CN104211586B - The method of continuous production methylal is realized by the on-line regeneration of catalyzer - Google Patents
The method of continuous production methylal is realized by the on-line regeneration of catalyzer Download PDFInfo
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- CN104211586B CN104211586B CN201410004977.0A CN201410004977A CN104211586B CN 104211586 B CN104211586 B CN 104211586B CN 201410004977 A CN201410004977 A CN 201410004977A CN 104211586 B CN104211586 B CN 104211586B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/48—Preparation of compounds having groups
- C07C41/50—Preparation of compounds having groups by reactions producing groups
- C07C41/56—Preparation of compounds having groups by reactions producing groups by condensation of aldehydes, paraformaldehyde, or ketones
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/009—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in combination with chemical reactions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J38/00—Regeneration or reactivation of catalysts, in general
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J38/00—Regeneration or reactivation of catalysts, in general
- B01J38/48—Liquid treating or treating in liquid phase, e.g. dissolved or suspended
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/48—Preparation of compounds having groups
- C07C41/58—Separation; Purification; Stabilisation; Use of additives
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
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Abstract
The invention provides a kind of method that on-line regeneration by catalyzer realizes continuous production methylal, the method can continuous production methylal while the on-line regeneration carrying out catalyzer.The reactive distillation column with multiple catalyst filling sections is employed in the process of the preparation of described methylal; The on-line regeneration of described catalyzer comprises following four steps of carrying out successively: isolate the catalyst filling section needing to carry out catalyst regeneration and the fluid preparing methylal, to describedly needing the catalyzer carried out in the catalyst filling section of catalyst regeneration to carry out manipulation of regeneration, rinsing and carry out recovery to the described catalyst filling section completing catalyst regeneration come into operation to the catalyst filling section completing catalyst regeneration.Use method provided by the invention, the production efficiency of methylal can be improved, reduce the wastage of material and environmental pollution brought because of parking regenerated catalyst, save manpower and cost.
Description
Technical field
The present invention relates to the preparation of methylal, realize the method for continuous production methylal in particular to a kind of on-line regeneration by catalyzer.
Background technology
In the process preparing methylal, foreign ion in reaction solution can make catalyst deactivation, in prior art, prepare the device used in the method for methylal and there is the reactive distillation column that middle part is provided with catalyst filling, because the catalyst filling in reactive distillation column is an entirety not segmentation, can not separately use, even if or segmentation can not be separated mutually, so when catalyst deactivation, need to carry out manipulation of regeneration with catalyst treatment agent to all catalyzer under dead ship condition, after completing the manipulation of regeneration of catalyzer, need to restart the program preparing methylal.
Use above-mentioned method of the prior art to prepare methylal, will the whole system preparing methylal be stopped when catalyzer needs to carry out manipulation of regeneration, regenerate and again start.Because each parking and again starter gear all can cause stopping production and environmental pollution, therefore there is the problems such as production efficiency is low, and cost is high, environmental pollution.
Therefore, need to transform the existing method preparing methylal, it can be solved the problem.
Summary of the invention
The object of the application is to provide a kind of on-line regeneration by catalyzer to realize the method for continuous production methylal, to solve the above problems.
The application provides a kind of on-line regeneration by catalyzer to realize the method for continuous production methylal, and the method is carrying out the on-line regeneration process carrying out catalyzer while prepared by methylal; The reactive distillation column 1 with multiple catalyst filling section 3 is employed in the process of the preparation of described methylal; The on-line regeneration process of described catalyzer comprises following four steps of carrying out successively: (a) isolates with the fluid preparing methylal the catalyst filling section needing to carry out catalyst regeneration process; B () carries out manipulation of regeneration to the described catalyzer carried out in the catalyst filling section of catalyst regeneration process that needs; C () rinses the catalyst filling section completing catalyst regeneration process; D () is carried out recovery to the described catalyst filling section completing catalyst regeneration process and is come into operation.
Optionally, the preparation of described methylal comprises the following steps:
E multiple catalyst filling sections 3 that () raw material reaction liquid enters in reactive distillation column 1 after pre-reaction carry out catalyzed reaction, enter into the bottom liquid section 4 of reactive distillation column after completing catalyzed reaction;
F the reaction solution of () bottom liquid section 4 enters into reboiler 10 by described reactive distillation column 1, the multiple catalyst filling sections 3 again entered after heating and gasifying in described reactive distillation column 1 carry out catalyzed reaction, enter into the top gas section 2 of reactive distillation column after completing catalyzed reaction;
G the gas of () top gas section 2 enters into condenser 8 by described reactive distillation column 1, enter phlegma storage tank 9 after condensation liquefaction;
H () phlegma is got back to the multiple catalyst filling sections 3 again entered in described reactive distillation column 1 after feedstock pipeline 70 mixes with raw material reaction liquid by described phlegma storage tank 9 and is carried out catalyzed reaction;
I () iterative cycles step (e)-(h), according to reacting the situation of carrying out, exports from phlegma feed back the material that 91 extraction contain product methylal.
Optionally, the described multiple catalyst filling sections 3 in described reactive distillation column 1 comprise 2-10 section catalyst filling section, and the longitudinal direction along described reactive distillation column 1 from top to bottom sets gradually.
According to the method that the application provides, step (a) comprises liquid isolation and gas barrier, and the isolation of described liquid and described gas barrier are carried out simultaneously; The isolation of described liquid and described gas barrier be by gently close need to carry out the catalyst filling section correspondence of catalyst regeneration process raw material discharging bifurcations, reaction material feed back bifurcations, gas feed bifurcations and gas discharge bifurcations on valve or valve group realization.
