recycles；Lightness-removing column module design realizes co-catalyst iodomethane
With efficiently separating for other light phases, a recovery efficiency is up to 98%, to realize the high efficiente callback of noble metal catalyst, recycles
It utilizes.The gas phase that pre-separation tower is isolated carries out classification cooling (cooling of level-one cooler, cold cooler at the beginning of second level and cooling eventually
Device), realize particular/special requirement of the orderly separation of material with different function tower to phegma component.Lightness-removing column and stripper string
Connection, gas-liquid two-phase are interconnected, and two towers share a reboiler heat supply, realize the concentrate of crude acid and the separation function of light component,
Achieve the purpose that sectional feeding classification separation.
The utility model has the beneficial effects that
The utility model is designed by modularization, function division, realizes expensive rhodium catalyst, co-catalyst iodomethane
It is efficiently separated with thick acetic acid substep, effectively reduces unit product consumption and cost.
Separation and recovery of catalyst device provided by the utility model realizes expensive rhodium catalyst, co-catalyst iodomethane
It is efficiently separated with thick acetic acid substep, reduces the consumption of major catalyst and co-catalyst, while the thick acetic acid that stripper extracts is dense
Degree about 90% further improves dehydrating tower charging acetate concentration, reduces the energy consumption of later separation device, obtain production cost
It obtained and declined to a great extent, and improved the market competitiveness of acetate products, and easily operated, it is at low cost, significantly improve separating effect.
Detailed description of the invention
Fig. 1 is the structure schematic diagram of the utility model embodiment.
Specific embodiment
Below in conjunction with Figure of description and specific embodiment to extremely low temperature pipe line steel of the present invention and its system
The method of making makes further explanation, however the explanation and illustration does not constitute improper limit to technical solution of the present invention
It is fixed.
Embodiment 1
Referring to Fig. 1, a kind of acetic synthesis separation and recovery of catalyst device provided by the utility model comprising,
Pre-separation tower 1, top, bottom are respectively equipped with gaseous phase outlet 101, liquid-phase outlet 102, and lower part is equipped with gas phase entrance
103；It is additionally provided with a circulation fluid entrance 104,104 position of circulation fluid entrance is higher than 103 position of gas phase entrance；It is described pre-
One circulating pump 2 is set outside knockout tower 1, and the both ends of the circulating pump 2 are separately connected 1 bottom of pre-separation tower and pre-separation tower 1 recycles
Liquid entrance 104；
Cooler 3, import are connect by pipeline with 1 gaseous phase outlet 101 of pre-separation tower；
First separator 4, which is provided with feed inlet 401, and top, bottom further respectively have gaseous phase outlet 402, liquid-phase outlet
403；The feed inlet 401 of first separator 4 is connect by pipeline with the outlet of cooler 3；
Stripper 5, upper part are respectively equipped with liquid phase entrance 501, heavy liquid inlet 502, and its underpart is equipped with boils liquid entrance again
503, top, bottom are respectively equipped with gaseous phase outlet 504, thick acetic acid outlet 505；The liquid phase entrance 501 of the stripper 5 passes through
Pipeline connects the liquid-phase outlet 403 of first separator 4；
Reboiler 6, both ends are separately connected 5 bottom of stripper and stripper 5 boils liquid entrance 503 again；
Lightness-removing column 7, top, bottom are respectively equipped with light phase export 701, heavy out 702, are additionally provided with the first gas phase thereon
Entrance 703, the second gas phase entrance 704, light phase inlet 705,704 position of the second gas phase entrance enter lower than first gas phase
703 positions of mouth；The 7 first gas phase entrance 703 of lightness-removing column connects the gaseous phase outlet 402 of first separator 4 by pipeline；
Second gas phase entrance 704 of the lightness-removing column 7 connects the gaseous phase outlet 504 of the stripper 5 by pipeline；
