CN110327678A - A kind of separating and reclaiming device and technique of the hydration catalyst of cyclohexene hydration cyclohexanol technique - Google Patents
A kind of separating and reclaiming device and technique of the hydration catalyst of cyclohexene hydration cyclohexanol technique Download PDFInfo
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- CN110327678A CN110327678A CN201910694012.1A CN201910694012A CN110327678A CN 110327678 A CN110327678 A CN 110327678A CN 201910694012 A CN201910694012 A CN 201910694012A CN 110327678 A CN110327678 A CN 110327678A
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- filter
- hydration
- separator
- cyclohexene
- coalescing
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- HGCIXCUEYOPUTN-UHFFFAOYSA-N cyclohexene Chemical compound C1CCC=CC1 HGCIXCUEYOPUTN-UHFFFAOYSA-N 0.000 title claims abstract description 106
- 238000006703 hydration reaction Methods 0.000 title claims abstract description 91
- 230000036571 hydration Effects 0.000 title claims abstract description 77
- 239000003054 catalyst Substances 0.000 title claims abstract description 59
- HPXRVTGHNJAIIH-UHFFFAOYSA-N cyclohexanol Chemical compound OC1CCCCC1 HPXRVTGHNJAIIH-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 30
- 239000007788 liquid Substances 0.000 claims abstract description 69
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 29
- 230000008676 import Effects 0.000 claims abstract description 22
- 238000000605 extraction Methods 0.000 claims abstract description 13
- 238000004064 recycling Methods 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 34
- 238000001914 filtration Methods 0.000 claims description 25
- 230000007246 mechanism Effects 0.000 claims description 14
- 238000004581 coalescence Methods 0.000 claims description 12
- 238000000926 separation method Methods 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 9
- 239000003513 alkali Substances 0.000 claims description 8
- 238000010276 construction Methods 0.000 claims description 8
- 238000007789 sealing Methods 0.000 claims description 8
- 239000012530 fluid Substances 0.000 claims description 6
- 239000013589 supplement Substances 0.000 claims description 6
- 238000005452 bending Methods 0.000 claims description 4
- 239000002699 waste material Substances 0.000 claims description 4
- 230000009471 action Effects 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 238000011084 recovery Methods 0.000 claims description 3
- 239000012141 concentrate Substances 0.000 claims description 2
- 239000011148 porous material Substances 0.000 claims description 2
- 239000000047 product Substances 0.000 abstract description 15
- 238000006243 chemical reaction Methods 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 238000010586 diagram Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 229910021536 Zeolite Inorganic materials 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000002808 molecular sieve Substances 0.000 description 3
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 3
- 239000010457 zeolite Substances 0.000 description 3
- ATQUFXWBVZUTKO-UHFFFAOYSA-N 1-methylcyclopentene Chemical compound CC1=CCCC1 ATQUFXWBVZUTKO-UHFFFAOYSA-N 0.000 description 2
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- JBKVHLHDHHXQEQ-UHFFFAOYSA-N epsilon-caprolactam Chemical compound O=C1CCCCCN1 JBKVHLHDHHXQEQ-UHFFFAOYSA-N 0.000 description 2
- 238000011010 flushing procedure Methods 0.000 description 2
- ZSIAUFGUXNUGDI-UHFFFAOYSA-N hexan-1-ol Chemical compound CCCCCCO ZSIAUFGUXNUGDI-UHFFFAOYSA-N 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000009434 installation Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 235000011037 adipic acid Nutrition 0.000 description 1
- 239000001361 adipic acid Substances 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 239000000872 buffer Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- HPXRVTGHNJAIIH-PTQBSOBMSA-N cyclohexanol Chemical group O[13CH]1CCCCC1 HPXRVTGHNJAIIH-PTQBSOBMSA-N 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 239000012065 filter cake Substances 0.000 description 1
- -1 hexamethylene alcohol Chemical compound 0.000 description 1
- 238000006317 isomerization reaction Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000002075 main ingredient Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 239000012264 purified product Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 230000010148 water-pollination Effects 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/02—Separation of non-miscible liquids
- B01D17/0202—Separation of non-miscible liquids by ab- or adsorption
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D29/00—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor
- B01D29/11—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor with bag, cage, hose, tube, sleeve or like filtering elements
- B01D29/31—Self-supporting filtering elements
- B01D29/33—Self-supporting filtering elements arranged for inward flow filtration
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D29/00—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor
- B01D29/50—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor with multiple filtering elements, characterised by their mutual disposition
- B01D29/52—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor with multiple filtering elements, characterised by their mutual disposition in parallel connection
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D29/00—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor
- B01D29/62—Regenerating the filter material in the filter
- B01D29/66—Regenerating the filter material in the filter by flushing, e.g. counter-current air-bumps
- B01D29/68—Regenerating the filter material in the filter by flushing, e.g. counter-current air-bumps with backwash arms, shoes or nozzles