Described liquid has isolated rear raw material reaction liquid from except other at least one catalyst filling section feeding of the described catalyst filling section needing to carry out catalyst regeneration process, preferably from the catalyst filling section feeding of the superiors or the second layer; The catalyst filling section that after described gas barrier completes, gas enters above except the described catalyst filling section needing to carry out catalyst regeneration process carries out catalyzed reaction, preferably enter an adjacent catalyst filling section above and carry out catalyzed reaction, or enter top gas section until enter condenser.
Step (b) comprises the following steps: catalyst treatment agent from catalyst treatment agent storage tank through catalyst treatment agent feeding pipe arrive the described catalyst filling section of carrying out catalyst regeneration process that needs manipulation of regeneration is carried out to catalyzer, complete the catalyst treatment agent after manipulation of regeneration through catalyst treatment agent recycling pipeline enter into catalyst treatment agent reclaim storage tank reclaim.
Step (c) comprises the following steps of carrying out successively:
P () closes the valve that valve that described catalyst treatment agent storage tank and catalyst treatment agent reclaim storage tank opens irrigation storage tank and waste liquid tank simultaneously;
The catalyst filling section completing catalyst regeneration process q () irrigation to arrive from described irrigation storage tank through described catalyst treatment agent feeding pipe described in is rinsed, and completes the waste liquid after flushing and enters waste liquid tank through described catalyst treatment agent recycling pipeline.
Step (d) comprises the following steps of carrying out successively:
R () stops completing the flushing after catalyst regeneration process;
S () has made the catalyst filling section of catalyst regeneration process recover to come into operation.
Preferably, described step (r) is valve by closing irrigation storage tank and the valve completed described in simultaneously gently closing on the catalyst treatment agent discharging bifurcations of the catalyst filling section correspondence of catalyst regeneration process, the branch inlet of liquid inlet opening and the branch outlet of liquid outlet opening or valve group realize.
Preferably, described step (s) is that valve in raw material discharging bifurcations, reaction material feed back bifurcations, gas feed bifurcations and gas discharge bifurcations by completing the catalyst filling section correspondence of catalyst regeneration process described in gently opening or valve group realize.
A kind of on-line regeneration by catalyzer using the application to provide realizes the method for continuous production methylal, following beneficial effect can be brought: do not need when carrying out on-line regeneration process to catalyzer to stop production to whole device, continuous seepage can be carried out for a long time, reducing the wastage of material and environmental pollution brought because stopping more catalyst changeout, saving manpower and cost.
Accompanying drawing explanation
A kind of schematic diagram (gas distributor, liquid distributor are not shown) preparing the reactive distillation column of methylal that Fig. 1 provides for the embodiment of the present application;
The schematic diagram (illustrating that label is different from Fig. 1) that Fig. 2 is the reactive distillation column shown in Fig. 1;
A kind of schematic diagram (gas distributor, liquid distributor are shown) preparing the reactive distillation column of methylal that Fig. 3 provides for the embodiment of the present application;
The sectional view of a kind of gas distributor that Fig. 4 provides for the embodiment of the present application;
The schematic diagram (not shown gear liquid parts) of a kind of gas distributor vertical view that Fig. 5 provides for the embodiment of the present application;
A kind of schematic diagram (feedstock pipeline, catalyst treatment agent feeding pipe, gas feed back discharging pipeline and catalyst treatment agent recycling pipeline are shown) preparing the reactive distillation column of methylal that Fig. 6 provides for the embodiment of the present application;
A kind of operation chart (when not needing to process catalyzer operational scheme) preparing the device of methylal that Fig. 7 provides for the embodiment of the present application;
A kind of operation chart (during process first paragraph catalyst filling section operational scheme) preparing the device of methylal that Fig. 8 provides for the embodiment of the present application;
A kind of operation chart (during process second segment catalyst filling section operational scheme) preparing the device of methylal that Fig. 9 provides for the embodiment of the present application;
A kind of operation chart (during process the 3rd section of catalyst filling section operational scheme) preparing the device of methylal that Figure 10 provides for the embodiment of the present application;
A kind of schematic diagram preparing the device of methylal that Figure 11 provides for the embodiment of the present application;
A kind of schematic diagram (reaction surge tank is shown) preparing the device of methylal that Figure 12 provides for the embodiment of the present application.
Embodiment
Below in conjunction with drawings and Examples, the application is described in further detail.Be understandable that, specific embodiment described herein is only for explaining the application, but not the restriction to the application.
A kind of schematic diagram (gas distributor, liquid distributor are not shown) preparing the reactive distillation column of methylal that Fig. 1 provides for the embodiment of the present application.
Reactive distillation column as shown in Figure 1, comprises internal space independently multiple catalyst filling section 3 at top gas section 2, middle part and bottom liquid section 4; Top gas section 2 is provided with top gas outlet 21 and top gas feedback outlet 22, and bottom liquid section 4 is provided with liquid inlet 41, bottom liquid outlet 42 and bottom gas outlet 43; Multiple catalyst filling section 3 is made up of 3 catalyst filling sections 31,32,33, and catalyst filling section 31,32,33 is arranged in series along described reactive distillation column longitudinal direction; This 3 catalyst filling sections 31,32,33 separate and by feed liquor outlet gas part 311,321,331, catalyst filling layer segment 312,322,332, air inlet dispensing parts 313,323,333 forms, catalyst filling layer segment 312,322,332 is provided with catalyzer and in described feed liquor outlet gas part 311, between 321,331 and air inlet dispensing parts 313,323,333.
The number of packing section can change.In an interchangeable embodiment, middle part multiple catalyst filling sections 3 can be separate comprise 2,3,4,5,6,7,8,9 or 10 sections of catalyst filling sections, and from top to bottom set gradually along the longitudinal direction of described reactive distillation column 1, in the application, each packing section can fluid isolation mutually, and namely the packing section of a certain section can carry out gas with adjacent packing section and liquid is isolated.Packing section after isolation can carry out catalyzer on-line regeneration when normally working for other sections.