First cold cooler 8, eventually cold cooler 9 are respectively equipped with material inlet 801/901, condensate outlet 802/902, no
The material inlet 801 of solidifying gas outlet 803/903, the just cold cooler 8 connects the light phase export of the lightness-removing column 7 by pipeline
701, the fixed gas outlet 803 of the just cold cooler 8 connects the material inlet 901 of the end cold cooler 9 by pipeline；
The fixed gas outlet 903 of the end cold cooler 9 is connected to by pipeline with a low-pressure absorption tower A；
Second separator 10 sets condensate inlet 1001, material outlet 1002, fixed gas outlet 1003 thereon；Described
The condensate inlet 1001 of two separators 10 connects the condensate outlet 902 of the end cold cooler 9 by pipeline；Described second
The fixed gas outlet 1003 of separator 10 is connected to by pipeline with low-pressure absorption tower A；
Quantizer 11 is respectively equipped with condensate inlet 1101, liquid phase entrance 1102, desalination water inlet 1103, light phase thereon
Export 1104, heavy out 1105；By pipeline connection, just cold cooler 8 condenses 11 condensate inlet 1101 of quantizer
Liquid outlet 802；The 11 liquid phase entrance 1102 of quantizer by pipeline connect 10 material outlet 1002 of the second separator, described point
Layer 11 desalination water inlet 1103 of device is connected to by pipeline with desalted water water source；11 heavy out 1105 of quantizer passes through pipe
12 connection reaction kettle B of road and heavy phase pump；11 light phase export 1104 of quantizer divides two-way, a-road-through piping and a reflux
13 connection 7 light phase inlet 705 of lightness-removing column of pump, another way pass through 14 connection reaction kettle B of pipeline and a pump.
Further, the liquid phase entrance 1102 of the quantizer 11, desalination water inlet 1103 share one by a common conduit
Entrance.
The gas phase entrance 103 of pre-separation tower 1 is manufactured in the technique of acetic acid by pipeline and methanol carbonylization in the present embodiment
Evaporator C connection, is entrained with a small amount of rhodium catalyst, by pre-separation tower 1 from the gas phase that evaporator C is sent to pre-separation tower 1
Outer circulation pump 2 provides circulating mother liquors and 1 lower tray of pre-separation tower and washs, pre-separation tower bottoms keep water content in acetic acid >
5%, hydrogen iodide largely also stays in tower reactor, then returns evaporator C together.Pre-separated 1 gaseous phase outlet 101 of tower discharge
Preseparator column overhead material enters gas-liquid two-phase feeding the first separator 4 progress gas-liquid that cooler 3 is cooling, and cooling obtains
Two-phase laminated flow.The gas phase that first separator 4 is isolated enter lightness-removing column 7 carry out secondary separation, the light phase isolated through top according to
It is secondary to enter first cold cooler 8, eventually cold cooler 9, the condensation such as iodomethane and methyl acetate, methanol in light phase, wherein in condensate liquid
Iodomethane density big (20 DEG C, 2.279g/ml) and it is insoluble in water, so into being precipitated as after quantizer 11 in quantizer 11
Heavy phase, the heavy phase manufacture the reaction kettle A in the technique of acetic acid by 12 return methanol carbonylization of heavy phase pump and recycle.It is just cold
Acetic acid, water and a small amount of methyl acetate, methanol become light phase in condenser 8, whole cold cooler 9, and a part is back to lightness-removing column 7, vapour
Stripper 5, it is most of to be recycled by thin acid pump return reaction kettle B.
The liquid phase that first separator 4 is isolated enters stripper 5, completes acetic acid by high-efficient tower plate in stripper 5 and produces
The thick acetic acid of concentration about 90% is taken out in the separation and concentrate of product, 5 lower part of stripper, is sent into dehydrating tower D.
The utility model is designed by modularization, function division, realizes expensive rhodium catalyst, co-catalyst iodomethane
It is efficiently separated with thick acetic acid substep, reduces the consumption of main co-catalyst, while it is dense to further improve dehydrating tower charging acetic acid
Degree, reduces the energy consumption of later separation device, production cost is made to be declined to a great extent, improve the market competition of acetate products
Power.