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/86—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by liquid-liquid treatment
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/005—Processes comprising at least two steps in series
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/10—Purification; Separation; Use of additives by extraction, i.e. purification or separation of liquid hydrocarbons with the aid of liquids
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2601/00—Systems containing only non-condensed rings
- C07C2601/12—Systems containing only non-condensed rings with a six-membered ring
- C07C2601/14—The ring being saturated
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2601/00—Systems containing only non-condensed rings
- C07C2601/12—Systems containing only non-condensed rings with a six-membered ring
- C07C2601/16—Systems containing only non-condensed rings with a six-membered ring the ring being unsaturated
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Water Supply & Treatment (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
Abstract
A kind of separating and reclaiming device of the hydration catalyst of cyclohexene hydration cyclohexanol technique, including separator, cooler, filter, surge tank, and cyclohexene extraction tower, the reaction product import of the separator connects feed pipe, for being connect with hydration reactor, the light phase export of separator with cyclohexanol knockout tower for connecting, the heavy out of separator is through cooler, it is connect with the feed inlet of filter, the feed inlet of the filter, slag-drip opening is located at the lower section of filter medium, the liquid outlet of the filter is located at the top of filter medium, the import of the surge tank is connect with the liquid outlet of the filter, the outlet of surge tank is fed cyclohexene extraction tower by dehvery pump.The configuration of the present invention is simple, operating cost are low, can efficiently separate purpose product and hydration catalyst in recycling cyclohexene hydration reaction product.
Description
Technical field
The present invention relates to chemical field, in particular to a kind of separation of the hydration catalyst of cyclohexene hydration cyclohexanol technique
Recyclable device and technique.
Background technique
Cyclohexanol is for field of new materials cyclohexanone, adipic acid and caprolactam important source material.Know and has passed through hexamethylene
The hydration reaction of alkene carrys out synthesizing cyclohexanol, the rear hexamethylene that high boiling fraction and low boiling fraction seperation are obtained to purifying by distilling
Alcohol.
Cyclohexene and water are under the action of zeolite molecular sieve catalyst, and 120~130 DEG C, under conditions of 0.5~0.6MPaG,
Cyclohexene and water are hydrated under the action of zeolite molecular sieve catalyst generates cyclohexanol, generates hexamethylene in general, cyclohexene is catalyzed
The zeolite molecular sieve catalyst of alcohol is commonly called as " hydration catalyst ".
During cyclohexene hydration reaction generates cyclohexanol, the separation and recycling of hydration catalyst seem most important.
If hydration catalyst separation is not thorough, it is bound to cause the waste of hydration catalyst, in addition, hydration catalyst can also in rear system
Cause the side reaction of cyclohexanol and cyclohexene.
As dehydration of cyclohexanol generates cyclohexene:
As the isomerization of cyclohexene generates methyl cyclopentene:
Currently, the hydration catalyst design consumption of cyclohexanol production device is mostly at 0.2~0.25kg/t (cyclohexanol), with
For producing 200000 tons of cyclohexanol device per year, hydration catalyst about 120~150kg is consumed daily, consumes hydration catalyst about in year
40~50t also will cause the generation of back reaction if if not being subject to recycling, being bound to cause a large amount of wastes of hydration catalyst, drop
Low device conversion ratio, and will cause the increase of by-product methyl cyclopentene, reduce plant yield.
Therefore, how to design a kind of device that can efficiently separate recycling hydration catalyst, be those skilled in the art urgently
It solves the problems, such as.
Summary of the invention
An object of the present invention is in view of the deficiencies of the prior art, to provide a kind of water of cyclohexene hydration cyclohexanol technique
The separating and reclaiming device of catalyst is closed, structure is simple, operating cost is low, can efficiently separate recycling cyclohexene hydration reaction product
In purpose product and hydration catalyst.
The second object of the present invention is to provide a kind of separation and recovery of the hydration catalyst of cyclohexene hydration cyclohexanol technique
Technique, the simple process, easy to operate, the purpose product and hydration that can be efficiently separated in recycling cyclohexene hydration reaction product are urged
Agent.
Realizing the technical solution of one of the object of the invention is, a kind of hydration catalyst of cyclohexene hydration cyclohexanol technique
Separating and reclaiming device, including separator, cooler, filter, surge tank and cyclohexene extraction tower, the separator it is anti-
Product inlet is answered to connect feed pipe, for connecting with hydration reactor, the light phase export of separator is used for and cyclohexanol knockout tower
Connection, the heavy out of separator are connect through cooler with the feed inlet of filter, the feed inlet of the filter, slag-drip opening position
In the lower section of filter medium, the liquid outlet of the filter is located at the top of filter medium, the import of the surge tank and the mistake
The liquid outlet of filter connects, and the outlet of surge tank is fed cyclohexene extraction tower by dehvery pump.