The schematic diagram (illustrating that label is different from Fig. 1) that Fig. 2 is the reactive distillation column shown in Fig. 1.Reactive distillation column as shown in Figure 1-2, wherein, feed liquor outlet gas part 311,321,331 is provided with liquid inlet opening 3111,3211,3311 and gas discharge port 3112,3212,3312, and air inlet dispensing parts 313,323,333 is provided with gas feedback outlet 3131,3231,3331 and liquid outlet opening 3132,3232,3332.
Reactive distillation column shown in Fig. 1 and Fig. 2 is identical reactive distillation column, only because the label needed is too much, when being placed on same accompanying drawing, drawing reference numeral can be caused crowded, reads complicated chaotic, therefore is divided into two accompanying drawings to illustrate.
A kind of schematic diagram (gas distributor, liquid distributor are shown) preparing the reactive distillation column of methylal that Fig. 3 provides for the embodiment of the present application.
Reactive distillation column (parts numbers is with reference to Fig. 1-2) as shown in Figure 3, be provided with liquid distributor 3113 in feed liquor outlet gas part 311, liquid distributor 3113 is connected with liquid inlet opening 3111; Be provided with liquid distributor 3213 in feed liquor outlet gas part 321, liquid distributor 3213 is connected with liquid inlet opening 3211; Be provided with liquid distributor 3313 in feed liquor outlet gas part 331, liquid distributor 3313 is connected with liquid inlet opening 3311.Be provided with gas distributor 3133 in air inlet dispensing parts 313, gas distributor 3133 is connected with gas feedback outlet 3131; Be provided with gas distributor 3233 in air inlet dispensing parts 323, gas distributor 3233 is connected with gas feedback outlet 3231; Be provided with gas distributor 3333 in air inlet dispensing parts 333, gas distributor 3333 is connected with gas feedback outlet 3331.
The sectional view of a kind of gas distributor that Fig. 4 provides for the embodiment of the present application.Gas distributor as shown in Figure 4, is provided with material outlet 5, and this material outlet, higher than the bottom gas distribution channel of gas distributor, material outlet 5 is provided with gear liquid parts 6.
The schematic diagram (not shown gear liquid parts) of a kind of gas distributor vertical view that Fig. 5 provides for the embodiment of the present application.Gas distributor as shown in Figure 5, rounded generally, material outlet 5 is evenly distributed on gas distributor, Fig. 5 not shown gear liquid parts.
Gas is delivered to material outlet 5 from the gas pipe line of gas distributor, due to being uniformly distributed of material outlet 5, gas can be made to distribute at air inlet dispensing parts 313,323,333 rapidly and uniformly, be conducive to reactant gases and fully contact with catalyzer, homogeneous reaction.
Liquid distributor is also evenly provided with liquid material outlet, for spraying reaction solution to catalyst filling layer uniformly.
The reaction solution sprayed out from liquid distributor is after the reaction of catalyst filling layer, enter air inlet dispensing parts 313,323,333, the gear liquid parts be now arranged on material outlet 5 stop reaction solution to enter gas distributor and pipeline thereof, to avoid liquid and flow backwards in gas feed back discharging pipeline 72.
The diameter of gas distributor is more smaller than the diameter of reactive distillation column, after when the liquid got off from catalyst filling laminar flow drops on gas distributor, liquid flows into below along the gap of gas distributor and tower body, and exports through liquid outlet opening 3132,3232,3332.In order to ensure the normal operation of reactive distillation column, can with air inlet dispensing parts 313,323,333 corresponding positions arrange fluid level controller, to control the liquid level of this part.
The form of liquid distributor 3113,3213,3313 and gas distributor 3133,3233,3333 can be diversified, be not limited to the scheme that the embodiment of the present application provides, the parts that those skilled in that art think can realize gas, uniform liquid distributes, all can be used for the liquid distributor described in alternative the application and gas distributor.
A kind of schematic diagram (feedstock pipeline, catalyst treatment agent feeding pipe, gas feed back discharging pipeline and catalyst treatment agent recycling pipeline are shown) preparing the reactive distillation column of methylal that Fig. 6 provides for the embodiment of the present application.Reactive distillation column shown in Fig. 6, is also provided with feedstock pipeline 70, catalyst treatment agent feeding pipe 71, gas feed back discharging pipeline 72 and catalyst treatment agent recycling pipeline 73.Be below concrete mode of connection (parts numbers is with reference to Fig. 2 and Figure 11):
Feedstock pipeline 70 is provided with 3 raw material discharging bifurcations, 701,702,703 and 3 reaction material feed back bifurcations 704,705,706, raw material discharging bifurcations 701,702,703 and liquid inlet opening 3111,3211,3311 correspondingly connect, and namely 701 to be connected with 3111,702 to be connected with 3211,703 to be connected with 3311; Reaction material feed back bifurcations 704,705,706 and liquid outlet opening 3132,3232,3332 correspondingly connect, and namely 704 to be connected with 3132,705 to be connected with 3232,706 to be connected with 3332.
Catalyst treatment agent feeding pipe 71 is provided with 3 catalyst treatment agent discharging bifurcations 711,712,713, the branch inlet 707 of catalyst treatment agent discharging bifurcations 711,712,713 and liquid inlet opening, 708,709 correspondingly connects, and namely 711 to be connected with 707,712 to be connected with 708,713 to be connected with 709.
