CN106278821B - The method and device of plurality of impurities in a kind of removing ethylene glycol - Google Patents

The method and device of plurality of impurities in a kind of removing ethylene glycol Download PDF

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CN106278821B
CN106278821B CN201610891324.8A CN201610891324A CN106278821B CN 106278821 B CN106278821 B CN 106278821B CN 201610891324 A CN201610891324 A CN 201610891324A CN 106278821 B CN106278821 B CN 106278821B
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outlet
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filter
monomer
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CN106278821A (en
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王文学
毛进池
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Kai Rui Environmental Protection Science And Technology Co Ltd
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Kai Rui Environmental Protection Science And Technology Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/74Separation; Purification; Use of additives, e.g. for stabilisation
    • C07C29/88Separation; Purification; Use of additives, e.g. for stabilisation by treatment giving rise to a chemical modification of at least one compound
    • C07C29/92Separation; 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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Abstract

The invention discloses a kind of method and devices of plurality of impurities in removing ethylene glycol, the device includes two the first finishing reactors in parallel, the second finishing reactor being made 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: process is simple, and removing impurities effect is good, high financial profit;Method of operation flexible operation, realization is not parking to change agent;The advantages of second finishing reactor has multistage set, compact-sized, saving space and investment, convenient for operation and manages;Liquid distribution trough is provided in reactor, when being uniformly distributed for feed stream not only having may be implemented, but also can avoid being lost to intercept solid catalyst particle when backwash into reactor by liquid distribution trough to purification ethylene glycol;It is provided with multiple filter caps on filter cap distribution grid in reactor, not only can guarantee stability of flow, but also solid catalyst particle can be intercepted, avoid losing.

Description

The method and device of plurality of impurities in a kind of removing ethylene glycol
Technical field
The present invention relates to a kind of method and devices of plurality of impurities in removing ethylene glycol, and UV transmittance can be improved, main It is used for purifying ethylene glycol technical field, belongs to technical field of petrochemical industry.
Background technique
Ethylene glycol (EG) is a kind of important Organic Chemicals, mainly for the production of polyester, anti-icing fluid, adhesive, oil White spirit, Everlube, surfactant and polyester polyol etc..Wherein polyester is the major consumers neck of China's ethylene glycol Domain, consumption figure account for about the 94.0% of gross domestic consumption amount, and in addition about 6.0% for antifreezing agent, adhesive, paint solvent, resistance to Cold lubricating oil, surfactant and polyester polyol etc..
Although the purity of the ethylene glycol product of China's oil route and Coal Chemical Industry Route is attained by 99.9% or more, It is all different degrees of there is beyond expression of words with content in product, there is the organic of absorption in 220nm~350nm wave-length coverage It is miscellaneous.The presence of these impurity declines the ultraviolet permeability of 220nm~350nm wave-length coverage, influences the quality of polyester, such as fiber Gloss, coloration, coloring and hardness etc..Therefore the quality of ethylene glycol depends primarily on ISOUV value index.
Studies have shown that the impurity for influencing quality of ethylene glycol product is mainly some by-products in production process.
Some by-products during impurity such as in petroleum path ethylene glycol product is mainly ethylene, including The organic compounds 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 micro by-products in the aerobic subtractive process of high temperature, comprising: esters and substituted cyclic diketones and grip aldehydes altogether on a small quantity Substance.And these contain carbonyl impurities biggish absorption in 220nm~350nm wave-length coverage, therefore reduce these carbonyls The content of compound impurities improves ethylene glycol product in the ultraviolet permeability of wavelength 220nm~350nm range, to raising second two The quality of alcohol is of great importance.
The present invention removes the method that plurality of impurities improves UV transmittance in ethylene glycol, passes through advanced purifying ethylene glycol work Skill is combined with the second finishing reactor with special internal structure, and by being equipped with multistage and several functions solid catalysis Agent is used cooperatively, and can effectively remove the various impurity in ethylene glycol, improves ethylene glycol product in wavelength 220nm~350nm model The ultraviolet permeability enclosed, achievees the purpose that purifying ethylene glycol.
Summary of the invention
The technical problem to be solved by the present invention is to be directed to the deficiencies in the prior art, and provide a kind of removing second two The device of plurality of impurities in alcohol, the device are anti-by advanced Purification Catalysts of Monoethylene Glycol and the second purification with special internal structure It answers device 202 to combine, through being used cooperatively for several functions solid catalyst, achievees the purpose that ethylene glycol exquisiteness.
The technical problem to be solved by the present invention is to be directed to the deficiencies in the prior art, and provide a kind of removing second two The method of plurality of impurities in alcohol, this method can remove aldehyde type impurities and removing micro in petroleum path ethylene glycol product Micro ester group and keto compounds impurity in coal-ethylene glycol product, to significantly improve the UV transmittance of ethylene glycol.
To achieve the goals above, the present invention adopts the following technical scheme:
A kind of method of plurality of impurities in removing ethylene glycol, comprising the following steps:
(1) be catalyzed solvent swell: using backwash liquor ethylene glycol respectively to the first solid catalyst and the second solid catalyst into Row swelling;
First solid catalyst is KC 108A, KC 108B, KC 108C, any in KC 108D type catalyst The mixture that one or two are mixed in any proportion;(four kinds of catalyst are that triumphant auspicious environmentally friendly Science and Technology Co., Ltd. exists CN102911013B is the catalyst invented in (2012104484052));
Second solid catalyst is KC 108A, KC 108B, KC 108C, any in KC 108D type catalyst Two or three of mixture being mixed in any proportion;(four kinds of catalyst are that triumphant auspicious environmentally friendly Science and Technology Co., Ltd. exists CN102911013B is the catalyst invented in (2012104484052));
(2) first time removing impurities: the ethylene glycol containing impurity is passed into the first solid catalyst, is 30~60 in temperature DEG C, pressure be 0.1~1MPa, material air speed is 3~12h-Under conditions of imurity-removal, catalyst absorb impurity after, ethylene glycol Material is passed into the second solid catalyst;
(3) second of removing impurities: the ethylene glycol material that step (2) obtains is passed into the second solid catalyst, is in temperature 30~60 DEG C, pressure be 0.1~1MPa, material air speed is 3~12h-Under conditions of imurity-removal, catalyst absorb impurity after, Purified ethylene glycol harvesting.
