CN106278821A - A kind of remove the method and device of plurality of impurities in ethylene glycol - Google Patents
A kind of remove the method and device of plurality of impurities in ethylene glycol Download PDFInfo
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- CN106278821A CN106278821A CN201610891324.8A CN201610891324A CN106278821A CN 106278821 A CN106278821 A CN 106278821A CN 201610891324 A CN201610891324 A CN 201610891324A CN 106278821 A CN106278821 A CN 106278821A
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- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 title claims abstract description 319
- 239000012535 impurity Substances 0.000 title claims abstract description 59
- 238000000034 method Methods 0.000 title claims abstract description 29
- 239000007788 liquid Substances 0.000 claims abstract description 264
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 220
- 239000000178 monomer Substances 0.000 claims abstract description 152
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 109
- 238000009826 distribution Methods 0.000 claims abstract description 93
- 239000011949 solid catalyst Substances 0.000 claims abstract description 92
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 33
- 230000008676 import Effects 0.000 claims description 48
- 239000003054 catalyst Substances 0.000 claims description 41
- 230000008961 swelling Effects 0.000 claims description 27
- 239000000463 material Substances 0.000 claims description 26
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 17
- 239000002699 waste material Substances 0.000 claims description 16
- 238000010521 absorption reaction Methods 0.000 claims description 14
- 239000007787 solid Substances 0.000 claims description 8
- 238000006555 catalytic reaction Methods 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 7
- 239000012530 fluid Substances 0.000 claims description 7
- 239000002356 single layer Substances 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 6
- 238000007670 refining Methods 0.000 claims description 5
- 238000010618 wire wrap Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 4
- 239000000376 reactant Substances 0.000 claims description 3
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 2
- 239000004744 fabric Substances 0.000 claims 1
- 230000008901 benefit Effects 0.000 abstract description 4
- 239000002245 particle Substances 0.000 abstract description 4
- 230000008569 process Effects 0.000 abstract description 4
- 238000000746 purification Methods 0.000 abstract description 3
- 230000008859 change Effects 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 10
- 230000035699 permeability Effects 0.000 description 5
- 150000001299 aldehydes Chemical class 0.000 description 4
- 238000007599 discharging Methods 0.000 description 4
- 239000006227 byproduct Substances 0.000 description 3
- 239000003245 coal Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229920000728 polyester Polymers 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000002834 transmittance Methods 0.000 description 3
- GTACSIONMHMRPD-UHFFFAOYSA-N 2-[4-[2-(benzenesulfonamido)ethylsulfanyl]-2,6-difluorophenoxy]acetamide Chemical compound C1=C(F)C(OCC(=O)N)=C(F)C=C1SCCNS(=O)(=O)C1=CC=CC=C1 GTACSIONMHMRPD-UHFFFAOYSA-N 0.000 description 2
- 101710130081 Aspergillopepsin-1 Proteins 0.000 description 2
- 102100031007 Cytosolic non-specific dipeptidase Human genes 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- 150000002576 ketones Chemical class 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 239000003208 petroleum Substances 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 210000003437 trachea Anatomy 0.000 description 2
- ZNQVEEAIQZEUHB-UHFFFAOYSA-N 2-ethoxyethanol Chemical compound CCOCCO ZNQVEEAIQZEUHB-UHFFFAOYSA-N 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- LOMVENUNSWAXEN-UHFFFAOYSA-N Methyl oxalate Chemical compound COC(=O)C(=O)OC LOMVENUNSWAXEN-UHFFFAOYSA-N 0.000 description 1
- 150000001728 carbonyl compounds Chemical class 0.000 description 1
- 238000009903 catalytic hydrogenation reaction Methods 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 125000004185 ester group Chemical group 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 125000000468 ketone group Chemical group 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000010687 lubricating oil Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000006396 nitration reaction Methods 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000000844 transformation Methods 0.000 description 1
Classifications
-
- 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
- C07C29/88—Separation; Purification; Use of additives, e.g. for stabilisation by treatment giving rise to a chemical modification of at least one compound
- C07C29/92—Separation; Purification; Use of additives, e.g. for stabilisation by treatment giving rise to a chemical modification of at least one compound by a consecutive conversion and reconstruction
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
Abstract
The invention discloses and a kind of remove the method and device of plurality of impurities in ethylene glycol, this device includes two the first finishing reactors in parallel, the second finishing reactor being made up of 2 sections of reactor monomers, filter A, filter B, filter C, ethylene glycol feed pipe, nitrogen tube, backwash tube, backwash liquor outlet.The invention has the advantages that: flow process is simple, and removing impurities is effective, high financial profit；Method of operation flexible operation, it is achieved not parking change agent；Second finishing reactor has multistage set, compact conformation, saves space and investment, it is simple to the advantage operating and managing；It is provided with liquid distribution trough in reactor, when treating purification ethylene glycol, enters reactor and pass through liquid distribution trough, both can realize being uniformly distributed of feed stream, again can be to intercept solid catalyst particle during backwash, it is to avoid run off；It is provided with multiple filter cap on filter cap distribution grid in reactor, both can guarantee that stability of flow, solid catalyst particle can be intercepted again, it is to avoid loss.
Description
Technical field
The present invention relates to a kind of remove the method and device of plurality of impurities in ethylene glycol, UV transmittance can be improved, main
Purifying ethylene glycol technical field to be used for, belongs to technical field of petrochemical industry.
Background technology
Ethylene glycol (EG) is a kind of important Organic Chemicals, mainly for the production of polyester, anti-icing fluid, binding agent, oil
White spirit, Everlube, surfactant and PEPA etc..Wherein polyester is the major consumers neck of China's ethylene glycol
Territory, its consumption figure accounts for the 94.0% of gross domestic consumption amount, and the most about 6.0% for antifreezing agent, binding agent, paint solvent, resistance to
Cold lubricating oil, surfactant and PEPA etc..
Although the purity of the ethylene glycol product of China's oil route and Coal Chemical Industry Route is attained by more than 99.9%, but
In product the most in various degree also exist with content beyond expression of words, in 220nm～350nm wave-length coverage, have the organic of absorption
Miscellaneous.The existence of these impurity makes the ultraviolet permeability of 220nm～350nm wave-length coverage decline, and affects the quality of polyester, such as fiber
Gloss, colourity, coloring and hardness etc..Therefore the quality of ethylene glycol depends primarily on ISOUV value index.
Research shows, affects some by-products that the impurity of quality of ethylene glycol product is mainly in production process.
As the impurity in petroleum path ethylene glycol product is mainly some by-products during oxidation of ethylene, including
The organic compound such as aldehyde, ketone.And the impurity in the ethylene glycol product of Coal Chemical Industry Route be mainly dimethyl oxalate. catalytic hydrogenation and
Some trace by-products in high temperature aerobic subtractive process, including: esters and substituted cyclic diketones and grip aldehydes altogether on a small quantity
Material.And these contain carbonyl impurities and have bigger absorption in 220nm～350nm wave-length coverage, therefore reduce these carbonyls
The content of compound impurities, raising ethylene glycol product is at wavelength 220nm～the ultraviolet permeability of 350nm scope, to improving second two
The quality of alcohol is of great importance.