Gas feed back discharging pipeline 72 is provided with 3 gas feed bifurcations, 721,722,723 and 3 gas discharge bifurcations 724,725,726, gas feed bifurcations 721,722,723 and gas feedback outlet 3131,3231,3331 correspondingly connect, and namely 721 to be connected with 3131,722 to be connected with 3231,723 to be connected with 3331; Gas discharge bifurcations 724,725,726 and gas discharge mouth 3112,3212,3312 correspondingly connect, and namely 724 to be connected with 3112,725 to be connected with 3212,726 to be connected with 3312.
Catalyst treatment agent recycling pipeline 73 is provided with 3 and reclaims bifurcations 731,732,733, reclaim the branch outlet 7100 of bifurcations 731,732,733 and liquid outlet opening, 7101,7102 correspondingly to connect, namely 731 to be connected with 7100,732 to be connected with 7101,733 to be connected with 7102.(label is see Figure 11)
Raw material discharging bifurcations 701,702,703, reaction material feed back bifurcations 704,705,706, catalyst treatment agent discharging bifurcations 711,712,713, the branch inlet of liquid inlet opening 707,708,709, the branch outlet of liquid outlet opening 7100,7101,7102, gas feed bifurcations 721,722,723 and gas discharge bifurcations 724,725,726 be provided with T-valve or valve group.By controlling T-valve or valve group, the direction of liquid or gas conveying can be controlled, to reach segmentation convey materials, the object of online disposal without shutting down decaying catalyst.
A kind of operation chart (when not needing to process catalyzer operational scheme) preparing the device of methylal that Fig. 7 provides for the embodiment of the present application.The device preparing methylal as shown in Figure 7, top gas outlet 21 is connected with a condenser 8, the outlet of condenser 8 is connected with a phlegma storage tank 9, phlegma storage tank 9 is provided with products export 91 and phlegma feed back outlet 92, phlegma feed back outlet 92 is connected with feedstock pipeline 70, is connected on the pipeline before first raw material discharging bifurcations 701; Liquid inlet 41 is connected with last reaction material feed back bifurcations 706; Bottom liquid outlet 42 is connected with a reboiler 10, and the outlet of reboiler 10 is connected with first gas feed bifurcations 721; Bottom gas outlet 43 is connected on the pipeline 44 between the outlet of reboiler 10 and first gas feed bifurcations 721.
Shown in Fig. 7 is when not needing to carry out decaying catalyst process regeneration, and the operation scheme of device is specific as follows:
Material benzenemethanol and formaldehyde are under feedstock pipeline 70 is carried, through raw material discharging bifurcations 701, after liquid inlet opening 3111, evenly spray to catalyst filling layer segment 312 under the distribution effect of liquid distributor 3113, air inlet dispensing parts is entered after catalyst filling layer segment 312 reacts, through liquid outlet opening 3132, reaction material feed back bifurcations 704, raw material discharging bifurcations 702, liquid inlet opening 3211 enters liquid distributor 3213 and evenly sprays to catalyst filling layer segment 322, air inlet dispensing parts is entered after catalyst filling layer segment 322 reacts, through liquid outlet opening 3232, reaction material feed back bifurcations 705, raw material discharging bifurcations 703, liquid inlet opening 3311 enters liquid distributor 3313 and evenly sprays to catalyst filling layer segment 332, air inlet dispensing parts is entered after catalyst filling layer segment 332 reacts, through liquid outlet opening 3332, reaction material feed back bifurcations 706, liquid inlet 41 enters bottom liquid section 4.
Reaction solution enters into reboiler 10 through bottom liquid outlet 42, reaction solution exports gas feed back discharging pipeline 72 in reboiler 10 after heating and gasifying, gas enters gas distributor 3333 through gas feedback outlet 3331, under the effect of gas distributor 3333, after catalyst filling layer segment 332 reacts, through gas discharge mouth 3312, gas discharge bifurcations 724, gas feed bifurcations 722, gas feedback outlet 3231 enters gas distributor 3233, under the effect of gas distributor 3233, after catalyst filling layer segment 322 reacts, through gas discharge mouth 3212, gas discharge bifurcations 725, gas feed bifurcations 723, gas feedback outlet 3131 enters gas distributor 3133, under the effect of gas distributor 3133, after catalyst filling layer segment 312 reacts, through gas discharge mouth 3112, gas discharge bifurcations 726, top gas feedback outlet 22 enters top gas section.
Gas enters condenser 8 through top gas outlet 21, and gas is after condenser 8 condensation, and phlegma enters phlegma storage tank 9, then gets back on the pipeline before the raw material discharging bifurcations 701 of feedstock pipeline 70 through phlegma feed back outlet 92.
Phlegma reenters reactive distillation column with raw material mixed solution and carries out circulating reaction.After reaction for some time, product exports from products export 91.
This application provides a kind of method that on-line regeneration by catalyzer realizes continuous production methylal, the method is carrying out the on-line regeneration process carrying out catalyzer while prepared by methylal; The reactive distillation column 1 with multiple catalyst filling section 3 is employed in the process of the preparation of methylal; The on-line regeneration process of catalyzer comprises following four steps of carrying out successively: (a) isolates with the fluid preparing methylal the catalyst filling section needing to carry out catalyst regeneration process; B () carries out manipulation of regeneration to the described catalyzer carried out in the catalyst filling section of catalyst regeneration process that needs; C () rinses the catalyst filling section completing catalyst regeneration process; D () is carried out recovery to the described catalyst filling section completing catalyst regeneration process and is come into operation.
The wherein preparation of methylal and prior art basic simlarity, the reactive distillation column 1 just used in the application comprises multiple isolable catalyst filling section 3.The operation preparing methylal can with reference to the technology and condition of prior art.
Step (a) comprises liquid isolation and gas barrier, and the isolation of described liquid and described gas barrier are carried out simultaneously; The isolation of described liquid and described gas barrier be by gently close need to carry out the catalyst filling section correspondence of catalyst regeneration process raw material discharging bifurcations, reaction material feed back bifurcations, gas feed bifurcations and gas discharge bifurcations on valve or valve group realization.