Claims (2)
1. a kind of acetic synthesis separation and recovery of catalyst device, which is characterized in that including,
Pre-separation tower, top, bottom are respectively equipped with gaseous phase outlet, liquid-phase outlet, and lower part is equipped with gas phase entrance；It is additionally provided with circulation
Liquid entrance, the circulation fluid entry position are higher than the gas phase entry position；One circulating pump is set outside the pre-separation tower, it is described
The both ends of circulating pump are separately connected pre-separation tower bottom and pre-separation tower circulation fluid entrance；
Cooler, import are connect by pipeline with the pre-separation tower gaseous phase outlet；
First separator, which is provided with feed inlet, and top, bottom further respectively have gaseous phase outlet, liquid-phase outlet；Described first point
Feed inlet from device is connected by the outlet of pipeline and cooler；
Stripper, upper part are respectively equipped with liquid phase entrance, heavy liquid inlet, and its underpart is equipped with boils liquid entrance again, top, bottom point
It She You not gaseous phase outlet, the outlet of thick acetic acid；The liquid phase entrance of the stripper connects the liquid of first separator by pipeline
Mutually export；
Reboiler, both ends are separately connected stripper bottom and stripper and boil liquid entrance again；
Lightness-removing column, top, bottom are respectively equipped with light phase export, heavy out, are additionally provided with the first gas phase entrance, the second gas thereon
Phase entrance, light phase inlet, second gas phase entry position are lower than first gas phase entry position；First gas of lightness-removing column
Phase entrance connects the gaseous phase outlet of first separator by pipeline；Second gas phase entrance of the lightness-removing column is connected by pipeline
Connect the gaseous phase outlet of the stripper；
First cold cooler, eventually cold cooler are respectively equipped with material inlet, condensate outlet, fixed gas outlet, the just cooling
The material inlet of device connects the light phase export of the lightness-removing column by pipeline, and the fixed gas outlet of the just cold cooler passes through pipe
What road connected the end cold cooler has material inlet；It is inhaled by pipeline and a low pressure fixed gas outlet of the end cold cooler
Receive tower connection；
Second separator sets condensate inlet, material outlet, fixed gas outlet thereon；The condensate liquid of second separator enters
Mouth connects the condensate outlet of the end cold cooler by pipeline；Second separator fixed gas outlet by pipeline with
The connection of one low-pressure absorption tower；
Quantizer is respectively equipped with condensate inlet, liquid phase entrance, desalination water inlet, light phase export, heavy out thereon；It is described
Quantizer condensate inlet connects just cold cooler condensate outlet by pipeline；The quantizer liquid phase entrance is connected by pipeline
The second separator material outlet is connect, the quantizer desalination water inlet is connected to by pipeline with desalted water water source；The quantizer
Heavy out passes through pipeline and heavy phase pump connection reaction kettle；The quantizer light phase export divides two-way, a-road-through piping and
One reflux pump connects the lightness-removing column light phase inlet, and another way removes spirit of vinegar pump connection reaction kettle by pipeline and one.
2. acetic synthesis separation and recovery of catalyst device according to claim 1, which is characterized in that the liquid of the quantizer
Phase entrance, desalination water inlet share an entrance by a common conduit.
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| CN201821648157.5U CN208995418U (en) | 2018-10-11 | 2018-10-11 | A kind of acetic synthesis separation and recovery of catalyst device |
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| CN201821648157.5U CN208995418U (en) | 2018-10-11 | 2018-10-11 | A kind of acetic synthesis separation and recovery of catalyst device |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111039775A (en) * | 2018-10-11 | 2020-04-21 | 河南顺达新能源科技有限公司 | Acetic acid synthesis catalyst separation recovery unit |
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2018
- 2018-10-11 CN CN201821648157.5U patent/CN208995418U/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111039775A (en) * | 2018-10-11 | 2020-04-21 | 河南顺达新能源科技有限公司 | Acetic acid synthesis catalyst separation recovery unit |
| CN111039775B (en) * | 2018-10-11 | 2024-05-14 | 河南顺达新能源科技有限公司 | Acetic acid synthesis catalyst separation recovery unit |
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