The present invention removes the method that in ethylene glycol, plurality of impurities improves UV transmittance, by advanced purifying ethylene glycol work
Skill combines with second finishing reactor with special internal structure, and by equipped with multistage and several functions solid catalysis
Agent with the use of, can effectively remove the various impurity in ethylene glycol, improve ethylene glycol product at wavelength 220nm～350nm model
The ultraviolet permeability enclosed, reaches the purpose of purifying ethylene glycol.
Summary of the invention
The technical problem to be solved is for the deficiencies in the prior art, and provides a kind of removing second two
The device of plurality of impurities in alcohol, this device is by refined with second with special internal structure for advanced Purification Catalysts of Monoethylene Glycol anti-
Answer device 202 to combine, through several functions solid catalyst with the use of, reach the purpose that ethylene glycol is exquisite.
The technical problem to be solved is for the deficiencies in the prior art, and provides a kind of removing second two
The method of plurality of impurities in alcohol, the method can remove the aldehyde type impurities of trace in petroleum path ethylene glycol product, can remove again
Trace ester group in coal-ethylene glycol product and keto compounds impurity, thus significantly improve the UV transmittance of ethylene glycol.
To achieve these goals, the present invention adopts the following technical scheme that
A kind of remove the method for plurality of impurities in ethylene glycol, comprise the following steps:
(1) catalyst is swelling: utilize backwash liquor ethylene glycol to enter the first solid catalyst and the second solid catalyst respectively
Row is swelling；
The first described solid catalyst is KC 108A, any in KC 108B, KC 108C, KC 108D type catalyst
One or both mixture mixed with arbitrary proportion；(four kinds of catalyst are that Kai Rui environmental protection Science and Technology Co., Ltd. exists
The catalyst of invention in CN102911013B i.e. (2012104484052))；
The second described solid catalyst is KC 108A, any in KC 108B, KC 108C, KC 108D type catalyst
Two or three mixture mixed with arbitrary proportion；(four kinds of catalyst are that Kai Rui environmental protection Science and Technology Co., Ltd. exists
The catalyst of invention in CN102911013B i.e. (2012104484052))；
(2) removing impurities for the first time: the ethylene glycol containing impurity is passed in the first solid catalyst, is 30～60 in temperature
DEG C, pressure be 0.1～1MPa, material air speed be 3～12h-Under conditions of imurity-removal, after catalyst absorption impurity, ethylene glycol
Material is passed in the second solid catalyst；
(3) removing impurities for the second time: the ethylene glycol material that step (2) obtains is passed in the second solid catalyst, in temperature is
30～60 DEG C, pressure be 0.1～1MPa, material air speed be 3～12h-Under conditions of imurity-removal, after catalyst absorption impurity,
Purified ethylene glycol is gathered.
In technique scheme, method include in detail below step (opening of all parts before use be defaulted as close
Closed state):
(1) catalyst is swelling: after loading the first solid catalyst respectively in the first finishing reactor A, B, opens each
Nitrogen inlet, nitrogen tube, backwash liquor import, backwash tube, backwash liquor and nitrogen enter in the first finishing reactor A, B, nitrogen
Gas makes backwash liquor be fully contacted with catalyst, is allowed to swelling, after difference swelling 30～300min, closedown backwash liquor import respectively,
Backwash tube, nitrogen inlet, nitrogen tube, open opening, and waste liquid is drained in filter B by backwash tube outlet；
After loading the second solid catalyst respectively in the second finishing reactor A, B, open backwash liquor entrance, backwash tube,
Nitrogen inlet, nitrogen tube, backwash liquor and nitrogen enter in the second finishing reactor monomer B, and nitrogen makes backwash liquor urge with solid
Agent is fully contacted, and is allowed to swelling, swelling 30～300min；Under valve a, valve b are closed mode, open valve c, nitrogen
Entering in the second finishing reactor monomer A through second segment liquid inlet, first liquid outlet successively with backwash liquor, nitrogen makes instead
Washing liquid is fully contacted with solid catalyst, after being allowed to swelling 30～300min, closes backwash tube, nitrogen inlet, opens first paragraph
Liquid inlet and valve d, the waste liquid in the second finishing reactor monomer A was discharged to through backwash liquor outlet from one section of liquid inlet
In filter B, the waste liquid in the second finishing reactor monomer B is discharged to filter B through valve d from backwash liquor entrance；Finally close
Backwash liquor entrance；Waste liquid obtains purified ethylene glycol in catalyst converter B after filtering, and is saved in ethylene glycol holding vessel；
In two the first finishing reactors, the kind of the first solid catalyst of filling is identical or different；
In second finishing reactor A, the solid catalyst of filling is solid catalyst A, loads in the second finishing reactor B
Solid catalyst be solid catalyst B, solid catalyst A, B are as the second solid catalyst, and kind is identical or different；
(2) removing impurities for the first time: the ethylene glycol containing plurality of impurities is had respectively entered first by ethylene glycol feed pipe through import
In finishing reactor A, B, obtain material ethylene glycol respectively through after the first solid catalyst absorption impurity；Open discharging respectively
Mouthful, the ethylene glycol material obtained is in outlet A enters into filter A, and filter A intercepts and reclaims the catalyst spilt；
Described the first finishing reactor A, B reaction condition are identical: temperature is 30～60 DEG C, pressure is 0.1～1MPa, thing
Material air speed is 3～12h-；
(3) removing impurities for the second time: open first paragraph liquid inlet, second segment liquid inlet, through the filter described in step (2)
Ethylene glycol material after A filters is directed respectively into the second finishing reactor monomer A and B through outlet B；Respectively through solid catalysis
Ethylene glycol is obtained after agent A, B absorption impurity；Open first paragraph liquid outlet, second segment liquid outlet, the ethylene glycol obtained respectively
Entering in filter C through first liquid outlet, second liquid outlet respectively, filter C intercepts and reclaims the catalysis spilt
Qualified ethylene glycol is obtained, in outlet C imports to the ethylene glycol holding vessel of outside after agent；
Second finishing reactor monomer A, B, operating condition is identical: temperature is 30～60 DEG C, pressure is 0.1～1MPa, thing
Material air speed is 3～12h-。
The present invention also provides for the device of plurality of impurities in the removing ethylene glycol used in a kind of said method, including the first essence
Reactor A processed, the first finishing reactor B, the second finishing reactor, filter A, filter B, filter C, ethylene glycol feed
Pipe, nitrogen tube, backwash tube, backwash liquor outlet:
Described ethanol feed pipe, import is connected with the device of the outside ethylene glycol containing plurality of impurities provided, outlet point
For two-way, a road is connected with the import of backwash tube, another road respectively with the first finishing reactor A, the first finishing reactor B
Liquid inlet is connected；First finishing reactor A, the liquid outlet of the first finishing reactor B pass through outlet A and filtration respectively
The import of device A is connected；The outlet of filter A is connected by the liquid inlet of outlet B and the second finishing reactor；Second
The liquid outlet of finishing reactor is connected with the import of filter C, and the outlet of filter C is by outlet C and outside second
Glycol holding vessel is connected；
Described backwash tube, import is connected with ethanol feed pipe or the outside device providing backwash liquor ethylene glycol, outlet
It is connected with the first finishing reactor A, the first finishing reactor B, the backwash liquor entrance of the second finishing reactor respectively, thus will
Backwash liquor is directed in each reactor；First finishing reactor A, the first finishing reactor B, the liquid of the second finishing reactor enter
Mouth also import with described backwash liquor outlet is connected, and backwash liquor derives from the liquid inlet of each reactor to backwash liquor
In mouth pipe；The outlet of backwash liquor outlet is connected with the import of filter B, and the outlet of filter B is by outlet D and outside
Ethylene glycol holding vessel be connected；
Described nitrogen tube, import and outside provide the device of nitrogen to be connected, export respectively with the first finishing reactor A,
First finishing reactor B, the nitrogen inlet of the second finishing reactor are connected.