In this specification sheets, all relating to, closes or all referring to of the valve opened in bifurcations or valve group is undertaken by the operation of the T-valve in bifurcations or valve group, and sometimes to close or open valve be by valve transfer thus change the flow direction preparing methylal fluid.Such as, close the valve in raw material discharging bifurcations 701, direction feedstock pipeline 70 being communicated with liquid inlet opening 3111 switches to feedstock pipeline 70 and is communicated with the direction of liquid inlet opening 3211 thus makes the fluid preparing methylal avoid catalyst filling section 31 to flow to other catalyst filling sections.
Liquid has isolated rear raw material reaction liquid at least one catalyst filling section feeding from other except the described catalyst filling section needing to carry out catalyst regeneration process, preferably from the catalyst filling section feeding of the superiors or the second layer; The catalyst filling section that after described gas barrier completes, gas enters above except the described catalyst filling section needing to carry out catalyst regeneration process carries out catalyzed reaction, preferably enter an adjacent catalyst filling section above and carry out catalyzed reaction, or enter top gas section 2 until enter condenser 8.It is steady that the process need of isolating notices that maintenance operates.Excessive if fluctuated, can temporary close products export, question response to reach steadily output products again.
Step (b) comprises the following steps: catalyst treatment agent arrives the described catalyst filling section of carrying out catalyst regeneration process that needs from catalyst treatment agent storage tank 16 through catalyst treatment agent feeding pipe 71 and carries out manipulation of regeneration to catalyzer, complete the catalyst treatment agent after manipulation of regeneration through catalyst treatment agent recycling pipeline 73 enter into catalyst treatment agent reclaim storage tank 17 reclaim.
Step (c) comprises the following steps of carrying out successively: (p) closes the valve that valve that catalyst treatment agent storage tank 16 and catalyst treatment agent reclaim storage tank 17 opens irrigation storage tank 19 and waste liquid tank 20 simultaneously; The catalyst filling section completing catalyst regeneration process q () irrigation to arrive from described irrigation storage tank 19 through described catalyst treatment agent feeding pipe 71 described in is rinsed, and completes the waste liquid after flushing and enters waste liquid tank 20 through described catalyst treatment agent recycling pipeline 73.
Step (d) comprises the following steps of carrying out successively: (r) stops completing the flushing after catalyst regeneration process; S () has made the catalyst filling section of catalyst regeneration process recover to come into operation.Wherein, step (r) is valve by closing irrigation storage tank 19 and the valve completed described in simultaneously gently closing on the catalyst treatment agent discharging bifurcations of the catalyst filling section correspondence of catalyst regeneration process, the branch inlet of liquid inlet opening and the branch outlet of liquid outlet opening or valve group realize.And step (s) to be valve in raw material discharging bifurcations, reaction material feed back bifurcations, gas feed bifurcations and gas discharge bifurcations by completing the catalyst filling section correspondence of catalyst regeneration process described in gently opening or valve group realize.In simple terms, recover to come into operation exactly corresponding catalyst filling section to be returned to original operational stage.It is steady that the process need recovered notices that maintenance operates, if desired also can temporary close products export.
A kind of operation chart (during process first paragraph catalyst filling section operational scheme) preparing the device of methylal that Fig. 8 provides for the embodiment of the present application.The device preparing methylal is as shown in Figure 8 the schematic flow sheet preparing the plant running of methylal while catalyst filling layer in catalyst filling section 31 carries out on-line regeneration process.Its carrying out practically mode is as follows:
Material benzenemethanol and formaldehyde are under feedstock pipeline 70 is carried, through raw material discharging bifurcations 701, reaction material feed back bifurcations 704, raw material discharging bifurcations 702, liquid inlet opening 3211 enters liquid distributor 3213 and evenly sprays to catalyst filling layer segment 322, air inlet dispensing parts is entered after catalyst filling layer segment 322 reacts, through liquid outlet opening 3232, reaction material feed back bifurcations 705, raw material discharging bifurcations 703, liquid inlet opening 3311 enters liquid distributor 3313 and evenly sprays to catalyst filling layer segment 332, air inlet dispensing parts is entered after catalyst filling layer segment 332 reacts, through liquid outlet opening 3332, reaction material feed back bifurcations 706, liquid inlet 41 enters bottom liquid section 4.
Reaction solution enters into reboiler 10 through bottom liquid outlet 42, reaction solution exports gas feed back discharging pipeline 72 in reboiler 10 after heating and gasifying, gas enters gas distributor 3333 through gas feedback outlet 3331, under the effect of gas distributor 3333, after catalyst filling layer segment 332 reacts, through gas discharge mouth 3312, gas discharge bifurcations 724, gas feed bifurcations 722, gas feedback outlet 3231 enters gas distributor 3233, under the effect of gas distributor 3233, after catalyst filling layer segment 322 reacts, through gas discharge mouth 3212, gas discharge bifurcations 725, gas feed bifurcations 723, gas discharge bifurcations 726, top gas feedback outlet 22 enters top gas section 2.
Gas enters condenser 8 through top gas outlet 21, and gas is after condenser 8 condensation, and phlegma enters phlegma storage tank 9, then gets back on the pipeline before the raw material discharging bifurcations 701 of feedstock pipeline 70 through phlegma feed back outlet 92.
Preparing methylal and carrying out simultaneously the idiographic flow following (with reference to Figure 11 or 12) of catalyzer on-line regeneration:
Isolate with other parts (comprising other catalyst filling sections) fluid of the device preparing methylal the catalyst filling section 31 needing to carry out catalyst regeneration process, this comprises and carries out liquid isolation and gas barrier simultaneously; Liquid isolation and gas barrier are by gently closing valve in raw material discharging bifurcations 701, reaction material feed back bifurcations 704, gas feed bifurcations 723 and gas discharge bifurcations 726 or the realization of valve group.