The separator includes separator tank body, and the separator tank body is in horizontally-arranged tubular construction, and sealing two ends, point
Reaction product import is set in the middle part of one end from device tank body, and light phase export is arranged in the top of the other end of separator tank body, another
Heavy out is arranged in the bottom at end, and liquid shield, coalescence mechanism, the liquid shield are equipped in the inner cavity of the separator tank body
L-shaped structure, the horizontal sides of the liquid shield of L-shaped structure are fixed on separator tank body one end, positioned at reaction product import
The vertical edge of top, the liquid shield of L-shaped structure is corresponding with reaction product import, and has interval, forms cushion space, institute
The middle part that coalescence mechanism is located at the inner cavity of separator tank body is stated, coalescence mechanism includes the coalescing-plate of several bendings that are serrated, respectively
The overbending direction of coalescing-plate extends along the length of separator tank body, and the angle α where each coalescing-plate between plane and plumb line is
10-80 °, these coalescing-plates are in arranged in parallel, and have spacing distance, between each coalescing-plate upper end and separator inner tank wall
Apart from identical, each coalescing-plate lower end is identical as the distance between separator inner tank wall, and the sawtooth height H of coalescing-plate is greater than adjacent
The distance between two coalescing-plates h makes the clearance space between two neighboring coalescing-plate form fluid flow paths.
The filter includes filter housings and several filter cores, and the filter housings are in vertical tubular construction,
And sealing two ends, the inner cavity of filter housings are arranged a horizontal-extending mounting plate, the inner cavity of filter housings are divided into phase
Mutual independent first chamber, second chamber, first chamber are located at the top of second chamber, feed inlet, the slag-drip opening of the filter
It being connected to second chamber, the liquid outlet of the filter is connected to first chamber, and the filter core includes filtering outer cylinder, recoil inner cylinder,
The recoil inner cylinder is set to one heart in filtering outer cylinder, and has clearance space, and the filtering outer cylinder is equipped with several filter openings, each to filter
The aperture in hole is 0.5-2 μm, and the recoil inner cylinder is equipped with several recoil holes, and each filter core is uniformly arranged in second chamber, with
Mounting plate is fixedly connected, and is connected to the nozzle for filtering outer cylinder, the nozzle for the inner cylinder that recoils with first chamber.
Setting recoil water inlet, the recoil water inlet are in parallel with the recoil inner cylinder of each filter core on the filter housings.
Alkali liquid washing mouth is set on the filter housings, and the alkali liquid washing mouth is in parallel with the recoil inner cylinder of each filter core.
The feed pipe is equipped with water supplement port.
Realizing two technical solution of the object of the invention is, separates and recovers hydration using any of the above-described separating and reclaiming device
The technique of catalyst, has follow steps:
1) cyclohexene hydration reaction product enters in separator through feed pipe, and the temperature of cyclohexene hydration reaction product is
120-130 DEG C, pressure 0.5-0.6MPa, disengaging time 10-45min；
2) light phase of the light phase export discharge of separator enters cyclohexanol knockout tower, the weight of the heavy out discharge of separator
It is mutually cooled to through cooler lower than 100 DEG C, filter is entered by the feed inlet of filter；
3) the feed inlet pressure of filter is 0.5-0.6MPa, and the liquid outlet pressure of filter is 0-0.1MPa, liquid outlet
The clear liquid of discharge enters surge tank, is pumped by dehvery pump to cyclohexene extraction tower, recycles cyclohexanol as raw material；
4) the slag-drip opening discharge concentrate and hydration catalyst of filter, for recycling or waste disposal.
It is added water in the feed pipe of step 1), the volume ratio of water and cyclohexene hydration reaction product is 1:10-150.
The pore size filter of the filter medium of step 3) filter is 0.5-2 μm.
It has the advantages that by adopting the above technical scheme
1, the separating and reclaiming device of the hydration catalyst of cyclohexene hydration cyclohexanol technique includes separator, cooler, mistake
Filter and surge tank, for separator therein for the light phase and heavy phase in separating cyclohexene hydration reaction product, light phase is main
Ingredient is cyclohexanol, and a small amount of cyclohexene and water, and heavy phase main component is water, and hydration catalyst and impurity on a small quantity, cold
But device avoids filtering medium openings from changing because of temperature change, guarantees that filter is stable, normal for keeping heavy phase temperature constant
Work, filter produce cyclohexanol for heavy phase, and the hydration catalyst in effectively catching heavy phase to be concentrated, for cyclohexene hydration
Process cycles use.The reaction product import of the separator connects feed pipe, for being connect with hydration reactor, separator
For connecting with cyclohexanol knockout tower, the heavy out of separator is connect through cooler with the feed inlet of filter light phase export,
The hydrated product of hydration reactor production enters in separator through feed pipe, and washed separation is final to be layered, and light phase is gone out by light phase
Mouth is discharged into cyclohexanol knockout tower, is discharged by heavy out, is dropped through cooler for further separation, purified product, heavy phase
Temperature and after keeping constant, is further concentrated into filter and retains hydration catalyst.The feed inlet of the filter, slag-drip opening position
In the lower section of filter medium, the liquid outlet of the filter is located at the top of filter medium, and the heavy phase of constant temperature is under filter medium
Side enters in filter, and after being tentatively layered, filter medium is crossed in the clear liquid cross flow in heavy phase, is discharged by liquid outlet, in heavy phase
Impurity and hydration catalyst are retained by filter medium, are assembled, are concentrated in the filter, and be directly discharged by slag-drip opening, are facilitated back
It receives, processing hydration catalyst.The import of the surge tank is connect with the liquid outlet of the filter, and the outlet of surge tank passes through defeated
Material pump is connect with feed pipe, filters the clear liquid of discharge after surge tank buffers, and is pumped to cyclohexene extraction tower, is recycled hexamethylene therein
Alcohol is as raw material.