In technique scheme, described the first finishing reactor A, the first finishing reactor B structure are identical and use also
The connected mode of connection links together: its top all offers liquid inlet, and liquid inlet is all by pipeline and described second two
The outlet of alcohol feed pipe is connected；All offer nitrogen inlet, backwash liquor entrance and liquid outlet bottom it, nitrogen inlet all with
The outlet of described nitrogen tube (20) is connected, and all outlets with described backwash tube of backwash liquor entrance are connected, liquid outlet
All it is connected with outlet A；Described backwash liquor entrance is the most all connected by the import of pipeline with backwash liquor outlet.
In technique scheme, the second described finishing reactor, top is provided with first paragraph liquid inlet, and middle part is provided with
One section of liquid outlet, second segment liquid inlet, bottom is provided with nitrogen inlet, second segment liquid outlet, backwash liquor entrance, wherein:
First paragraph liquid inlet, second segment liquid inlet are all connected with described outlet B；First paragraph liquid outlet connects the first liquid
Body outlet, second segment liquid outlet connect a second liquid outlet, and first liquid outlet, second liquid outlet are equal
Import with described filter C is connected；Nitrogen inlet is connected with the outlet of described nitrogen tube, backwash liquor entrance and institute
The outlet of the backwash tube stated is connected；Described first paragraph liquid inlet is entered also by pipeline and described backwash liquor outlet
Mouth is connected；
Described outlet B, the branch road being connected with second segment liquid inlet is provided with valve a；Described first liquid
Valve b is installed on outlet；Connect between described first liquid outlet, second segment liquid inlet and have backwash liquor passage I, instead
Valve c is installed on washing liquid channel I；Described backwash liquor entrance is also by the import III phase of backwash liquor passage II with filter B
Even, backwash liquor passage II is provided with valve d.
In technique scheme, the second described finishing reactor is made up of 2 sections of reactor monomers, i.e. refined anti-by second
Answering device monomer A, the second finishing reactor monomer B to constitute according to order up and down, structure is as follows:
The second described finishing reactor monomer A top offers first paragraph liquid inlet, bottom offers first paragraph liquid
Body exports, and body wall top offers first paragraph solid catalyst loading port and is provided with first paragraph visor, and body wall bottom offers
First paragraph solid catalyst unloads agent mouth；Monomer A is internally installed first paragraph liquid distribution trough, and first paragraph liquid distribution trough is positioned at
Bottom, first paragraph liquid inlet, the top of first paragraph visor；Monomer A is internally installed first paragraph filter cap distribution grid, and first paragraph
Filter cap distribution grid is positioned at first paragraph solid catalyst and unloads agent mouth bottom, first paragraph liquid outlet top；Described first paragraph visor,
It is filled with solid catalyst A in monomer between first paragraph filter cap distribution grid；
The second described finishing reactor monomer B, the body wall topmost of monomer offers second segment liquid inlet, second segment
Liquid inlet connects has feed tube, the leakage fluid dram of feed tube end to be positioned at inside monomer B；The bottom of monomer B offers nitrogen and enters
Mouth, second segment liquid outlet, backwash liquor entrance；The body wall top of monomer B offers second segment solid catalyst loading port and peace
Equipped with second segment visor, body wall bottom offers second segment solid catalyst and unloads agent mouth；Monomer B is internally installed second segment liquid
Distributor, and second segment liquid distribution trough is positioned at leakage fluid dram bottom, the top of second segment visor；Monomer B is internally installed second
Section filter cap distribution grid, and second segment filter cap distribution grid is positioned at second segment solid catalyst and unloads agent mouth bottom, second segment liquid outlet
Top；It is filled with solid catalyst B in monomer between described second segment visor, second segment filter cap distribution grid；
Described first paragraph liquid distribution trough, second segment liquid distribution trough structure are identical, are calandria or annular tube type liquid
Body distributor, the filter tube of liquid distribution trough is wrapping wire filter tube or the filter tube being cased with filter bag；
Described first paragraph filter cap distribution grid, second segment filter cap distributing plate structure are identical, equipped with some on filter cap distribution grid
Filter cap；Described filter cap is wire wrap filter cap or filter bag type filter cap；Described filter cap uses with the connected mode of filter cap distribution grid
Threaded or locknut connects.
In technique scheme, two monomers of the main body constituting the second finishing reactor can be split as two independent lists
Layer bed reactor monomer, is i.e. split as the second independent finishing reactor monomer A and the second independent finishing reactor monomer B:
The bottom of the second finishing reactor monomer A uses with the second finishing reactor monomer B after offering nitrogen inlet and backwash liquor entrance
After connected mode in parallel or in series connects, then with backwash liquor outlet, outlet B, nitrogen tube, backwash tube, filter C phase
Connect:
When second finishing reactor monomer A, the second finishing reactor monomer B connect in a series arrangement: outlet B and second
The first paragraph liquid inlet of finishing reactor monomer A is connected, the first paragraph liquid outlet of the second finishing reactor monomer A and
The second segment liquid inlet of two finishing reactors B is connected, the second segment liquid outlet of the second finishing reactor B and filter C
It is connected；Nitrogen inlet that first finishing reactor monomer A newly opens and the nitrogen inlet of the second finishing reactor monomer B are all and nitrogen
Trachea is connected；Backwash liquor entrance and the backwash liquor entrance of the second finishing reactor monomer B that first finishing reactor A is newly opened are equal
It is connected with backwash tube；First paragraph liquid inlet, second segment liquid inlet are the most all connected with backwash liquor outlet；
When second finishing reactor monomer A, the second finishing reactor monomer B connect with parallel way: the second refining reaction
The first paragraph liquid inlet of device monomer A, the second segment liquid inlet of the second finishing reactor B are all connected with outlet B, the second essence
The first paragraph liquid outlet of reactor monomer A processed, second segment liquid outlet are all connected with filter C；First finishing reactor list
Nitrogen inlet and the nitrogen inlet of the second finishing reactor monomer B that body A newly opens all are connected with nitrogen tube, the first refining reaction
Backwash liquor entrance and the backwash liquor entrance of the second finishing reactor monomer B that device A newly opens all are connected with backwash tube；First paragraph liquid
Body entrance, second segment liquid inlet are the most all connected with backwash liquor outlet.