Catalyst treatment agent from catalyst treatment agent storage tank 16 catalyst treatment agent feeding pipe 71 conveying, after the branch inlet 707, liquid inlet opening 3111 of catalyst treatment agent discharging bifurcations 711, liquid inlet opening, under the distribution effect of liquid distributor 3113, evenly spray, to catalyst filling layer segment 312, carries out manipulation of regeneration to catalyst filling layer segment 312.Complete the catalyst treatment agent after manipulation of regeneration through liquid outlet opening 3132, liquid outlet opening branch outlet 7100, reclaim bifurcations 731 export, through catalyst treatment agent recycling pipeline 73 enter into catalyst treatment agent reclaim storage tank 17 reclaim.
The valve of closing catalyst treatment agent storage tank 16 and catalyst treatment agent recovery storage tank 17 opens the valve of irrigation storage tank 19 and waste liquid tank 20 simultaneously, irrigation from irrigation storage tank 19 catalyst treatment agent feeding pipe 71 conveying, after the branch inlet 707, liquid inlet opening 3111 of catalyst treatment agent discharging bifurcations 711, liquid inlet opening, under the distribution effect of liquid distributor 3113, evenly spray, to catalyst filling layer segment 312, rinses catalyst filling layer segment 312.Complete the waste liquid after flushing through liquid outlet opening 3132, liquid outlet opening branch outlet 7100, reclaim bifurcations 731 export, enter waste liquid tank 20.
Closing the valve of irrigation storage tank 19 and the valve of simultaneously gently closing on catalyst treatment agent discharging bifurcations 711, the branch inlet 707 of liquid inlet opening and the branch outlet 7100 of liquid outlet opening or valve group, stopping completing the flushing after catalyst regeneration process.Gently open valve in raw material discharging bifurcations 701, reaction material feed back bifurcations 704, gas feed bifurcations 723 and gas discharge bifurcations 726 or valve group has made the catalyst filling section 31 of catalyst regeneration process recover to come into operation.
When isolating packing section and recovering to come into operation, the operation of whole tower there will be fluctuation, so want slowly to the influential operation of molecular balance (such as opening or closing) generally, avoid the balance destroying reaction, the operational condition of tower can be adjusted if desired, such as reduce or increase the load of tower, adjustment temperature or pressure.The operation little to the balance influence of reaction can be carried out fast.
The on-line regeneration of catalyzer can be realized like this, avoid whole device drive frequently and stop, improve the cycle of operation of device, and the waste decreased because start-stop car causes and environmental pollution.The catalyst regeneration of other sections and the operation of first paragraph substantially similar, after have detailed description.
A kind of operation chart (during process second segment catalyst filling section operational scheme) preparing the device of methylal that Fig. 9 provides for the embodiment of the present application.The device preparing methylal is as shown in Figure 9 the schematic flow sheet preparing the plant running of methylal while catalyst filling layer in catalyst filling section 32 carries out on-line regeneration process.Its carrying out practically mode is as follows:
Material benzenemethanol and formaldehyde are under feedstock pipeline 70 is carried, through raw material discharging bifurcations 701, liquid inlet opening 3111 enters liquid distributor 3113 and evenly sprays to catalyst filling layer segment 312, air inlet dispensing parts is entered after catalyst filling layer segment 312 reacts, through liquid outlet opening 3132, reaction material feed back bifurcations 704, raw material discharging bifurcations 702, reaction material feed back bifurcations 705, raw material discharging bifurcations 703, liquid inlet opening 3311 enters liquid distributor 3313 and evenly sprays to catalyst filling layer segment 332, air inlet dispensing parts is entered after catalyst filling layer segment 332 reacts, through liquid outlet opening 3332, reaction material feed back bifurcations 706, liquid inlet 41 enters bottom liquid section 4.
Reaction solution enters into reboiler 10 through bottom liquid outlet 42, reaction solution exports gas feed back discharging pipeline 72 in reboiler 10 after heating and gasifying, gas enters gas distributor 3333 through gas feedback outlet 3331, under the effect of gas distributor 3333, after catalyst filling layer segment 332 reacts, through gas discharge mouth 3312, gas discharge bifurcations 724, gas feed bifurcations 722, gas discharge bifurcations 725, gas feed bifurcations 723, gas feedback outlet 3131 enters gas distributor 3133, under the effect of gas distributor 3133, after catalyst filling layer segment 312 reacts, through gas discharge mouth 3112, gas discharge bifurcations 726, top gas feedback outlet 22 enters top gas section 2.
Gas enters condenser 8 through top gas outlet 21, and gas is after condenser 8 condensation, and phlegma enters phlegma storage tank 9, then gets back on the pipeline before the raw material discharging bifurcations 701 of feedstock pipeline 70 through phlegma feed back outlet 92.
Following with the idiographic flow of the on-line regeneration process preparing the catalyzer that methylal carries out simultaneously (with reference to Figure 11 or 12):
To needing the catalyst filling section 32 of carrying out catalyst regeneration process to isolate with other parts (comprising other catalyst filling sections) fluid of the device preparing methylal, this comprises the liquid isolation and gas barrier carried out simultaneously; Liquid isolation and gas barrier are by gently closing valve in raw material discharging bifurcations 702, reaction material feed back bifurcations 705, gas feed bifurcations 722 and gas discharge bifurcations 725 or the realization of valve group.