2, separator of the present invention includes separator tank body, and separator tank body is in horizontally-arranged tubular construction, and sealing two ends, point
Reaction product import is set in the middle part of one end from device tank body, and light phase export is arranged in the top of the other end of separator tank body, another
Heavy out is arranged in the bottom at end, and hydrated product is entered the inner cavity of separator tank body by one end of separator tank body, along horizontal position
The other end is moved to, and is gradually disengaged, is layered and is discharged in the other end.It is equipped with liquid shield in the inner cavity of the separator tank body, gathers
Mechanism, the L-shaped structure of liquid shield are tied, the horizontal sides of the liquid shield of L-shaped structure are fixed on separator tank body one end,
Positioned at the top of reaction product import, the vertical edge of the liquid shield of L-shaped structure is corresponding with reaction product import, and between having
Every, form cushion space, into separator pot intracoelomic cavity hydrated product impinge upon liquid shield vertical edge on, slow down, be slow
After punching, it is displaced at a slow speed towards the separator tank body other end, in displacement process, light phase, heavy phase component delamination, the more liquid toward upper layer
Body is the higher light phase of accounting, is more the higher heavy phase of accounting toward the liquid of lower layer.The coalescence mechanism is located at separator tank body
Inner cavity middle part, coalescence mechanism include several bendings that are serrated coalescing-plate, the overbending direction of each coalescing-plate is along separator
The length of tank body extends, and the angle α where each coalescing-plate between plane and plumb line is 10-80 °, these coalescing-plates are in parallel
Column, and have spacing distance, each coalescing-plate upper end is identical with the distance between separator inner tank wall, each coalescing-plate lower end with divide
Identical from the distance between device inner tank wall, the sawtooth height H of coalescing-plate is greater than the distance between two neighboring coalescing-plate h, makes
Clearance space between two neighboring coalescing-plate forms fluid flow paths, and fluid flow passageway is located at coalescing-plate sawtooth tooth tip
Circulation area expand, into the small liquid pearl of the light phase accelerating impact first in the hydrated product of fluid flow paths in coalescing-plate one
On a flank of tooth, slowed down, gather into the big liquid pearl of light phase, and under buoyancy, along the short transverse direction separation of coalescing-plate
The upper layer of device tank inner chamber is mobile, until the other end for being detached from coalescing-plate continuation towards separator tank body is mobile, in hydrated product
The same accelerating impact of hydration catalyst little particle is slowed down on a flank of tooth of coalescing-plate, gathers into bulky grain, and in weight
It under effect, is moved along the lower layer of short transverse towards the separator pot intracoelomic cavity of coalescing-plate, until being detached from coalescing-plate continues direction
The separator tank body other end is mobile.Hydrated product after being slowed down for the first time, being coalesced slows down again in coalescing-plate tooth tip position (to circulate
Area expands), it after turning, again speeds up (circulation area becomes smaller) and impinges upon on another flank of tooth of adjacent coalescing-plate, hydrated product
In the small liquid pearl of light phase slowed down, gather into the big liquid pearl of light phase, and under buoyancy, along the short transverse direction of coalescing-plate
The upper layer of separator pot intracoelomic cavity is mobile, until being detached from coalescing-plate continues, hydrated product mobile towards the other end of separator tank body
In hydration catalyst little particle slowed down, gather into bulky grain, and under weight effect, along the short transverse court of coalescing-plate
It is mobile to the lower layer of separator pot intracoelomic cavity, continue until being detached from coalescing-plate towards the movement of the separator tank body other end.By multiple
Accelerate, slow down, turning, light phase, the heavy phase being effectively ensured in hydrated product are completely separated, and improve separating effect.