In technique scheme, described the first finishing reactor A, the first finishing reactor B, structure is refined with second anti-
Answer device monomer A, the second independent finishing reactor monomer B identical；Two monomers i.e. constituting the second finishing reactor main body can
After being split as two independent monolayer bed reactor monomers, make as the first finishing reactor A and the first finishing reactor B
With, cut-away view is referring to the second finishing reactor: top offers opening, and bottom offers nitrogen inlet, backwash liquor import
And discharging opening；Body wall top offers solid catalyst loading port, body wall top is mounted on visor；Body wall bottom offers solid
Body catalyst unloads agent mouth；Internally installed have liquid distribution trough, and liquid distribution trough is positioned at the top of lower opening portion, visor；Monomer
Internally installed have filter cap distribution grid, and filter cap distribution grid is positioned at solid catalyst and unloads agent mouth bottom, discharging opening top；Described regards
It is filled with solid catalyst in monomer between mirror, filter cap distribution grid.
In technique scheme, the second finishing reactor can also be made up of multistage reactor monomer, i.e. by N section reactor
Monomer constitute (2 ＜ N≤10, preferably 2 ＜ N≤8, further preferred 2 ＜ N≤5), in every section of monomer respectively fill have identical or
The solid catalyst of difference in functionality, solid catalyst kind is n, 1 ＜ n≤10, preferably 2≤N≤5；
The top of every section of described reactor monomer all offers liquid inlet, bottom and all offers liquid outlet；Body wall
Top all offers solid catalyst loading port, body wall top is mounted on visor；Body wall bottom all offers solid catalyst
Unload agent mouth；It is mounted on liquid distribution trough inside monomer, and liquid distribution trough is positioned at the top of bottom, liquid inlet, visor；Single
Internal portion is provided with filter cap distribution grid, and filter cap distribution grid is positioned at solid catalyst and unloads agent mouth bottom, liquid outlet top；Described
Visor, be filled with solid catalyst in monomer between filter cap distribution grid；Final stage monomer, also opens in addition to liquid outlet
It is provided with nitrogen inlet and backwash liquor entrance；The liquid inlet of every section of monomer is all connected with outlet B, and liquid outlet is all and filter
C is connected；Nitrogen inlet is connected with nitrogen tube, reactant liquor entrance is connected with backwash tube；The liquid inlet of first paragraph monomer also with instead
Washing liquid outlet is connected；
Described liquid distribution trough, for calandria or annular tube type liquid distribution trough, the filter tube of liquid distribution trough is wrapping wire
Filter tube or be cased with the filter tube of filter bag；Described filter cap distribution grid, equipped with some filter caps on filter cap distribution grid, filter cap is wrapping wire
Formula filter cap or filter bag type filter cap, filter cap is threaded with the employing of the connected mode of filter cap distribution grid or locknut is connected.
In technique scheme, described multistage reactor monomer can also split into N number of independent monolayer bed reactor
((2 ＜ N≤10, preferably 2 ＜ N≤8, further preferred 2 ＜ N≤5), except final stage monomer, the bottom of other monomers for monomer
Use connected mode to be in parallel or in series connected with final stage monomer after offering nitrogen inlet and backwash liquor entrance, connect or
Person is in parallel identical with the catenation principle splitting into two monomers and connected mode.
The advantage of technical solution of the present invention is: 1, flow process is simple, and the impurity removal in ethylene glycol is effective, economic benefit
High；2, two the first finishing reactors are in parallel, and the second finishing reactor upper-lower section can realize series connection and two kinds of operations in parallel
Mode, flexible operation, it is achieved not parking change agent；3, the second finishing reactor has: 1) multistage set, compact conformation, saves sky
Between and investment, it is simple to operate and manage；2) in reactor cylinder body, it is provided with liquid distribution trough, when treating purification ethylene glycol,
Enter reactor and pass through liquid distribution trough, both can realize being uniformly distributed of feed stream, and can urge to intercept solid during backwash again
Catalyst particles, it is to avoid run off；3) it is provided with multiple filter cap on the filter cap distribution grid in reactor cylinder body, both can guarantee that flow was steady
Fixed, solid catalyst particle can be intercepted again, it is to avoid loss.
Accompanying drawing explanation
The overall structure schematic diagram of Fig. 1: apparatus of the present invention；
Fig. 2: knot when the second finishing reactor is split as two independent monolayer bed reactor monomers in apparatus of the present invention
Structure schematic diagram；
Fig. 3: structure schematic diagram when the second finishing reactor is made up of 2 sections of reactor monomers in apparatus of the present invention；
Wherein: 1, first paragraph liquid inlet 2, first paragraph solid catalyst loading port 3, first paragraph visor 4, first paragraph
Solid catalyst unload agent mouth 5, first paragraph liquid outlet 6, second segment solid catalyst loading port 7, second segment visor 8,
Agent mouth 10, nitrogen inlet 11, second segment liquid outlet 12, backwash liquor are unloaded in two-stage nitration liquid inlet 9, second segment solid catalyst
Entrance 13, first paragraph liquid distribution trough 14, first paragraph filter cap distribution grid 15, second segment liquid distribution trough 16, second segment are filtered
Cap distribution grid 17, solid catalyst A 18, solid catalyst B 19, ethylene glycol feed pipe 20, nitrogen tube 21, first refine
Reactor A the 22, first finishing reactor B the 23, second finishing reactor the 231, second finishing reactor monomer A 232, second
Finishing reactor monomer B 24, outlet A 25, filter A26, outlet B 27, first liquid outlet 28, second liquid
Outlet 29, filter C 30, outlet C 31, filter B 32, outlet D 33, backwash tube 34, backwash liquor outlet
35, valve a 36, valve b 37, valve c 38, valve d.
Detailed description of the invention
Hereinafter the detailed description of the invention of technical solution of the present invention is described in detail, but the present invention is not limited in following description
Hold:
The present invention provides a kind of and removes the method for plurality of impurities in ethylene glycol, comprises the following steps:
(1) catalyst is swelling: after loading the first solid catalyst respectively in the first finishing reactor A, B, opens each
Nitrogen inlet, nitrogen tube 20, backwash liquor entrance, backwash tube 33, backwash liquor and nitrogen enter into the first finishing reactor A, B
In, nitrogen makes backwash liquor be fully contacted with catalyst, is allowed to swelling, after difference swelling 30～300min, closes backwash liquor respectively
Entrance, backwash tube, nitrogen inlet, nitrogen tube, open liquid inlet, and waste liquid drains into filter B 31 by backwash tube outlet 34
In；
After loading the second solid catalyst respectively in the second finishing reactor A, B, open backwash liquor entrance 12, backwash tube
33, nitrogen inlet 10, nitrogen tube 20, backwash liquor and nitrogen enter in the second finishing reactor monomer B, nitrogen make backwash liquor with
Catalyst is fully contacted, and is allowed to swelling, swelling 30～300min；Under valve a35, valve b36 are closed mode, open valve
C37, nitrogen and backwash liquor enter into the second finishing reactor monomer A through second segment liquid inlet 8, first liquid outlet 5 successively
In, nitrogen makes backwash liquor be fully contacted with catalyst, after being allowed to swelling 30～300min, closes backwash tube 33, nitrogen inlet 10,
Open first paragraph liquid inlet 1 and valve d38, the waste liquid in the second finishing reactor monomer A from one section of liquid inlet 1 through backwash
Liquid outlet 34 is discharged in filter B 31, and the waste liquid in the second finishing reactor monomer B is arranged through valve d from backwash liquor entrance 12
In filter B 31；Finally close backwash liquor entrance 12；Described waste liquid obtains pure in catalyst converter B after filtering
Ethylene glycol, is saved in ethylene glycol holding vessel；
(2) removing impurities for the first time: the ethylene glycol containing plurality of impurities is had respectively entered first by ethylene glycol feed pipe 19 and refines
In reactor A, B, obtain material ethylene glycol respectively through after the first solid catalyst absorption impurity；Open liquid outlet respectively,
The ethylene glycol material obtained is in outlet A24 enters into filter A25, and filter A intercepts and reclaims the catalyst spilt；
(3) removing impurities for the second time: open first paragraph liquid inlet 1, second segment liquid inlet 8, through the filtration described in step (2)
Ethylene glycol material after device A25 filters is directed respectively into the second finishing reactor monomer A and B through outlet B26；Respectively through
Ethylene glycol is obtained after two solid catalyst absorption impurities；Open first paragraph liquid outlet 5, second segment liquid outlet 11 respectively,
To ethylene glycol enter in filter C29 through first liquid outlet 27, second liquid outlet 28 respectively, filter C blocks
Cut and obtain qualified ethylene glycol after reclaiming the catalyst spilt, in outlet C30 imports to the ethylene glycol holding vessel of outside.