In above-mentioned technical proposal, method includes that (opening of all components is defaulted as closing before use step in detail below Closed state):
(1) it is catalyzed solvent swell: after loading the first solid catalyst respectively into the first finishing reactor A, B, opening respective Nitrogen inlet, nitrogen tube, backwash liquor import, backwash tube, backwash liquor and nitrogen enters in the first finishing reactor A, B, nitrogen Gas comes into full contact with backwash liquor with catalyst, is allowed to be swollen, respectively be swollen 30~300min after, respectively close backwash liquor import, Backwash tube, nitrogen inlet, nitrogen tube, open opening, and waste liquid is drained into filter B by backwash tube outlet;
After loading the second solid catalyst respectively into 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 urges backwash liquor with solid Agent comes into full contact with, and is allowed to be swollen, and is swollen 30~300min;In the case where valve a, valve b are in closed state, valve c, nitrogen are opened It is successively entered in the second finishing reactor monomer A through second segment liquid inlet, the first liquid outlet with backwash liquor, nitrogen makes instead Washing lotion comes into full contact with solid catalyst, is allowed to after being swollen 30~300min, closes backwash tube, nitrogen inlet, opens first segment Waste liquid in liquid inlet and valve d, the second finishing reactor monomer A was discharged to from one section of liquid inlet through backwash liquor outlet In filter B, the waste liquid in the second finishing reactor monomer B is discharged in filter B from backwash liquor entrance through valve d;Finally close Backwash liquor entrance;Waste liquid obtains purified ethylene glycol after filtering in catalyst converter B, is stored in ethylene glycol holding vessel;
The type of the first solid catalyst loaded in two the first finishing reactors is identical or different;
The solid catalyst loaded in second finishing reactor A is solid catalyst A, is loaded in the second finishing reactor B Solid catalyst be solid catalyst B, as the second solid catalyst, type is identical or different by solid catalyst A, B;
(2) first time removing impurities: the ethylene glycol containing plurality of impurities has respectively entered first through import by ethylene glycol feed pipe In finishing reactor A, B, material ethylene glycol is obtained after the first solid catalyst absorbs impurity respectively;Discharging is opened respectively Mouthful, obtained ethylene glycol material enters in filter A through outlet A, and filter A intercepts the catalyst that recycling leaks out;
First finishing reactor A, the B reaction condition is identical: temperature is 30~60 DEG C, pressure is 0.1~1MPa, object Material air speed is 3~12h-
(3) second of removing impurities: first segment liquid inlet, second segment liquid inlet are opened, through filter described in step (2) The filtered ethylene glycol material of A is directed respectively into through outlet B to the second finishing reactor monomer A and B;Pass through solid catalysis respectively Agent A, B obtain ethylene glycol after absorbing impurity;First segment liquid outlet, second segment liquid outlet, obtained ethylene glycol are opened respectively It is entered in filter C through the first liquid outlet tube, second liquid outlet respectively, filter C intercepts the catalysis that recycling leaks out Qualified ethylene glycol is obtained after agent, is imported into external ethylene glycol holding vessel through outlet C;
Second finishing reactor monomer A, B, operating condition are identical: temperature is 30~60 DEG C, pressure is 0.1~1MPa, object Material air speed is 3~12h-
The present invention also provides the devices of plurality of impurities in the removing ethylene glycol used in a kind of above 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 charging Pipe, nitrogen tube, backwash tube, backwash liquor outlet:
The ethyl alcohol feed pipe, import are connect with the device for the ethylene glycol containing plurality of impurities that outside provides, outlet point For two-way, be connected all the way with the import of backwash tube, another way respectively with the first finishing reactor A, the first finishing reactor B Liquid inlet is connected;First finishing reactor A, the first finishing reactor B liquid outlet pass through respectively outlet A and filtering The import of device A is connected;The outlet of filter A is connected by outlet B with the liquid inlet of 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 passes through outlet C and external second Glycol holding vessel is connected;
The backwash tube, import are connected with ethyl alcohol feed pipe or the external device for providing backwash liquor ethylene glycol, export It is connected respectively with the backwash liquor entrance of the first finishing reactor A, the first finishing reactor B, the second finishing reactor, thus will Backwash liquor is directed into each reactor;First finishing reactor A, the first finishing reactor B, the second finishing reactor liquid enter Mouth is also connected with the import of the backwash liquor outlet, and backwash liquor exports to backwash liquor from the liquid inlet of each reactor In mouth pipe;The outlet of backwash liquor outlet is connected with the import of filter B, and the outlet of filter B passes through outlet D and outside Ethylene glycol holding vessel be connected;
The nitrogen tube, import are connected with the external device for providing nitrogen, export respectively with the first finishing reactor A, First finishing reactor B, the second finishing reactor nitrogen inlet be connected.
In above-mentioned technical proposal, the first finishing reactor A, the first finishing reactor B structure are identical and using simultaneously The connection type of connection links together: its top offers liquid inlet, and liquid inlet passes through pipeline and the second two The outlet of alcohol feed pipe is connected;Its bottom offers nitrogen inlet, backwash liquor entrance and liquid outlet, nitrogen inlet with The outlet of the nitrogen tube (20) is connected, and backwash liquor entrance is connected with the outlet of the backwash tube, liquid outlet It is connected with outlet A;The backwash liquor entrance is also connected by pipeline with the import of backwash liquor outlet.