3, filter of the present invention includes filter housings and several filter cores, and filter housings are in vertical tubular construction,
And sealing two ends, the inner cavity of filter housings are arranged a horizontal-extending mounting plate, the inner cavity of filter housings are divided into phase
Mutual independent first chamber, second chamber, first chamber are located at the top of second chamber, feed inlet, the slag-drip opening of the filter
It is connected to second chamber, the liquid outlet of the filter is connected to first chamber.The filter core includes filtering outer cylinder, recoil inner cylinder,
The recoil inner cylinder is set to one heart in filtering outer cylinder, and has clearance space, and the filtering outer cylinder is equipped with several filter openings, each to filter
The aperture in hole is 0.5-2 μm, and the recoil inner cylinder is equipped with several recoil holes, and each filter core is uniformly arranged in second chamber, with
Mounting plate is fixedly connected, and is connected to the nozzle for filtering outer cylinder, the nozzle for the inner cylinder that recoils with first chamber, due to hydration catalyst grain
For diameter distribution between 0.5-5 μm, hydration catalyst is mobile towards filter core under pressure, and there is a small amount of little particle water at initial stage
It closes catalyst and passes through filter opening, bulky grain hydration catalyst then forms cake layer in cartridge surface, and with the increasing of cake layer thickness
Add, the duct in cake layer is less than the partial size of hydration catalyst, clear liquid permeation filtration cake layer and filter opening, into filter core inside be discharged into
First chamber is discharged by liquid outlet, and hydrated solid particle is trapped within second chamber, therefore, if too small, water is arranged in filter opening aperture
It closes catalyst and easily blocks filter opening, need frequent clean, influence normal operation, if the setting of filter opening aperture is excessive, filter initial stage water
It closes catalyst to be not easy to form filter cake, excessive hydration catalyst is caused to be discharged across filter core, influence the retention effect of hydration catalyst
Rate.Cake layer thickness is thicker, and pressure needed for filtering is bigger, until filtering is terminated, to each filter when the clear liquid amount of liquid outlet discharge is smaller
The recoil inner cylinder of core filters outer tube inner wall, will filter outer cylinder table for backwash liquid, recoil hole directive of the backwash liquid on recoil inner cylinder
Cake layer is formed on face to rinse out, and is discharged by slag-drip opening, guarantees that filter operates normally, and recycling, processing hydration is facilitated to urge
Agent.
4, the recoil inner cylinder of setting recoil water inlet on filter housings of the present invention, the recoil water inlet and each filter core is simultaneously
Join, the cake layer washed away in cartridge surface for providing back-flushing, alkali liquid washing mouth, the alkali liquid washing are set on filter housings
Mouthful in parallel with the recoil inner cylinder of each filter core, the filter core after back-flushing washes away is washed away by lye again, and small in filter core filter opening
The reaction of particle hydration catalyst thoroughly restores the strainability of filter core at thinner cotton-shaped particle.
5, in present invention process, in feed pipe plus water, since hydration catalyst has hydrophily, the water of addition can promote water
It closes catalyst to separate into water, into heavy phase, if the hypervolia of addition, the sewage quantity of generation is larger, reduces point of separator
From efficiency and the filter efficiency of filter, if the water of addition is too small, the serious washing and separation for reducing hydration catalyst
Effect.
6, the pressure 0.5-0.6MPa of present invention control hydrated product, liquid outlet pressure are 0-0.1MPa, the maximum of filtering
Power pressure difference is 0.6MPa, meets the needs of filtering power by the pressure of heavy phase itself, does not need outside power pressurization dress
It sets.
It is further described with reference to the accompanying drawings and detailed description.
Detailed description of the invention
Fig. 1 is connection schematic diagram of the invention；
Fig. 2 is the structural schematic diagram of filter of the present invention；
Fig. 3 is the structural schematic diagram of filter core of the present invention；
Fig. 4 is the structural schematic diagram of separator of the present invention；
Fig. 5 is the distribution map of present invention aggregation mechanism；
Fig. 6 is the cross-sectional view of separator of the present invention；
Fig. 7 is the arrangement schematic diagram of coalescing-plate of the present invention.
In attached drawing, 1 is separator, and 1a is reaction product import, and 1b is light phase export, and 1c is heavy out, and 11 be separation
Device tank body, 12 be liquid shield, and 13 be coalescence mechanism, and 14 be cushion space, and 15 be coalescing-plate, and 16 be fluid flow paths, and 2 are
Cooler, 3 be filter, and 3a is feed inlet, and 3b is slag-drip opening, and 3c is liquid outlet, and 31 be filter housings, and 32 be filter core, 33
It is first chamber for mounting plate, 34,35 be second chamber, and 36 be filtering outer cylinder, and 37 be recoil inner cylinder, and 38 be recoil water inlet,
39 be alkali liquid washing mouth, and 4 be surge tank, and 4a is import, and 4b is outlet, and 5 be feed pipe, and 5a is water supplement port, and 6 be dehvery pump, and 7 are
Cyclohexene extraction tower.
Specific embodiment
In the present invention, the equipment for not indicating specific connection type, item usually according to normal condition or according to the manufacturer's recommendations
Part carries out, the equipment for not indicating concrete model, usually the equipment of chemical field routine.