Catalyst treatment agent from catalyst treatment agent storage tank 16 catalyst treatment agent feeding pipe 71 conveying, after the branch inlet 708, liquid inlet opening 3211 of catalyst treatment agent discharging bifurcations 712, liquid inlet opening, under the distribution effect of liquid distributor 3213, evenly spray, to catalyst filling layer segment 322, carries out manipulation of regeneration to catalyst filling layer segment 322.After completing manipulation of regeneration remaining catalyst treatment agent through liquid outlet opening 3232, liquid outlet opening branch outlet 7101, reclaim bifurcations 732 export, through catalyst treatment agent recycling pipeline 73 enter into catalyst treatment agent reclaim storage tank 17 reclaim.
The valve of closing catalyst treatment agent storage tank 16 and catalyst treatment agent recovery storage tank 17 opens the valve of irrigation storage tank 19 and waste liquid tank 20 simultaneously, irrigation from irrigation storage tank 19 catalyst treatment agent feeding pipe 71 conveying, after the branch inlet 708, liquid inlet opening 3211 of catalyst treatment agent discharging bifurcations 712, liquid inlet opening, under the distribution effect of liquid distributor 3213, evenly spray, to catalyst filling layer segment 322, rinses catalyst filling layer segment 322.Complete the waste liquid after flushing through liquid outlet opening 3232, liquid outlet opening branch outlet 7101, reclaim bifurcations 732 export, enter waste liquid tank 20.
Closing the valve of irrigation storage tank 19 and the valve of simultaneously gently closing on catalyst treatment agent discharging bifurcations 712, the branch inlet 708 of liquid inlet opening and the branch outlet 7101 of liquid outlet opening or valve group, stopping completing the flushing after catalyst regeneration process; Gently open valve in raw material discharging bifurcations 702, reaction material feed back bifurcations 705, gas feed bifurcations 722 and gas discharge bifurcations 725 or valve group has made the catalyst filling section 32 of catalyst regeneration process recover to come into operation.
A kind of operation chart (during process the 3rd section of catalyst filling section operational scheme) preparing the device of methylal that Figure 10 provides for the embodiment of the present application.The device preparing methylal is as shown in Figure 10 the schematic flow sheet preparing the plant running of methylal while catalyst filling layer in catalyst filling section 33 carries out on-line regeneration process.Its carrying out practically mode is as follows:
Material benzenemethanol and formaldehyde are under feedstock pipeline 70 is carried, through raw material discharging bifurcations 701, liquid inlet opening 3111 enters liquid distributor 3113 and evenly sprays to catalyst filling layer segment 312, air inlet dispensing parts is entered after catalyst filling layer segment 312 reacts, through liquid outlet opening 3132, reaction material feed back bifurcations 704, raw material discharging bifurcations 702, liquid inlet opening 3211 enters liquid distributor 3213 and evenly sprays to catalyst filling layer segment 322, air inlet dispensing parts is entered after catalyst filling layer segment 322 reacts, through liquid outlet opening 3232, reaction material feed back bifurcations 705, raw material discharging bifurcations 703, reaction material feed back bifurcations 706, liquid inlet 41 enters bottom liquid section 4.
Reaction solution enters into reboiler 10 through bottom liquid outlet 42, reaction solution exports gas feed back discharging pipeline 72 to after heating and gasifying is converted into gas in reboiler 10, gas is through gas feed bifurcations 721, gas discharge bifurcations 724, gas feed bifurcations 722, gas feedback outlet 3231 enters gas distributor 3233, under the effect of gas distributor 3233, after catalyst filling layer segment 322 reacts, through gas discharge mouth 3212, gas discharge bifurcations 725, gas feed bifurcations 723, gas feedback outlet 3131 enters gas distributor 3133, under the effect of gas distributor 3133, after catalyst filling layer segment 312 reacts, through gas discharge mouth 3112, gas discharge bifurcations 726, top gas feedback outlet 22 enters top gas section 2.
Gas enters condenser 8 through top gas outlet 21, and gas is after condenser 8 condensation, and phlegma enters phlegma storage tank 9, then gets back on the pipeline before the raw material discharging bifurcations 701 of feedstock pipeline 70 through phlegma feed back outlet 92.
Following with the idiographic flow of the on-line regeneration process preparing the catalyzer that methylal carries out simultaneously (with reference to Figure 11 or 12):
To needing the catalyst filling section 33 of carrying out catalyst regeneration process to isolate with other parts (comprising other catalyst filling sections) fluid of the device preparing methylal, this comprises the liquid isolation and gas barrier carried out simultaneously; Liquid isolation and gas barrier are by gently closing valve in raw material discharging bifurcations 703, reaction material feed back bifurcations 706, gas feed bifurcations 721 and gas discharge bifurcations 724 or the realization of valve group.
Catalyst treatment agent from catalyst treatment agent storage tank 16 catalyst treatment agent feeding pipe 71 conveying, after the branch inlet 709, liquid inlet opening 3311 of catalyst treatment agent discharging bifurcations 713, liquid inlet opening, under the distribution effect of liquid distributor 3313, evenly spray, to catalyst filling layer segment 332, carries out manipulation of regeneration to catalyst filling layer segment 332.After completing manipulation of regeneration remaining catalyst treatment agent through liquid outlet opening 3332, liquid outlet opening branch outlet 7102, reclaim bifurcations 733 export, through catalyst treatment agent recycling pipeline 73 enter into catalyst treatment agent reclaim storage tank 17 reclaim.
The valve of closing catalyst treatment agent storage tank 16 and catalyst treatment agent recovery storage tank 17 opens the valve of irrigation storage tank 19 and waste liquid tank 20 simultaneously, irrigation from irrigation storage tank 19 catalyst treatment agent feeding pipe 71 conveying, after the branch inlet 709, liquid inlet opening 3311 of catalyst treatment agent discharging bifurcations 713, liquid inlet opening, under the distribution effect of liquid distributor 3313, evenly spray, to catalyst filling layer segment 332, rinses catalyst filling layer segment 332.Complete the waste liquid after flushing through liquid outlet opening 3332, liquid outlet opening branch outlet 7102, reclaim bifurcations 733 export, enter waste liquid tank 20.