In above-mentioned technical proposal, second finishing reactor, top is equipped with first segment liquid inlet, and middle part is equipped with the One section of liquid outlet, second segment liquid inlet, bottom are equipped with nitrogen inlet, second segment liquid outlet, backwash liquor entrance, in which: First segment liquid inlet, second segment liquid inlet are connected with the outlet B;First segment liquid outlet is connected with the first liquid Body outlet, second segment liquid outlet are connected with second liquid outlet, and the first liquid outlet tube, second liquid outlet are equal It is connected with the import of the filter C;Nitrogen inlet is connected with the outlet of the nitrogen tube, backwash liquor entrance and institute The outlet for the backwash tube stated is connected;The first segment liquid inlet also pass through pipeline and the backwash liquor outlet into Mouth is connected;
The outlet B, the branch road being connected with second segment liquid inlet are equipped with valve a;First liquid Valve b is installed on outlet;It is connected with backwash liquor channel I between first liquid outlet, second segment liquid inlet, instead Valve c is installed on washing liquid channel I;The backwash liquor entrance also passes through import III phase of the backwash liquor channel II with filter B Even, valve d is installed on the II of backwash liquor channel.
In above-mentioned technical proposal, second finishing reactor is made of 2 sections of reactor monomers, i.e., anti-by the second purification Device monomer A, the second finishing reactor monomer B is answered to constitute according to sequence up and down, structure is as follows:
First segment liquid inlet is offered at the top of the second finishing reactor monomer A, bottom offers first segment liquid Body outlet, body wall top offer first segment solid catalyst loading port and are equipped with first segment visor, and body wall lower part offers First segment solid catalyst unloads agent mouth;First segment liquid distribution trough is installed, and first segment liquid distribution trough is located inside monomer A First segment liquid inlet lower part, first segment visor top;First segment filter cap distribution grid, and first segment are installed inside monomer A Filter cap distribution grid is located at first segment solid catalyst and unloads agent mouth lower part, first segment liquid outlet top;The first segment visor, Solid catalyst A is filled in monomer between first segment filter cap distribution grid;
The second finishing reactor monomer B, the body wall topmost of monomer offer second segment liquid inlet, second segment Liquid inlet is connected with inlet tube, and the leakage fluid dram of feed liquor pipe end is located 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 lower part offers second segment solid catalyst and unloads agent mouth;Second segment liquid is installed inside monomer B Distributor, and second segment liquid distribution trough is located at the top of leakage fluid dram lower part, second segment visor;Second is equipped with inside monomer B Section filter cap distribution grid, and second segment filter cap distribution grid is located at second segment solid catalyst and unloads agent mouth lower part, second segment liquid outlet Top;Solid catalyst B is filled in monomer between the second segment visor, second segment filter cap distribution grid;
The first segment liquid distribution trough, second segment liquid distribution trough structure are identical, are calandria or annular tube type liquid Body distributor, the screen pipe of liquid distribution trough are wrapping wire screen pipe or the screen pipe for being cased with filter bag;
The first segment filter cap distribution grid, second segment filter cap distributing plate structure are identical, equipped with several on filter cap distribution grid Filter cap;The filter cap is wire wrap filter cap or filter bag type filter cap;The connection type of the filter cap and filter cap distribution grid uses It is threadedly coupled or locknut connects.
In above-mentioned technical proposal, two monomers for constituting the main body of the second finishing reactor can be split as two independent lists Layer bed reactor monomer, that is, split and be independent the second finishing reactor monomer A and independent second finishing reactor monomer B: The bottom of second finishing reactor monomer A uses after opening up nitrogen inlet and backwash liquor entrance with the second finishing reactor monomer B In parallel or in series connection type connection after, then with backwash liquor outlet, outlet B, nitrogen tube, backwash tube, filter C phase Connection:
When second finishing reactor monomer A, the second finishing reactor monomer B are connected in a series arrangement: outlet B and second The first segment liquid inlet of finishing reactor monomer A is connected, the first segment liquid outlet of the second finishing reactor monomer A and The second segment liquid inlet of two finishing reactor B is connected, the second segment liquid outlet and filter C of the second finishing reactor B It is connected;The nitrogen inlet of nitrogen inlet and the second finishing reactor monomer B that first finishing reactor monomer A is newly opened is and nitrogen Tracheae is connected;The backwash liquor entrance of the backwash liquor entrance that first finishing reactor A is newly opened and the second finishing reactor monomer B is equal It is connected with backwash tube;First segment liquid inlet, second segment liquid inlet are also connected with backwash liquor outlet;
When second finishing reactor monomer A, the second finishing reactor monomer B are connected with parallel way: the second refining reaction The first segment liquid inlet of device monomer A, the second finishing reactor B second segment liquid inlet be connected with outlet B, second essence First segment liquid outlet, the second segment liquid outlet of reactor monomer A processed is connected with filter C;First finishing reactor list The nitrogen inlet that body A is newly opened is connected with nitrogen tube with the nitrogen inlet of the second finishing reactor monomer B, the first refining reaction The backwash liquor entrance that device A is newly opened is connected with backwash tube with the backwash liquor entrance of the second finishing reactor monomer B;First segment liquid Body entrance, second segment liquid inlet are also connected with backwash liquor outlet.
In above-mentioned technical proposal, the first finishing reactor A, the first finishing reactor B, structure and the second purification are anti- Answer device monomer A, independent second finishing reactor monomer B identical;Two monomers for constituting the second finishing reactor main body can After being split as two independent single layer bed reactor monomers, make as the first finishing reactor A and the first finishing reactor B With internal structure chart is referring to the second finishing reactor: top offers opening, and bottom offers nitrogen inlet, backwash liquor import And discharge port;Body wall top offers solid catalyst loading port, body wall top is mounted on visor;Body wall lower part offers solid Body catalyst unloads agent mouth;Inside is equipped with liquid distribution trough, and liquid distribution trough is located at the top of lower opening portion, visor;Monomer Inside is equipped with filter cap distribution grid, and filter cap distribution grid is located at solid catalyst and unloads agent mouth lower part, discharge port top;The view Solid catalyst is filled in monomer between mirror, filter cap distribution grid.