It is a kind of tool of the separating and reclaiming device of the hydration catalyst of cyclohexene hydration cyclohexanol technique referring to Fig. 1 to Fig. 7
Body embodiment.The separating and reclaiming device that cyclohexene hydration produces the hydration catalyst of cyclohexanol technique includes separator 1, cooler
2, filter 3, surge tank 4 and cyclohexene extraction tower 7.The reaction product import 1a connection feed pipe 5 of the separator 1 is used
It is connect in hydration reactor, specifically, the feed pipe 5 is equipped with water supplement port 5a.The light phase export 1b of separator 1 is used for and ring
The connection of hexanol knockout tower, the heavy out 1c of separator 1 are connect, the present embodiment through cooler 2 with the feed inlet 3a of filter 3
In, separator 1 includes separator tank body 11, and the separator tank body 11 is in horizontally-arranged tubular construction, and sealing two ends, usually
, at the both ends of separator tank body respectively by being threadedly engaged end cap, is sealed, facilitate installation, disassembly.Separator tank body 11
One end in the middle part of reaction product import 1a is set, light phase export 1b, the other end is arranged in the top of the other end of separator tank body 11
Bottom heavy out 1c is set, liquid shield 12, coalescence mechanism 13, the liquid are equipped in the inner cavity of the separator tank body 11
The L-shaped structure of body baffle 12, the horizontal sides of the liquid shield 12 of L-shaped structure are fixed on 11 one end of separator tank body, are located at anti-
The top for answering product inlet 1a can be used bolt and fix, can also be used and be welded and fixed.The liquid shield 12 of L-shaped structure erects
Straight flange is corresponding with reaction product import 1a, and has interval, forms cushion space 14, lower end, front end, the rear end of the cushion space
It is connected to separator pot intracoelomic cavity.The coalescence mechanism 13 is located at the middle part of the inner cavity of separator tank body 11, coalesces mechanism 13
Coalescing-plate 15 including several bendings that are serrated, specifically, being 17 pieces.The overbending direction of each coalescing-plate 15 is along separator pot
The length of body 11 extends, and the angle α between each 15 place plane of coalescing-plate and plumb line is 10-80 °, specifically, angle α is
27°.These coalescing-plates 15 have spacing distance in arranged in parallel, each 15 upper end of coalescing-plate and 11 inner wall of separator tank body it
Between distance it is identical, each 15 lower end of coalescing-plate is identical as the distance between 11 inner wall of separator tank body, and the sawtooth of coalescing-plate 15 is high
It spends H and is greater than the distance between two neighboring coalescing-plate 15 h, the clearance space between two neighboring coalescing-plate 15 is made to form liquid flow
Circulation passage 16.Feed inlet 3a, the slag-drip opening 3b of the filter 3 are located at the lower section of filter medium, and liquid outlet 3c of the filter 3
In the top of filter medium, in the present embodiment, filter 3 includes filter housings 31 and several filter cores 32, the filter
Shell 31 is in vertical tubular construction, and sealing two ends are common, is threadedly engaged end cap at the both ends of filter housings and is sealed
Mouthful, facilitate installation, disassembly.A horizontal-extending mounting plate 33 is arranged in the inner cavity of filter housings 31, by filter housings 31
Inner cavity is divided into mutually independent first chamber 34, second chamber 35, and first chamber 34 is located at the top of second chamber 35.The mistake
Feed inlet 3a, the slag-drip opening 3b of filter 3 are connected to second chamber 35, and the liquid outlet 3c of the filter 3 is connected to first chamber 34,
Specifically, feed inlet 3a is located on the side wall of filter housings, slag-drip opening is located at the bottom of filter housings, and liquid outlet was located at
The top of filter shell.The filter core 32 includes filtering outer cylinder 36, recoil inner cylinder 37, and the recoil inner cylinder 37 is set to filtering with one heart
In outer cylinder 36, and there is clearance space, it is common, it is arranged multiple supports along its length between recoil inner cylinder and filtering outer cylinder
Ring, the inner ring of support ring and the cooperation of recoil inner cylinder periphery, the outer ring of support ring and the inner wall of filtering outer cylinder cooperate, and form whole knot
Structure.The filtering outer cylinder 36 is equipped with several filter openings, and the aperture of each filter opening is 0.5-2 μm, and common, these filter openings are outer along filtering
The side wall of cylinder is uniformly distributed.The recoil inner cylinder 37 is equipped with several recoil holes, common, these recoil holes are along recoil inner cylinder
Side wall is uniformly distributed, and the aperture in hole of recoiling is greater than the aperture of filter opening.Each filter core 32 is uniformly arranged in second chamber 35, with peace
Loading board 33 is fixedly connected, and is connected to the nozzle for filtering outer cylinder 36, the nozzle for the inner cylinder 37 that recoils with first chamber 34, specifically,
Several threaded holes are uniformly arranged on mounting plate, filter core is threadedly engaged with threaded hole, is uniformly arranged on a mounting board.The surge tank
4 import 4a is connect with the liquid outlet 3c of the filter 3, and the outlet 4b of surge tank 4 is by dehvery pump 6 to cyclohexene extraction tower
Feed recycles the cyclohexene in clear liquid, as hydrated feedstock.