The present invention also provides for a kind of removing the device of plurality of impurities in ethylene glycol, including the first finishing reactor A21, first
Finishing reactor B the 22, second finishing reactor 23, filter A25, filter B 31, filter C 29, ethylene glycol feed pipe
19, nitrogen tube 20, backwash tube 33, backwash liquor outlet 34, as shown in Figure 1:
Described ethanol feed pipe 19, import is connected with the device of the outside ethylene glycol containing plurality of impurities provided, outlet
Being divided into two-way, a road is connected with the import of backwash tube 33, another road respectively with the first finishing reactor A, the first refining reaction
The liquid inlet of device B is connected；First finishing reactor A, the liquid outlet of the first finishing reactor B pass through outlet respectively
A24 is connected with the import of filter A25；The outlet of filter A is entered by the liquid of outlet B26 and the second finishing reactor
Mouth is connected；The liquid outlet of the second finishing reactor is connected with the import of filter C29, and the outlet of filter C is by going out
Mouth pipe C30 is connected with outside ethylene glycol holding vessel；
Described backwash tube 33, import is connected with ethanol feed pipe or the outside device providing backwash liquor ethylene glycol, goes out
Mouth is connected with the first finishing reactor A, the first finishing reactor B, the backwash liquor entrance of the second finishing reactor respectively, thus
Backwash liquor is directed in each reactor；First finishing reactor A, the first finishing reactor B, the liquid of the second finishing reactor
Entrance also import with described backwash liquor outlet 34 is connected, and backwash liquor is derived to backwash from the liquid inlet of each reactor
In liquid outlet；The outlet of backwash liquor outlet is connected with the import of filter B 31, and outlet is passed through in the outlet of filter B
D32 is connected with outside ethylene glycol holding vessel；
Described nitrogen tube 20, import and outside provide the device of nitrogen to be connected, export respectively with the first finishing reactor
A, the first finishing reactor B, the nitrogen inlet of the second finishing reactor are connected；
Described the first finishing reactor A, identical and employing parallel connection the connected mode of the first finishing reactor B structure connect
It is connected together: its top all offers liquid inlet, liquid inlet all going out by pipeline and described ethylene glycol feed pipe 19
Mouth is connected；All offer nitrogen inlet, backwash liquor entrance and liquid outlet bottom it, nitrogen inlet all with described nitrogen tube
The outlet of 20 is connected, and all outlets with described backwash tube 33 of backwash liquor entrance are connected, liquid outlet all with outlet A24
It is connected；Described backwash liquor entrance is the most all connected by the import of pipeline with backwash liquor outlet 34；
The second described finishing reactor, top is provided with first paragraph liquid inlet 1, middle part be provided with first paragraph liquid outlet 5,
Second segment liquid inlet 8, bottom is provided with nitrogen inlet 10, second segment liquid outlet 11, backwash liquor entrance 12, wherein: first paragraph
Liquid inlet 1, second segment liquid inlet 8 are all connected with described outlet B26；First paragraph liquid outlet 5 connects the first liquid
Body outlet 27, second segment liquid outlet 11 connect second liquid outlet 28, and first liquid outlet, second liquid go out
The import of mouth filter C29 described in Guan Junyu is connected；Nitrogen inlet 10 is connected, instead with the outlet of described nitrogen tube 20
Wash liquor inlet 12 is connected with the outlet of described backwash tube 33；Described first paragraph liquid inlet 1 also by pipeline with described
The import of backwash liquor outlet 34 be connected；
Described outlet B, the branch road being connected with second segment liquid inlet is provided with valve a 35；First liquid exports
Valve b 36 is installed on pipe；Connecting between first liquid outlet, second segment liquid inlet and have backwash liquor passage I, backwash liquor leads to
Valve c 37 is installed on road I；Backwash liquor entrance is connected with the import III of filter B also by backwash liquor passage II, backwash liquor
Valve d 38 is installed on passage II.
The second finishing reactor in the present invention is made up of 2 sections of reactor monomers, i.e. by the second finishing reactor monomer
A231, the second finishing reactor monomer B 232 are constituted, structure chart as shown in Figure 3:
Second finishing reactor monomer A top offers first paragraph liquid inlet, bottom offers first paragraph liquid outlet,
Body wall top offers first paragraph solid catalyst loading port 2, and body wall top is provided with first paragraph visor 3, and body wall bottom is offered
First paragraph solid catalyst is had to unload agent mouth 4；Monomer is internally installed first paragraph liquid distribution trough 13, and first paragraph liquid distribution trough
It is positioned at bottom, first paragraph liquid inlet, the top of first paragraph visor；Monomer is internally installed first paragraph filter cap distribution grid 14, and
One section of filter cap distribution grid is positioned at first paragraph solid catalyst and unloads agent mouth bottom, first paragraph liquid outlet top；Described first paragraph
It is filled with solid catalyst A17 in monomer between visor, first paragraph filter cap distribution grid；
The second described finishing reactor monomer B, the body wall topmost of monomer offers second segment liquid inlet, second segment
Liquid inlet connects has feed tube, the leakage fluid dram of feed tube end to be positioned at inside monomer；The bottom of monomer offer nitrogen inlet,
Second segment liquid outlet, backwash liquor entrance；The body wall top of monomer offers second segment solid catalyst loading port 6, on body wall
Portion is provided with second segment visor 7, and body wall bottom offers second segment solid catalyst and unloads agent mouth 9；Monomer is internally installed second
Section liquid distribution trough 15, and second segment liquid distribution trough is positioned at leakage fluid dram bottom, the top of second segment visor；Monomer is internally installed
There is second segment filter cap distribution grid 16, and second segment filter cap distribution grid is positioned at second segment solid catalyst and unloads agent mouth bottom, second segment
Liquid outlet top；It is filled with solid catalyst B in monomer between described second segment visor, second segment filter cap distribution grid
18；
Described first paragraph liquid distribution trough, second segment liquid distribution trough structure are identical, are calandria or annular tube type liquid
Body distributor, the filter tube of liquid distribution trough is wrapping wire filter tube or the filter tube being cased with filter bag；
Described first paragraph filter cap distribution grid, second segment filter cap distributing plate structure are identical, equipped with some on filter cap distribution grid
Filter cap；Described filter cap is wire wrap filter cap or filter bag type filter cap；Described filter cap uses with the connected mode of filter cap distribution grid
Threaded or locknut connects.