In above-mentioned technical proposal, the second finishing reactor can also be made of multistage reactor monomer, i.e., by N sections of reactors Monomer constitutes (2 N≤10 <, preferably 2 N≤8 <, N≤5 further preferred 2 <), in every section of monomer respectively filling have it is identical or The solid catalyst of different function, solid catalyst type are n, 1 n≤10 <, preferably 2≤N≤5;
The top of reactor monomer described in every section offers liquid inlet, bottom and offers liquid outlet;Body wall Top offers solid catalyst loading port, body wall top is mounted on visor;Body wall lower part offers solid catalyst Unload agent mouth;Liquid distribution trough is mounted on inside monomer, and liquid distribution trough is located at the top of liquid inlet lower part, visor;It is single Internal portion is equipped with filter cap distribution grid, and filter cap distribution grid is located at solid catalyst and unloads agent mouth lower part, liquid outlet top;It is described Visor, be filled with solid catalyst in the monomer between filter cap distribution grid;Final stage monomer, is also opened other than liquid outlet Equipped with nitrogen inlet and backwash liquor entrance;The liquid inlet of every section of monomer is connected with outlet B, and liquid outlet is and filter C is connected;Nitrogen inlet is connected with nitrogen tube, reaction solution entrance is connected with backwash tube;The liquid inlet of first segment monomer is also and instead Washing lotion outlet pipe is connected;
The liquid distribution trough, is calandria or annular tube type liquid distribution trough, and the screen pipe of liquid distribution trough is wrapping wire Screen pipe or the screen pipe for being cased with filter bag;The filter cap distribution grid is equipped with several filter caps on filter cap distribution grid, and filter cap is wrapping wire Formula filter cap or filter bag type filter cap, filter cap are connect with the connection type of filter cap distribution grid using threaded connection or locknut.
In above-mentioned technical proposal, the multistage reactor monomer can also split into N number of independent single layer bed reactor Monomer ((2 N≤10 <, preferably 2 N≤8 <, N≤5 further preferred 2 <), in addition to final stage monomer, the bottom of other monomers Open up and connect with final stage monomer using connection type in parallel or in series after nitrogen inlet and backwash liquor entrance, connect or Person's parallel connection is identical as the catenation principle and connection type that split into two monomers.
The advantages of technical solution of the present invention is: 1, process is simple, and the impurity removal effect in ethylene glycol is good, economic benefit It is 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, realization is not parking to change agent;3, the second finishing reactor includes 1) multistage set, compact-sized, saves empty Between and invest, convenient for operation and management;2) liquid distribution trough is provided in reactor cylinder body, when to purification ethylene glycol, Into reactor by liquid distribution trough, being uniformly distributed for feed stream not only may be implemented, but also can have been urged with intercepting solid when backwash Catalyst particles avoid being lost;3) it is provided with multiple filter caps on the filter cap distribution grid in reactor cylinder body, both can guarantee that flow was steady It is fixed, and solid catalyst particle can be intercepted, it avoids losing.
Detailed description of the invention
Fig. 1: the overall structure diagram of apparatus of the present invention;
Fig. 2: knot when the second finishing reactor is split as two independent single layer bed reactor monomers in apparatus of the present invention Structure schematic diagram;
Fig. 3: structure schematic diagram when the second finishing reactor is made of 2 sections of reactor monomers in apparatus of the present invention;
Wherein: 1, first segment liquid inlet 2, first segment solid catalyst loading port 3, first segment visor 4, first segment Solid catalyst unloads agent mouth 5, first segment 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 sections of liquid inlets 9, second segment solid catalyst Entrance 13, first segment liquid distribution trough 14, first segment filter cap distribution grid 15, second segment liquid distribution trough 16, second segment filter Cap distribution grid 17, solid catalyst A 18, solid catalyst B 19, ethylene glycol feed pipe 20, nitrogen tube 21, first refine Reactor A 22, the first finishing reactor B 23, the second finishing reactor 231, the second finishing reactor monomer A 232, second Finishing reactor monomer B 24, outlet A 25, filter A26, outlet B 27, the first liquid outlet tube 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.
Specific embodiment
The specific embodiment of technical solution of the present invention is described in detail below, but the present invention is not limited in being described below Hold:
The present invention provides a kind of method for removing plurality of impurities in ethylene glycol, comprising the following steps:
(1) it is catalyzed solvent swell: after loading the first solid catalyst respectively into the first finishing reactor A, B, opening respective Nitrogen inlet, nitrogen tube 20, backwash liquor entrance, backwash tube 33, backwash liquor and nitrogen enter the first finishing reactor A, B Interior, nitrogen comes into full contact with backwash liquor with catalyst, is allowed to be swollen, and after being swollen 30~300min respectively, 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 into the second finishing reactor A, B, backwash liquor entrance 12, backwash tube are opened 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 comes into full contact with, and is allowed to be swollen, and is swollen 30~300min;In the case where valve a35, valve b36 are in closed state, valve is opened C37, nitrogen and backwash liquor successively enter the second finishing reactor monomer A through second segment liquid inlet 8, the first liquid outlet 5 In, nitrogen comes into full contact with backwash liquor with catalyst, is allowed to after being swollen 30~300min, backwash tube 33, nitrogen inlet 10 are closed, The waste liquid in first segment liquid inlet 1 and valve d38, the second finishing reactor monomer A is opened 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 from backwash liquor entrance 12 through valve d Into filter B 31;Finally close backwash liquor entrance 12;The waste liquid obtains after filtering pure in catalyst converter B Ethylene glycol is stored in ethylene glycol holding vessel;
(2) first time removing impurities: the ethylene glycol containing plurality of impurities has respectively entered the first purification by ethylene glycol feed pipe 19 In reactor A, B, material ethylene glycol is obtained after the first solid catalyst absorbs impurity respectively;Liquid outlet is opened respectively, Obtained ethylene glycol material enters in filter A25 through outlet A24, and filter A intercepts the catalyst that recycling leaks out;
(3) second of removing impurities: first segment liquid inlet 1, second segment liquid inlet 8 are opened, through filtering described in step (2) The filtered ethylene glycol material of device A25 is directed respectively into through outlet B26 to the second finishing reactor monomer A and B;Respectively by the Two solid catalysts obtain ethylene glycol after absorbing impurity;First segment liquid outlet 5, second segment liquid outlet 11 are opened respectively, are obtained To ethylene glycol entered in filter C29 through the first liquid outlet tube 27, second liquid outlet 28 respectively, filter C is blocked Qualified ethylene glycol is obtained after cutting the catalyst that recycling leaks out, is imported into through outlet C30 in external ethylene glycol holding vessel.