Further, in order to thoroughly restore the strainability of filter core, setting recoil water inlet 38 on filter housings 31 should
The water inlet 38 that recoils is in parallel with the recoil inner cylinder 37 of each filter core 32, and alkali liquid washing mouth 39, the lye are arranged on filter housings 31
It is in parallel with the recoil inner cylinder 37 of each filter core 32 to wash mouth 39.
Using the technique of above-mentioned separating and reclaiming device separation and recovery hydration catalyst, have follow steps:
1) cyclohexene hydration reaction product enters in separator through feed pipe, and the temperature of cyclohexene hydration reaction product is
125 DEG C, pressure 0.55MPa, by the desalted water of water supplement port supplement 1/50th volume of hydration reaction product (flow), stop
Stay time 32min；
2) light phase of the light phase export discharge of separator enters cyclohexanol knockout tower, the weight of the heavy out discharge of separator
100 DEG C mutually are cooled to through cooler, filter is entered by the feed inlet of filter；
3) the feed inlet pressure of filter is 0.55MPa, and the liquid outlet pressure of filter is 0MPa, and liquid outlet is discharged clear
Liquid enters surge tank, is pumped by dehvery pump to cyclohexene extraction tower, recycles cyclohexene therein；
4) cartridge surface forms the cake layer of 3mm thickness, and cake layer is removed dry weighing and obtains hydration catalyst.
The hydration catalyst of recycling is tested for the property:
Test equipment: the stainless steel cauldron of 1L, band stirring；Hydration catalyst 93g adds water 280mL, and cyclohexene is added
200mL；
Reaction condition: 125 DEG C of reaction temperature, reaction pressure 0.55-0.6MPa, reaction time 30min, speed of agitator
600r/min；
Oily phase after gas chromatographic analysis is reacted, hexamethylene alcohol content reach 9.1% (w), illustrate the hydration catalysis of recycling
Agent has very big use value.
Claims (9)
1. a kind of separating and reclaiming device of the hydration catalyst of cyclohexene hydration cyclohexanol technique, it is characterised in that: including separation
Device (1), cooler (2), filter (3), surge tank (4) and cyclohexene extraction tower (7),
The reaction product import (1a) of the separator (1) connects feed pipe (5), for being connect with hydration reactor, separator
(1) light phase export (1b) for being connect with cyclohexanol knockout tower, the heavy out (1c) of separator (1) through cooler (2), with
The feed inlet (3a) of filter (3) connects, and feed inlet (3a), the slag-drip opening (3b) of the filter (3) are located under filter medium
Side, the liquid outlet (3c) of the filter (3) are located at the top of filter medium,
The import (4a) of the surge tank (4) is connect with the liquid outlet (3c) of the filter (3), the outlet of surge tank (4)
(4b) is fed cyclohexene extraction tower (7) by dehvery pump (6).
2. the separating and reclaiming device of the hydration catalyst of cyclohexene hydration cyclohexanol technique according to claim 1, special
Sign is: the separator (1) includes separator tank body (11), and the separator tank body (11) is in horizontally-arranged tubular construction, and
Reaction product import (1a) is arranged in one end middle part of sealing two ends, separator tank body (11), the other end of separator tank body (11)
Top light phase export (1b) is set, heavy out (1c) is arranged in the bottom of the other end, the inner cavity of the separator tank body (11)
In be equipped with liquid shield (12), coalescence mechanism (13), the L-shaped structure of the liquid shield (12), the liquid shield of L-shaped structure
(12) horizontal sides are fixed on separator tank body (11) one end, are located at the top of reaction product import (1a), the liquid of L-shaped structure
The vertical edge of body baffle (12) is corresponding with reaction product import (1a), and has interval, is formed cushion space (14), the coalescence
Mechanism (13) is located at the middle part of the inner cavity of separator tank body (11), and coalescence mechanism (13) includes the coalescence of several bendings that are serrated
The overbending direction of plate (15), each coalescing-plate (15) extends along the length of separator tank body (11), plane where each coalescing-plate (15)
Angle α between plumb line is 10-80 °, these coalescing-plates (15) are in arranged in parallel, and have spacing distance, each coalescing-plate
(15) upper end is identical as the distance between separator tank body (11) inner wall, in each coalescing-plate (15) lower end and separator tank body (11)
The distance between wall is identical, and the sawtooth height H of coalescing-plate (15) is greater than the distance between two neighboring coalescing-plate (15) h, makes phase
Clearance space between adjacent two coalescing-plates (15) forms fluid flow paths (16).