Two monomers of the main body of composition the second finishing reactor in the present invention can be split as two independent monolayer beds
Reactor monomer, is i.e. split as the second independent finishing reactor monomer A and the second independent finishing reactor monomer B: the second
The bottom of finishing reactor monomer A uses in parallel with the second finishing reactor monomer B after offering nitrogen inlet and backwash liquor entrance
Or the connected mode of series connection connects, as shown in Figure 2.
The first finishing reactor A in the present invention, the structure of the first finishing reactor B and the second finishing reactor monomer A,
The structure of the second finishing reactor monomer B is identical, referring to Fig. 3.
In the present invention, the second finishing reactor can also be made up of N section reactor monomer, 2 ＜ N≤10；Divide in every section of monomer
Tian Chong not have the solid catalyst of identical or different function, solid catalyst kind is n, 1 ＜ n≤10.Every section described anti-
The top answering device monomer all offers liquid inlet, bottom and all offers liquid outlet；Body wall top all offers solid catalysis
Agent loading port, body wall top are mounted on visor；Body wall bottom all offers solid catalyst and unloads agent mouth；It is respectively mounted inside monomer
There is liquid distribution trough, and liquid distribution trough is positioned at the top of bottom, liquid inlet, visor；Monomer is internally installed has filter cap to be distributed
Plate, and filter cap distribution grid is positioned at solid catalyst and unloads agent mouth bottom, liquid outlet top；Described visor, filter cap distribution grid it
Between monomer in be filled with solid catalyst；Final stage monomer, is further opened with nitrogen inlet and backwash in addition to liquid outlet
Liquid entrance；The liquid inlet of every section of monomer is all connected with outlet B, and liquid outlet is all connected with filter C；Nitrogen inlet and nitrogen
Trachea is connected, reactant liquor entrance is connected with backwash tube；The liquid inlet of first paragraph monomer is also connected with backwash liquor outlet；Described
Liquid distribution trough, for calandria or annular tube type liquid distribution trough, the filter tube of liquid distribution trough is wrapping wire filter tube or is cased with
The filter tube of filter bag；Described filter cap distribution grid, equipped with some filter caps on filter cap distribution grid, filter cap is wire wrap filter cap or filter bag
Formula filter cap, filter cap is threaded with the employing of the connected mode of filter cap distribution grid or locknut is connected.Constitute the second finishing reactor 23
N number of monomer of main body also can be split as N number of independent monolayer bed reactor monomer, 2 ＜ N≤10；Except final stage monomer, its
The bottom of his monomer uses connection side in parallel or in series with final stage monomer after offering nitrogen inlet and backwash liquor entrance
Formula connects.
Below in conjunction with specific embodiment, the inventive method is further described:
Embodiment 1:
A kind of remove the method for plurality of impurities in ethylene glycol, comprise the following steps:
(1) catalyst is swelling: load the first solid catalyst (being KC108B) in the first finishing reactor A, B respectively
After, open respective nitrogen inlet, nitrogen tube, backwash liquor import, backwash tube, backwash liquor and nitrogen enter into the first refining reaction
In device A, B, nitrogen makes backwash liquor be fully contacted with catalyst, is allowed to swelling, after difference swelling 160～170min, closes respectively
Backwash liquor import, backwash tube, nitrogen inlet, nitrogen tube, open opening, and waste liquid is drained in filter B by backwash tube outlet；
The second solid catalyst i.e. solid catalyst A, B (solid catalyst A, B phase is loaded in the second finishing reactor
With, be the mixture that KC 108C, KC108D type catalyst mixes with the mass ratio of 4:1) after, open backwash liquor entrance,
Backwash tube, nitrogen inlet, nitrogen tube, backwash liquor and nitrogen enter in the second finishing reactor monomer B, nitrogen make backwash liquor with
Solid catalyst B is fully contacted, and is allowed to swelling, swelling 160～170min；Under valve a, valve b are closed mode, open valve
Door c, nitrogen and backwash liquor enter in the second finishing reactor monomer A through second segment liquid inlet, first liquid outlet successively,
Nitrogen makes backwash liquor be fully contacted with solid catalyst A, after being allowed to swelling 160～170min, closes backwash tube, nitrogen inlet,
Opening first paragraph liquid inlet and valve d, the waste liquid in the second finishing reactor monomer A goes out through backwash liquor from one section of liquid inlet
Mouthful bank of tubes is in filter B, and the waste liquid in the second finishing reactor monomer B is discharged to filter B from backwash liquor entrance through valve d
In；Finally close backwash liquor entrance；
Described waste liquid obtains pure ethylene glycol in catalyst converter B after filtering, and is saved in ethylene glycol holding vessel；
(2) removing impurities for the first time: the ethylene glycol containing plurality of impurities is had respectively entered first by ethylene glycol feed pipe through import
In finishing reactor A, B, obtain material ethylene glycol respectively through after the first solid catalyst absorption impurity；Open discharging respectively
Mouthful, the ethylene glycol material obtained is in outlet A enters into filter A, and filter A intercepts and reclaims the catalyst spilt；
Described the first finishing reactor A, B reaction condition are identical: temperature is 40～50 DEG C, pressure is 0.5～0.6MPa,
Material air speed is 7～8h-；
(3) removing impurities for the second time: open first paragraph liquid inlet, second segment liquid inlet, through the filter described in step (2)
Ethylene glycol material after A filters is directed respectively into the second finishing reactor monomer A and B through outlet B；Respectively through solid catalysis
Ethylene glycol is obtained after agent A, B absorption impurity；Open first paragraph liquid outlet, second segment liquid outlet, the ethylene glycol obtained respectively
Entering in filter C through first liquid outlet, second liquid outlet respectively, filter C intercepts and reclaims the catalysis spilt
Qualified ethylene glycol is obtained, in outlet C imports to the ethylene glycol holding vessel of outside after agent；
Second finishing reactor monomer A, B, operating condition is identical: temperature is 40～50 DEG C, pressure is 0.5～0.6MPa,
Material air speed is 7～8h-。
Production result shows: this Technology and equipment can be greatly reduced the esters in coal ethyl glycol, aldehyde material,
The carbonyl compounds such as ketone and the content of other impurity, can be effectively improved ethylene glycol product in wavelength 220nm～350nm scope
Ultraviolet permeability, the ultraviolet permeability of the ethylene glycol after process is at 220nm > 80%, 275nm > 94%, 350nm > 99%.
Examples detailed above simply for technology design and the technical characterstic of the present invention are described, can not limit the present invention's with this
Protection domain.All equivalent transformations done according to the essence of the present invention or modification, all should contain in protection scope of the present invention
Within.