The present invention also provides a kind of devices of plurality of impurities in removing ethylene glycol, including the first finishing reactor A21, first Finishing reactor B 22, the 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:
The ethyl alcohol feed pipe 19, import are connect with the device for the ethylene glycol containing plurality of impurities that outside provides, and are exported Be divided into two-way, be connected all the way with the import of backwash tube 33, another way respectively with the first finishing reactor A, the first refining reaction The liquid inlet of device B is connected;First finishing reactor A, the first finishing reactor B liquid outlet pass through outlet respectively A24 is connected with the import of filter A25;The outlet of filter A is entered by outlet B26 and the liquid of the second finishing reactor Mouth is connected;The liquid outlet of 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 external ethylene glycol holding vessel;
The backwash tube 33, import are connected with ethyl alcohol feed pipe or the external device for providing backwash liquor ethylene glycol, out Mouth is connected with the backwash liquor entrance of the first finishing reactor A, the first finishing reactor B, the second finishing reactor respectively, thus Backwash liquor is directed into each reactor;First finishing reactor A, the first finishing reactor B, the second finishing reactor liquid Entrance is also connected with the import of the backwash liquor outlet 34, and backwash liquor is exported from the liquid inlet of each reactor to backwash In liquid outlet;The outlet of backwash liquor outlet is connected with the import of filter B 31, and the outlet of filter B passes through outlet D32 is connected with external ethylene glycol holding vessel;
The nitrogen tube 20, import are connected with the external device for providing nitrogen, export respectively with the first finishing reactor A, the first finishing reactor B, the second finishing reactor nitrogen inlet be connected;
The first finishing reactor A, the first finishing reactor B structure are identical and are connected using connection type in parallel Be connected together: its top offers liquid inlet, and liquid inlet passes through going out for pipeline and the ethylene glycol feed pipe 19 Mouth is connected;Its bottom offers nitrogen inlet, backwash liquor entrance and liquid outlet, nitrogen inlet with the nitrogen tube 20 outlet is connected, and backwash liquor entrance is connected with the outlet of the backwash tube 33, liquid outlet with outlet A24 It is connected;The backwash liquor entrance is also connected by pipeline with the import of backwash liquor outlet 34;
Second finishing reactor, top be equipped with first segment liquid inlet 1, middle part be equipped with first segment liquid outlet 5, Second segment liquid inlet 8, bottom are equipped with nitrogen inlet 10, second segment liquid outlet 11, backwash liquor entrance 12, in which: first segment Liquid inlet 1, second segment liquid inlet 8 are connected with the outlet B26;First segment liquid outlet 5 is connected with the first liquid Body outlet 27, second segment liquid outlet 11 are connected with second liquid outlet 28, and the first liquid outlet tube, second liquid go out The import of filter C29 described in mouth Guan Junyu is connected;Nitrogen inlet 10 is connected with the outlet of the nitrogen tube 20, instead Wash liquor inlet 12 is connected with the outlet of the backwash tube 33;The first segment liquid inlet 1 also by pipeline with it is described The import of backwash liquor outlet 34 be connected;
The outlet B, the branch road being connected with second segment liquid inlet are equipped with valve a 35;First liquid outlet Valve b 36 is installed on pipe;Backwash liquor channel I is connected between first liquid outlet, second segment liquid inlet, backwash liquor is logical Valve c 37 is installed on road I;Backwash liquor entrance also passes through backwash liquor channel II and is connected with the import III of filter B, backwash liquor Valve d 38 is installed on the II of channel.
The second finishing reactor in the present invention is made of 2 sections of reactor monomers, i.e., by the second finishing reactor monomer A231, the second finishing reactor monomer B 232 are constituted, and structure chart is as shown in Figure 3:
Second top finishing reactor monomer A offers first segment liquid inlet, bottom offers first segment liquid outlet, Body wall top offers first segment solid catalyst loading port 2, and body wall top is equipped with first segment visor 3, and body wall lower part opens up There is first segment solid catalyst to unload agent mouth 4;First segment liquid distribution trough 13, and first segment liquid distribution trough are installed inside monomer Positioned at first segment liquid inlet lower part, the top of first segment visor;First segment filter cap distribution grid 14, and are installed inside monomer One section of filter cap distribution grid is located at first segment solid catalyst and unloads agent mouth lower part, first segment liquid outlet top;The first segment Solid catalyst A17 is filled in monomer between visor, first segment filter cap distribution grid;
The second finishing reactor monomer B, the body wall topmost of monomer offer second segment liquid inlet, second segment Liquid inlet is connected with inlet tube, and the leakage fluid dram of feed liquor pipe end is located 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 equipped with second segment visor 7, and body wall lower part offers second segment solid catalyst and unloads agent mouth 9;Second is equipped with inside monomer Section liquid distribution trough 15, and second segment liquid distribution trough is located at the top of leakage fluid dram lower part, second segment visor;Installation inside monomer There is second segment filter cap distribution grid 16, and second segment filter cap distribution grid is located at second segment solid catalyst and unloads agent mouth lower part, second segment Liquid outlet top;Solid catalyst B is filled in monomer between the second segment visor, second segment filter cap distribution grid 18;
The first segment liquid distribution trough, second segment liquid distribution trough structure are identical, are calandria or annular tube type liquid Body distributor, the screen pipe of liquid distribution trough are wrapping wire screen pipe or the screen pipe for being cased with filter bag;
The first segment filter cap distribution grid, second segment filter cap distributing plate structure are identical, equipped with several on filter cap distribution grid Filter cap;The filter cap is wire wrap filter cap or filter bag type filter cap;The connection type of the filter cap and filter cap distribution grid uses It is threadedly coupled or locknut connects.