3. the separating and reclaiming device of the hydration catalyst of cyclohexene hydration cyclohexanol technique according to claim 1, special
Sign is: the filter (3) includes filter housings (31) and several filter cores (32), and the filter housings (31) are in
A horizontal-extending mounting plate (33) is arranged in the inner cavity of vertical tubular construction, and sealing two ends, filter housings (31), incited somebody to action
The inner cavity of filter shell (31) is divided into mutually independent first chamber (34), second chamber (35), and first chamber (34) is located at
The top of second chamber (35), feed inlet (3a), the slag-drip opening (3b) of the filter (3) are connected to second chamber (35), the mistake
The liquid outlet (3c) of filter (3) is connected to first chamber (34), and the filter core (32) includes filtering outer cylinder (36), recoil inner cylinder
(37), the recoil inner cylinder (37) is set in filtering outer cylinder (36) with one heart, and has clearance space, on the filtering outer cylinder (36)
Equipped with several filter openings, the aperture of each filter opening is 0.5-2 μm, and the recoil inner cylinder (37) is equipped with several recoil holes, each filter core
(32) it is uniformly arranged in second chamber (35), is fixedly connected with mounting plate (33), make to filter the nozzle of outer cylinder (36), in recoil
The nozzle of cylinder (37) is connected to first chamber (34).
4. the separating and reclaiming device of the hydration catalyst of cyclohexene hydration cyclohexanol technique according to claim 3, special
Sign is: setting recoil water inlet (38) on the filter housings (31), the recoil water inlet (38) and each filter core (32)
Recoil inner cylinder (37) parallel connection.
5. the separating and reclaiming device of the hydration catalyst of cyclohexene hydration cyclohexanol technique according to claim 3, special
Sign is: alkali liquid washing mouth (39) is arranged on the filter housings (31), the alkali liquid washing mouth (39) and each filter core (32)
Recoil inner cylinder (37) parallel connection.
6. the separating and reclaiming device of the hydration catalyst of cyclohexene hydration cyclohexanol technique according to claim 1, special
Sign is: the feed pipe (5) is equipped with water supplement port (5a).
7. using the technique of claim 1-6 any separating and reclaiming device separation and recovery hydration catalyst, which is characterized in that tool
There are following steps:
1) cyclohexene hydration reaction product enters in separator through feed pipe, and the temperature of cyclohexene hydration reaction product is 120-
130 DEG C, pressure 0.5-0.6MPa, disengaging time 10-45min；
2) light phase of the light phase export discharge of separator enters cyclohexanol knockout tower, the heavy phase warp of the heavy out discharge of separator
Cooler is cooled to lower than 100 DEG C, enters filter by the feed inlet of filter；
3) the feed inlet pressure of filter is 0.5-0.6MPa, and the liquid outlet pressure of filter is 0-0.1MPa, liquid outlet discharge
Clear liquid enter surge tank, pumped by dehvery pump to cyclohexene extraction tower, recycle cyclohexanol as raw material；
4) the slag-drip opening discharge concentrate and hydration catalyst of filter, for recycling or waste disposal.
8. technique according to claim 8, which is characterized in that water, water and cyclohexene water are added in the feed pipe of step 1)
The volume ratio for closing reaction product is 1:10-150.
9. technique according to claim 8, which is characterized in that the pore size filter of the filter medium of step 3) filter is
0.5-2μm。
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| CN201910694012.1A CN110327678B (en) | 2019-07-30 | 2019-07-30 | Separation and recovery device and process for hydration catalyst of cyclohexene hydration cyclohexanol process |
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| CN205182348U (en) * | 2015-12-04 | 2016-04-27 | 西安超滤化工有限责任公司 | Can exempt from to dismantle abluent methyl alcohol filter |
| CN106422420A (en) * | 2016-10-17 | 2017-02-22 | 青岛科技大学 | Horizontal type oil and water phase separator |
| CN108440241A (en) * | 2018-04-10 | 2018-08-24 | 成都凯特力华科技有限公司 | A kind of purification system and method for high purity cyclohexanol |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102911017A (en) * | 2012-11-16 | 2013-02-06 | 河南大学 | New method and device for preparing cyclohexanol by catalyzing direct hydration of cyclohexene with ionic liquid |
| CN103709010A (en) * | 2014-01-06 | 2014-04-09 | 河北工业大学 | Method for synthesizing cyclohexanol by reacting cyclohexene, carboxylic acid and water |
| CN204447493U (en) * | 2015-01-14 | 2015-07-08 | 东华工程科技股份有限公司 | Rinse trapezoidal methyl alcohol filter thoroughly |
| CN205182348U (en) * | 2015-12-04 | 2016-04-27 | 西安超滤化工有限责任公司 | Can exempt from to dismantle abluent methyl alcohol filter |
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