Claims (10)
1. one kind removes the method for plurality of impurities in ethylene glycol, it is characterised in that comprise the following steps:
(1) catalyst is swelling: utilize backwash liquor ethylene glycol to carry out molten to the first solid catalyst and the second solid catalyst respectively
Swollen；
The first described solid catalyst is KC 108A, any one in KC 108B, KC 108C, KC 108D type catalyst
Or two kinds of mixture mixed with arbitrary proportion；
The second described solid catalyst is KC 108A, in KC 108B, KC 108C, KC 108D type catalyst any two kinds
Or three kinds of mixture mixed with arbitrary proportion；
(2) removing impurities for the first time: the ethylene glycol containing impurity is passed in the first solid catalyst, temperature be 30～60 DEG C,
Pressure is 0.1～1MPa, material air speed is 3～12h-Under conditions of imurity-removal, after catalyst absorption impurity, ethylene glycol material
It is passed in the second solid catalyst；
(3) removing impurities for the second time: the ethylene glycol material that step (2) obtains is passed in the second solid catalyst, temperature be 30～
60 DEG C, pressure be 0.1～1MPa, material air speed be 3～12h-Under conditions of imurity-removal, after catalyst absorption impurity, pure
Ethylene glycol is gathered.
Method the most according to claim 1, it is characterised in that comprise the following steps:
(1) catalyst is swelling: after loading the first solid catalyst respectively in the first finishing reactor A, B, opens respective nitrogen
Gas entrance, nitrogen tube (20), backwash liquor entrance, backwash tube (33), backwash liquor and nitrogen enter into the first finishing reactor A, B
In, nitrogen makes backwash liquor be fully contacted with catalyst, is allowed to swelling, after difference swelling 30～300min, closes backwash liquor respectively
Entrance, backwash tube, nitrogen inlet, nitrogen tube, open liquid inlet, and waste liquid drains into filter B by backwash tube outlet (34)
(31) in；
After loading the second solid catalyst respectively in the second finishing reactor A, B, open backwash liquor entrance (12), backwash tube
(33), nitrogen inlet (10), nitrogen tube (20), backwash liquor and nitrogen enters in the second finishing reactor monomer B, and nitrogen makes instead
Washing liquid is fully contacted with catalyst, is allowed to swelling, swelling 30～300min；At valve a (35), valve b (36) in closed mode
Under, open valve c (37), nitrogen and backwash liquor enter into the through second segment liquid inlet (8), first liquid outlet (5) successively
In two finishing reactor monomer A, nitrogen makes backwash liquor be fully contacted with catalyst, after being allowed to swelling 30～300min, closes anti-
Wash pipe (33), nitrogen inlet (10), open first paragraph liquid inlet (1) and valve d (38), in the second finishing reactor monomer A
Waste liquid from one section of liquid inlet (1) through backwash liquor outlet (34) is discharged to filter B (31), the second finishing reactor monomer
Waste liquid in B from backwash liquor entrance (12) through valve d is discharged to filter B (31)；Finally close backwash liquor entrance (12)；Described
Waste liquid in catalyst converter B through filtration after obtain pure ethylene glycol, be saved in ethylene glycol holding vessel；
(2) removing impurities for the first time: it is refined anti-that the ethylene glycol containing plurality of impurities is had respectively entered first by ethylene glycol feed pipe (19)
Answer in device A, B, obtain material ethylene glycol respectively through after the first solid catalyst absorption impurity；Open liquid outlet respectively,
To ethylene glycol material in outlet A (24) enters into filter A (25), filter A intercepts and reclaims the catalyst that spills；
(3) removing impurities for the second time: open first paragraph liquid inlet (1), second segment liquid inlet (8), through the filtration described in step (2)
Ethylene glycol material after device A (25) filters is directed respectively into the second finishing reactor monomer A and B through outlet B (26)；Warp respectively
Ethylene glycol is obtained after crossing the second solid catalyst absorption impurity；Open first paragraph liquid outlet (5), second segment liquid outlet respectively
(11) ethylene glycol, obtained enters into filter C (29) through first liquid outlet (27), second liquid outlet (28) respectively
In, filter C intercepts after reclaiming the catalyst spilt and obtains qualified ethylene glycol, imports to the second two of outside through outlet C (30)
In alcohol holding vessel.
3. a device for plurality of impurities in the removing ethylene glycol in method described in claim 2, including the first finishing reactor A
(21), the first finishing reactor B (22), the second finishing reactor (23), filter A (25), filter B (31), filter C
(29), ethylene glycol feed pipe (19), nitrogen tube (20), backwash tube (33), backwash liquor outlet (34), it is characterised in that:
Described ethanol feed pipe (19), import is connected with the device of the outside ethylene glycol containing plurality of impurities provided, outlet point
For two-way, a road is connected with the import of backwash tube (33), another road respectively with the first finishing reactor A, the first refining reaction
The liquid inlet of device B is connected；First finishing reactor A, the liquid outlet of the first finishing reactor B pass through outlet A respectively
(24) import with filter A (25) is connected；The outlet of filter A is by outlet B (26) and the second finishing reactor
Liquid inlet is connected；The liquid outlet of the second finishing reactor is connected with the import of filter C (29), and filter C goes out
Mouth is connected with outside ethylene glycol holding vessel by outlet C (30)；
Described backwash tube (33), import is connected with ethanol feed pipe or the outside device providing backwash liquor ethylene glycol, outlet
It is connected with the first finishing reactor A, the first finishing reactor B, the backwash liquor entrance of the second finishing reactor respectively, thus will
Backwash liquor is directed in each reactor；First finishing reactor A, the first finishing reactor B, the liquid of the second finishing reactor enter
Mouth also import with described backwash liquor outlet (34) is connected, and backwash liquor is derived to backwash from the liquid inlet of each reactor
In liquid outlet；The outlet of backwash liquor outlet is connected with the import of filter B (31), and the outlet of filter B is by outlet
Pipe D (32) is connected with outside ethylene glycol holding vessel；
Described nitrogen tube (20), import and outside provide the device of nitrogen to be connected, export respectively with the first finishing reactor A,
First finishing reactor B, the nitrogen inlet of the second finishing reactor are connected.
Device the most according to claim 3, it is characterised in that: described the first finishing reactor A, the first finishing reactor
B structure is identical and uses connected mode in parallel to link together: its top all offers liquid inlet, and liquid inlet is the most logical
Piping is connected with the outlet of described ethylene glycol feed pipe (19)；Nitrogen inlet, backwash liquor entrance is all offered bottom it
And liquid outlet, nitrogen inlet all outlets with described nitrogen tube (20) are connected, backwash liquor entrance all with described backwash
The outlet of pipe (33) is connected, and liquid outlet is all connected with outlet A (24)；Described backwash liquor entrance the most all passes through pipeline
Import with backwash liquor outlet (34) is connected；
The second described finishing reactor, top is provided with first paragraph liquid inlet (1), middle part be provided with first paragraph liquid outlet (5),
Second segment liquid inlet (8), bottom is provided with nitrogen inlet (10), second segment liquid outlet (11), backwash liquor entrance (12), its
In: first paragraph liquid inlet (1), second segment liquid inlet (8) are all connected with described outlet B (26)；First paragraph liquid discharge
Mouth (5) connection has first liquid outlet (27), second segment liquid outlet (11) to connect and has second liquid outlet (28), and the
The all imports with described filter C (29) of one liquid outlet tube, second liquid outlet are connected；Nitrogen inlet (10) and institute
The outlet of the nitrogen tube (20) stated is connected, and backwash liquor entrance (12) is connected with the outlet of described backwash tube (33)；Described
First paragraph liquid inlet (1) be connected also by the import of pipeline with described backwash liquor outlet (34).