Two monomers of the main body of the second finishing reactor of composition in the present invention can be split as two independent single layer beds Reactor monomer splits and is independent the second finishing reactor monomer A and independent second finishing reactor monomer B: the second The bottom of finishing reactor monomer A opens up after nitrogen inlet and backwash liquor entrance with the second finishing reactor monomer B using in parallel Or concatenated connection type connection, as shown in Figure 2.
The structure of the first finishing reactor A, the first finishing reactor B in the present invention and the second finishing reactor monomer A, The structure of second finishing reactor monomer B is identical, referring to Fig. 3.
The second finishing reactor can also be made of N sections of reactor monomers in the present invention, 2 N≤10 <;Divide in every section of monomer It Tian Chong be not n, 1 n≤10 < with the solid catalyst of identical or different function, solid catalyst type.It is anti-described in every section It answers the top of device monomer to offer liquid inlet, bottom and offers liquid outlet;Body wall top offers solid catalysis Agent loading port, body wall top are mounted on visor;Body wall lower part offers solid catalyst and unloads agent mouth;It is respectively mounted inside monomer There is liquid distribution trough, and liquid distribution trough is located at the top of liquid inlet lower part, visor;Filter cap distribution is installed inside monomer Plate, and filter cap distribution grid is located at solid catalyst and unloads agent mouth lower part, liquid outlet top;The visor, filter cap distribution grid it Between monomer in be filled with solid catalyst;Final stage monomer, is also provided with nitrogen inlet and backwash other than liquid outlet Liquid entrance;The liquid inlet of every section of monomer is connected with outlet B, and liquid outlet is connected with filter C;Nitrogen inlet and nitrogen Tracheae is connected, reaction solution entrance is connected with backwash tube;The liquid inlet of first segment monomer is also connected with backwash liquor outlet;It is described Liquid distribution trough, be calandria or annular tube type liquid distribution trough, the screen pipe of liquid distribution trough is wrapping wire screen pipe or is cased with The screen pipe of filter bag;The filter cap distribution grid, several filter caps are equipped on filter cap distribution grid, and filter cap is wire wrap filter cap or filter bag Formula filter cap, filter cap are connect with the connection type of filter cap distribution grid using threaded connection or locknut.Constitute the second finishing reactor 23 N number of monomer of main body can also be split as N number of independent single layer bed reactor monomer, 2 N≤10 <;In addition to final stage monomer, The bottom of his monomer opens up after nitrogen inlet and backwash liquor entrance with final stage monomer using connection side in parallel or in series Formula connection.
The method of the present invention is further described combined with specific embodiments below:
Embodiment 1:
A kind of method of plurality of impurities in removing ethylene glycol, comprising the following steps:
(1) it is catalyzed solvent swell: loading the first solid catalyst (being KC108B) respectively into the first finishing reactor A, B Afterwards, respective nitrogen inlet, nitrogen tube, backwash liquor import, backwash tube are opened, backwash liquor and nitrogen enter the first refining reaction In device A, B, nitrogen comes into full contact with backwash liquor with catalyst, is allowed to be swollen, and after being swollen 160~170min respectively, closes respectively Backwash liquor import, backwash tube, nitrogen inlet, nitrogen tube, open opening, and waste liquid is drained into filter B by backwash tube outlet;
The second solid catalyst i.e. solid catalyst A, B (solid catalyst A, B phase is loaded into the second finishing reactor Together, be the mixture that KC 108C, KC108D type catalyst are mixed 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 comes into full contact with, and is allowed to be swollen, and is swollen 160~170min;In the case where valve a, valve b are in closed state, valve is opened Door c, nitrogen and backwash liquor successively enter in the second finishing reactor monomer A through second segment liquid inlet, the first liquid outlet, Nitrogen comes into full contact with backwash liquor with solid catalyst A, is allowed to after being swollen 160~170min, closes backwash tube, nitrogen inlet, The waste liquid opened in first segment liquid inlet and valve d, the second finishing reactor monomer A goes out from one section of liquid inlet through backwash liquor Mouth pipe is discharged in filter B, and the waste liquid in the second finishing reactor monomer B is discharged to filter B through valve d from backwash liquor entrance In;Finally close backwash liquor entrance;
The waste liquid obtains pure ethylene glycol after filtering in catalyst converter B, is stored in ethylene glycol holding vessel;
(2) first time removing impurities: the ethylene glycol containing plurality of impurities has respectively entered first through import by ethylene glycol feed pipe In finishing reactor A, B, material ethylene glycol is obtained after the first solid catalyst absorbs impurity respectively;Discharging is opened respectively Mouthful, obtained ethylene glycol material enters in filter A through outlet A, and filter A intercepts the catalyst that recycling leaks out;
First finishing reactor A, the B reaction condition is identical: temperature is 40~50 DEG C, pressure is 0.5~0.6MPa, Material air speed is 7~8h-
(3) second of removing impurities: first segment liquid inlet, second segment liquid inlet are opened, through filter described in step (2) The filtered ethylene glycol material of A is directed respectively into through outlet B to the second finishing reactor monomer A and B;Pass through solid catalysis respectively Agent A, B obtain ethylene glycol after absorbing impurity;First segment liquid outlet, second segment liquid outlet, obtained ethylene glycol are opened respectively It is entered in filter C through the first liquid outlet tube, second liquid outlet respectively, filter C intercepts the catalysis that recycling leaks out Qualified ethylene glycol is obtained after agent, is imported into external ethylene glycol holding vessel through outlet C;
Second finishing reactor monomer A, B, operating condition are identical: temperature is 40~50 DEG C, pressure is 0.5~0.6MPa, Material air speed is 7~8h-
Production the result shows that: this technology and equipment can be greatly reduced esters in coal ethyl glycol, aldehyde material, The content of the carbonyls such as ketone and other impurities can effectively improve ethylene glycol product in wavelength 220nm~350nm range Ultraviolet permeability, the ultraviolet permeability for ethylene glycol that treated is in 220nm > 80%, 275nm > 94%, 350nm > 99%.
Examples detailed above is technical conception and technical characteristics to illustrate the invention, can not be limited with this of the invention Protection scope.The equivalent transformation or modification that all essence according to the present invention is done, should all cover in protection scope of the present invention Within.

Claims (9)

1. a kind of method of plurality of impurities in removing ethylene glycol, which comprises the following steps:
(1) it is catalyzed solvent swell: after loading the first solid catalyst respectively into the first finishing reactor A, B, opening respective nitrogen Gas entrance, nitrogen tube (20), backwash liquor entrance, backwash tube (33), backwash liquor and nitrogen enter the first finishing reactor A, B Interior, nitrogen comes into full contact with backwash liquor with catalyst, is allowed to be swollen, and after being swollen 30~300min respectively, 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 into the second finishing reactor A, B, backwash liquor entrance (12), backwash tube are opened (33), nitrogen inlet (10), nitrogen tube (20), backwash liquor and nitrogen enter in the second finishing reactor monomer B, and nitrogen makes instead Washing lotion comes into full contact with catalyst, is allowed to be swollen, and is swollen 30~300min;It is in closed state in valve a (35), valve b (36) Under, it opens valve c (37), nitrogen and backwash liquor successively enter the through second segment liquid inlet (8), the first liquid outlet (5) In two finishing reactor monomer A, nitrogen comes into full contact with backwash liquor with catalyst, is allowed to after being swollen 30~300min, closes anti- Pipe (33), nitrogen inlet (10) are washed, is opened in first segment liquid inlet (1) and valve d (38), the second finishing reactor monomer A Waste liquid be discharged in filter B (31) from one section of liquid inlet (1) through backwash liquor outlet (34), the second finishing reactor monomer Waste liquid in B is discharged in filter B (31) from backwash liquor entrance (12) through valve d;Finally close backwash liquor entrance (12);It is described Waste liquid in catalyst converter B by filtering after obtain pure ethylene glycol, be stored in ethylene glycol holding vessel;
The backwash liquor is ethylene glycol;
First solid catalyst is KC 108A, KC 108B, KC 108C, any one in KC 108D type catalyst Or two kinds of mixtures being mixed in any proportion;
Second solid catalyst is KC 108A, KC 108B, KC 108C, any two kinds in KC 108D type catalyst Or three kinds of mixtures being mixed in any proportion;
(2) first time removing impurities: it is anti-that the ethylene glycol containing plurality of impurities by ethylene glycol feed pipe (19) has respectively entered the first purification It answers in device A, B, obtains material ethylene glycol after the first solid catalyst absorbs impurity respectively;Liquid outlet is opened respectively, is obtained To ethylene glycol material entered in filter A (25) through outlet A (24), filter A intercept recycling leak out catalyst;
The condition of first time removing impurities are as follows: temperature is 30~60 DEG C, pressure is 0.1~1MPa, material air speed is 3~12h-
(3) second of removing impurities: first segment liquid inlet (1), second segment liquid inlet (8) are opened, through filtering described in step (2) The filtered ethylene glycol material of device A (25) is directed respectively into through outlet B (26) to the second finishing reactor monomer A and B;It passes through respectively It crosses after the second solid catalyst absorbs impurity and obtains ethylene glycol;First segment liquid outlet (5), second segment liquid outlet are opened respectively (11), the ethylene glycol obtained enters filter C (29) through the first liquid outlet tube (27), second liquid outlet (28) respectively In, filter C obtains qualified ethylene glycol after intercepting the catalyst that recycling leaks out, and external second two is imported into through outlet C (30) In alcohol holding vessel;
The condition of second of removing impurities are as follows: temperature is 30~60 DEG C, pressure is 0.1~1MPa, material air speed is 3~12h-
2. the device of plurality of impurities in the removing ethylene glycol in a kind of claim 1 the method, 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:
The ethyl alcohol feed pipe (19), import are connect with the device for the ethylene glycol containing plurality of impurities that outside provides, outlet point For two-way, be connected all the way with the import of backwash tube (33), another way respectively with the first finishing reactor A, the first refining reaction The liquid inlet of device B is connected;First finishing reactor A, the first finishing reactor B liquid outlet pass through outlet A respectively (24) it is connected with the import of filter A (25);The outlet of filter A passes through outlet B (26) and the second finishing reactor Liquid inlet is connected;The liquid outlet of second finishing reactor is connected with the import of filter C (29), and filter C's goes out Mouth is connected by outlet C (30) with external ethylene glycol holding vessel;
The backwash tube (33), import are connected with ethyl alcohol feed pipe or the external device for providing backwash liquor ethylene glycol, export It is connected respectively with the backwash liquor entrance of the first finishing reactor A, the first finishing reactor B, the second finishing reactor, thus will Backwash liquor is directed into each reactor;First finishing reactor A, the first finishing reactor B, the second finishing reactor liquid enter Mouth is also connected with the import of the backwash liquor outlet (34), and backwash liquor is exported from the liquid inlet of each reactor to backwash In liquid outlet;The outlet of backwash liquor outlet is connected with the import of filter B (31), and the outlet of filter B passes through outlet Pipe D (32) is connected with external ethylene glycol holding vessel;
The nitrogen tube (20), import are connected with the external device for providing nitrogen, export respectively with the first finishing reactor A, First finishing reactor B, the second finishing reactor nitrogen inlet be connected.
3. the apparatus of claim 2, it is characterised in that: the first finishing reactor A, the first finishing reactor B structure is identical and is linked together using connection type in parallel: its top offers liquid inlet, and liquid inlet is logical Piping is connected with the outlet of the ethylene glycol feed pipe (19);Its bottom offers nitrogen inlet, backwash liquor entrance And liquid outlet, nitrogen inlet are connected with the outlet of the nitrogen tube (20), backwash liquor entrance with the backwash The outlet of pipe (33) is connected, and liquid outlet is connected with outlet A (24);The backwash liquor entrance also passes through pipeline It is connected with the import of backwash liquor outlet (34);
Second finishing reactor, top be equipped with first segment liquid inlet (1), middle part be equipped with first segment liquid outlet (5), Second segment liquid inlet (8), bottom are equipped with nitrogen inlet (10), second segment liquid outlet (11), backwash liquor entrance (12), In: first segment liquid inlet (1), second segment liquid inlet (8) are connected with the outlet B (26);First segment liquid discharge (5) are connected with the first liquid outlet tube (27) to mouth, second segment liquid outlet (11) is connected with second liquid outlet (28), and the One liquid outlet tube, second liquid outlet are connected with the import of the filter C (29);Nitrogen inlet (10) and institute The outlet for the nitrogen tube (20) stated is connected, and backwash liquor entrance (12) is connected with the outlet of the backwash tube (33);It is described First segment liquid inlet (1) be also connected by pipeline with the import of the backwash liquor outlet (34).