Device the most according to claim 4, it is characterised in that described outlet B (26) and second segment liquid inlet (8)
Being provided with valve a (35) on the branch road being connected, first liquid outlet (27) is provided with valve b (36), first liquid exports
(5), connect between second segment liquid inlet (8) and have backwash liquor passage I, backwash liquor passage I is provided with valve c (37), backwash
Liquid entrance (12) is connected also by the import of backwash liquor passage II with filter B (31), and backwash liquor passage II is provided with valve
Door d (38).
Device the most according to claim 4, it is characterised in that described the second finishing reactor (23) is by 2 sections of reactors
Monomer is constituted, and is i.e. made up of according to order up and down the second finishing reactor monomer A (231), the second finishing reactor monomer B (232),
Structure is as follows:
The second described finishing reactor monomer A top offers first paragraph liquid inlet (1), bottom offers first paragraph liquid
Outlet (5), body wall top offers first paragraph solid catalyst loading port (2) and is provided with first paragraph visor (3), body wall bottom
Offer first paragraph solid catalyst and unload agent mouth (4)；Monomer A is internally installed first paragraph liquid distribution trough (13), and first paragraph
Liquid distribution trough is positioned at bottom, first paragraph liquid inlet, the top of first paragraph visor；Monomer A is internally installed has first paragraph filter cap to divide
Fabric swatch (14), and first paragraph filter cap distribution grid is positioned at first paragraph solid catalyst and unloads agent mouth bottom, first paragraph liquid outlet top；
It is filled with solid catalyst A (17) in monomer between described first paragraph visor, first paragraph filter cap distribution grid；
The second described finishing reactor monomer B, the body wall topmost of monomer offers second segment liquid inlet (8), second segment
Liquid inlet connects has feed tube, the leakage fluid dram of feed tube end to be positioned at inside monomer B；The bottom of monomer B offers nitrogen and enters
Mouth (10), second segment liquid outlet (11), backwash liquor entrance (12)；The body wall top of monomer B offers second segment solid catalysis
Agent loading port (6) and be provided with second segment visor (7), body wall bottom offers second segment solid catalyst and unloads agent mouth (9)；Monomer
B is internally installed second segment liquid distribution trough (15), and second segment liquid distribution trough is positioned at leakage fluid dram bottom, second segment visor
(7) top；Monomer B is internally installed second segment filter cap distribution grid (16), and second segment filter cap distribution grid is positioned at second segment admittedly
Body catalyst unloads agent mouth (9) bottom, second segment liquid outlet (11) top；Described second segment visor, second segment filter cap are distributed
Solid catalyst B (18) it is filled with in monomer between plate；
Described first paragraph liquid distribution trough (13), second segment liquid distribution trough (15) structure are identical, are calandria or endless tube
Formula liquid distribution trough, the filter tube of liquid distribution trough is wrapping wire filter tube or the filter tube being cased with filter bag；
Described first paragraph filter cap distribution grid (14), second segment filter cap distribution grid (16) structure are identical, on filter cap distribution grid equipped with
Some filter caps；Described filter cap is wire wrap filter cap or filter bag type filter cap；Described filter cap and the connected mode of filter cap distribution grid
Use threaded or locknut connection.
Device the most according to claim 6, it is characterised in that constitute two lists of the main body of the second finishing reactor (23)
Physical ability is split as two independent monolayer bed reactor monomers, be i.e. split as the second independent finishing reactor monomer A (231) and
The second independent finishing reactor monomer B (232): nitrogen inlet (10) and anti-is offered in the bottom of the second finishing reactor monomer A
Wash liquor inlet (12) uses connected mode to be in parallel or in series connected with the second finishing reactor monomer B afterwards.
Device the most according to claim 6, it is characterised in that the first finishing reactor A, the knot of the first finishing reactor B
Structure is identical with the structure of the second described finishing reactor monomer A (231), the second finishing reactor monomer B (232).
Device the most according to claim 4, it is characterised in that described the second finishing reactor (23) is by N section reactor
Monomer is constituted, 2 ＜ N≤10；The solid catalyst with identical or different function, solid catalyst is filled respectively in every section of monomer
Kind is n, 1 ＜ n≤10；
The top of every section of described reactor monomer all offers liquid inlet, bottom and all offers liquid outlet；Body wall top
All offer solid catalyst loading port and visor is installed；Body wall bottom all offers solid catalyst and unloads agent mouth；Internal equal
Liquid distribution trough is installed, and liquid distribution trough is positioned at the top of bottom, liquid inlet, visor；Internally installed have filter cap to be distributed
Plate, and filter cap distribution grid is positioned at solid catalyst and unloads agent mouth bottom, liquid outlet top；Described visor, filter cap distribution grid it
Between monomer in be filled with solid catalyst；Final stage monomer, is further opened with nitrogen inlet and backwash in addition to liquid outlet
Liquid entrance；The liquid inlet of every section of monomer is all connected with outlet B (26), liquid outlet all with the import phase of filter C (29)
Connect；Nitrogen inlet is connected with the outlet of nitrogen tube (20), reactant liquor entrance is connected with the outlet of backwash tube (33)；First
The also import with backwash liquor outlet (34) of the liquid inlet of Duan Danti is connected；
Described liquid distribution trough, for calandria or annular tube type liquid distribution trough, the filter tube of liquid distribution trough is that wrapping wire filters
Manage or be cased with the filter tube of filter bag；Described filter cap distribution grid, equipped with some filter caps on filter cap distribution grid, filter cap is wire wrap filter
Cap or filter bag type filter cap, filter cap is threaded with the employing of the connected mode of filter cap distribution grid or locknut is connected.
Device the most according to claim 9, it is characterised in that constitute N number of monomer of the second finishing reactor (23) main body
N number of independent monolayer bed reactor monomer, 2 ＜ N≤10 can be split as；Except final stage monomer, the bottom of other monomers is opened
If using connected mode to be in parallel or in series connected with final stage monomer after nitrogen inlet and backwash liquor entrance.
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| CN106975323A (en) * | 2017-04-06 | 2017-07-25 | 西安石油大学 | One kind failure selexol process regenerative device of solution |
| CN117466712A (en) * | 2022-07-21 | 2024-01-30 | 中国石油化工股份有限公司 | Recovery method of extractant of methyl acetate refining system |
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| CN106975323A (en) * | 2017-04-06 | 2017-07-25 | 西安石油大学 | One kind failure selexol process regenerative device of solution |
| CN106975323B (en) * | 2017-04-06 | 2023-12-05 | 西安石油大学 | Invalid natural gas desulfurization solution regeneration device |
| CN117466712A (en) * | 2022-07-21 | 2024-01-30 | 中国石油化工股份有限公司 | Recovery method of extractant of methyl acetate refining system |
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