4. device according to claim 3, which is characterized in that the outlet B (26) and second segment liquid inlet (8) Connected branch road is equipped with valve a (35), and valve b (36), the first liquid outlet are equipped on the first liquid outlet tube (27) (5), it is connected with backwash liquor channel I between second segment liquid inlet (8), valve c (37), backwash are installed on the I of backwash liquor channel Liquid entrance (12) is also connected by backwash liquor channel II with the import of filter B (31), is equipped with valve on the II of backwash liquor channel Door d (38).
5. device according to claim 3, which is characterized in that second finishing reactor (23) is by 2 sections of reactors Monomer is constituted, i.e., is made of the second finishing reactor monomer A (231), the second finishing reactor monomer B (232) according to sequence up and down, Structure is as follows:
First segment liquid inlet (1) is offered at the top of the second finishing reactor monomer A, bottom offers first segment liquid It exports (5), body wall top offers first segment solid catalyst loading port (2) and is equipped with first segment visor (3), body wall lower part It offers first segment solid catalyst and unloads agent mouth (4);It is equipped with inside monomer A first segment liquid distribution trough (13), and first segment Liquid distribution trough is located at the top of first segment liquid inlet lower part, first segment visor;First segment filter cap point is installed inside monomer A Fabric swatch (14), and first segment filter cap distribution grid is located at first segment solid catalyst and unloads agent mouth lower part, first segment liquid outlet top; Solid catalyst A (17) are filled in monomer between the first segment visor, first segment filter cap distribution grid;
The second finishing reactor monomer B, the body wall topmost of monomer offer second segment liquid inlet (8), second segment Liquid inlet is connected with inlet tube, and the leakage fluid dram of feed liquor pipe end is located 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 It agent loading port (6) and is equipped with second segment visor (7), body wall lower part offers second segment solid catalyst and unloads agent mouth (9);Monomer It is equipped with inside B second segment liquid distribution trough (15), and second segment liquid distribution trough is located at leakage fluid dram lower part, second segment visor (7) top;Second segment filter cap distribution grid (16) is installed, and second segment filter cap distribution grid is solid positioned at second segment inside monomer B Body catalyst unloads agent mouth (9) lower part, second segment liquid outlet (11) top;The second segment visor, the distribution of second segment filter cap Solid catalyst B (18) are filled in monomer between plate;
The first segment liquid distribution trough (13), second segment liquid distribution trough (15) structure are identical, are calandria or endless tube Formula liquid distribution trough, the screen pipe of liquid distribution trough are wrapping wire screen pipe or the screen pipe for being cased with filter bag;
The first segment filter cap distribution grid (14), second segment filter cap distribution grid (16) structure are identical, are equipped on filter cap distribution grid Several filter caps;The filter cap is wire wrap filter cap or filter bag type filter cap;The connection type of the filter cap and filter cap distribution grid Using threaded connection or locknut connection.
6. device according to claim 5, which is characterized in that constitute two lists of the main body of the second finishing reactor (23) Physical efficiency is split as two independent single layer bed reactor monomers, that is, split be independent the second finishing reactor monomer A (231) and Independent second finishing reactor monomer B (232): the bottom of the second finishing reactor monomer A opens up nitrogen inlet (10) and anti- Wash liquor inlet (12) is connect with the second finishing reactor monomer B using connection type in parallel or in series afterwards.
7. device according to claim 5, which is characterized in that the knot of the first finishing reactor A, the first finishing reactor B Structure is identical as the second finishing reactor monomer A (231), the structure of the second finishing reactor monomer B (232).
8. device according to claim 3, which is characterized in that second finishing reactor (23) is by N sections of reactors Monomer is constituted, 2 N≤10 <;Filling has the solid catalyst of identical or different function, solid catalyst respectively in every section of monomer Type is n, 1 n≤10 <;
The top of reactor monomer described in every section offers liquid inlet, bottom and offers liquid outlet;Body wall top It offers solid catalyst loading port and visor is installed;Body wall lower part offers solid catalyst and unloads agent mouth;It is internal equal Liquid distribution trough is installed, and liquid distribution trough is located at the top of liquid inlet lower part, visor;Inside is equipped with filter cap distribution Plate, and filter cap distribution grid is located at solid catalyst and unloads agent mouth lower part, liquid outlet top;The visor, filter cap distribution grid it Between monomer in be filled with solid catalyst;Final stage monomer, is also provided with nitrogen inlet and backwash other than liquid outlet Liquid entrance;The liquid inlet of every section of monomer is connected with outlet B (26), import phase of the liquid outlet with filter C (29) Connection;Nitrogen inlet is connected with the outlet of nitrogen tube (20), reaction solution entrance is connected with the outlet of backwash tube (33);First The liquid inlet of Duan Danti is also connected with the import of backwash liquor outlet (34);
The liquid distribution trough, is calandria or annular tube type liquid distribution trough, and the screen pipe of liquid distribution trough is wrapping wire filtering Manage or be cased with the screen pipe of filter bag;The filter cap distribution grid, several filter caps are equipped on filter cap distribution grid, and filter cap is that wire wrap is filtered Cap or filter bag type filter cap, filter cap are connect with the connection type of filter cap distribution grid using threaded connection or locknut.
9. device according to claim 8, which is characterized in that constitute N number of monomer of the second finishing reactor (23) main body It can be split as N number of independent single layer bed reactor monomer, 2 N≤10 <;In addition to final stage monomer, the bottom of other monomers is opened If being connect with final stage monomer using connection type in parallel or in series after nitrogen inlet and backwash liquor entrance.
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