Closing the valve of irrigation storage tank 19 and the valve of simultaneously gently closing on catalyst treatment agent discharging bifurcations 713, the branch inlet 709 of liquid inlet opening and the branch outlet 7102 of liquid outlet opening or valve group, stopping completing the flushing after catalyst regeneration process; Gently open valve in raw material discharging bifurcations 703, reaction material feed back bifurcations 706, gas feed bifurcations 721 and gas discharge bifurcations 724 or valve group has made the catalyst filling section 33 of catalyst regeneration process recover to come into operation.
A kind of schematic diagram preparing the device of methylal that Figure 11 provides for the embodiment of the present application.The device preparing methylal as shown in figure 11, also comprises reaction pretreatment unit; Reaction pretreatment unit comprises material mixer 14 and pre-reactor 15; Material mixer is provided with methanol inlet 141, formaldehyde entrance 142 and mixture outlet 143; Pre-reactor 15 is provided with material inlet 151 and pre-reaction liquid outlet 152, and material inlet 151 and mixture export 143 and be connected, and pre-reaction liquid outlet 152 is connected with feedstock pipeline 70.
Pre-reactor 15 inside is provided with pre-reaction catalyst filling layer; Pre-reactor 15 is provided with 1-50 group, and often group is set to 1-10, and the outlet of upper one group of pre-reactor is connected with next entrance organizing pre-reactor.
This device preparing methylal also comprises catalyst treatment agent storage tank 16, storage tank 17 and Matter Transfer pump 18 are reclaimed in catalyst treatment agent; Catalyst treatment agent storage tank 16 is provided with entrance and exit, and the outlet of catalyst treatment agent storage tank is connected with catalyst treatment agent feeding pipe 71; Catalyst treatment agent is reclaimed storage tank 17 and is provided with entrance and exit, and the entrance that storage tank is reclaimed in catalyst treatment agent is connected with catalyst treatment agent recycling pipeline 73; Matter Transfer pump 18 is arranged between the entrance of bottom liquid outlet 42 and reboiler 10; Bottom liquid section 4 is also provided with waste liquid outlet 45.
A kind of schematic diagram (reaction surge tank is shown) preparing the device of methylal that Figure 12 provides for the embodiment of the present application.The device preparing methylal as shown in figure 12, the one group of raw material discharging bifurcations 701,702,703 corresponding to each catalyst filling section in its 3 catalyst filling sections and be provided with between reaction material feed back bifurcations 704,705,706 one reaction surge tank 11,12,13, be namely provided with 11 between 701 and 704, between 702 and 705, be provided with 12, between 703 and 706, be provided with 13; Catalyst filling layer is provided with in reaction surge tank.
In an optional embodiment, one can be arranged there is the reaction surge tank being flexibly connected interface, when a certain section of catalyst filling layer in reactive distillation column needs process regeneration, be connected between this section corresponding raw material discharging bifurcations and reaction material feed back bifurcations, to reduce the quantity of reaction surge tank, reduce costs.
The foregoing is only the preferred embodiment of the application, be not limited to the application, for a person skilled in the art, the application can have various modifications and variations.Within all spirit in the application and principle, any amendment done, equivalent replacement, improvement etc., within the protection domain that all should be included in the application.
Claims (9)
1. realized a method for continuous production methylal by the on-line regeneration of catalyzer, it is characterized in that, the method is carrying out the on-line regeneration process carrying out catalyzer while prepared by methylal;
The reactive distillation column (1) with multiple catalyst filling section (3) is employed in the process of the preparation of described methylal;
The on-line regeneration process of described catalyzer comprises following four steps of carrying out successively:
A () isolates with the fluid preparing methylal needing the catalyst filling section of carrying out catalyst regeneration process;
B () regenerates the described catalyzer carried out in the catalyst filling section of catalyst regeneration process that needs;
C () rinses the catalyst filling section completing catalyst regeneration process;
D () is carried out recovery to the described catalyst filling section completing catalyst regeneration process and is come into operation,
Wherein, described step (a) comprises liquid isolation and gas barrier, and the isolation of described liquid and described gas barrier are carried out simultaneously; The isolation of described liquid and described gas barrier be by gently close need to carry out the catalyst filling section correspondence of catalyst regeneration process raw material discharging bifurcations, reaction material feed back bifurcations, gas feed bifurcations and gas discharge bifurcations on valve or valve group realization;
The preparation of described methylal comprises the following steps:
E multiple catalyst filling sections (3) that () raw material reaction liquid enters in reactive distillation column (1) after pre-reaction carry out catalyzed reaction, enter into the bottom liquid section (4) of reactive distillation column after completing catalyzed reaction;
F the reaction solution of () bottom liquid section (4) enters into reboiler (10) by described reactive distillation column (1), the multiple catalyst filling sections (3) again entered after heating and gasifying in described reactive distillation column (1) carry out catalyzed reaction, enter into the top gas section (2) of reactive distillation column after completing catalyzed reaction;
G the gas of () top gas section (2) enters into condenser (8) by described reactive distillation column (1), enter phlegma storage tank (9) after condensation liquefaction;
H () phlegma is got back to the multiple catalyst filling sections (3) again entered in described reactive distillation column (1) after feedstock pipeline (70) mixes with raw material reaction liquid by described phlegma storage tank (9) and is carried out catalyzed reaction;
I () iterative cycles step (e)-(h), according to reacting the situation of carrying out, contains the material of product methylal from phlegma feed back outlet (91) extraction.
2. method according to claim 1, it is characterized in that, described multiple catalyst filling sections (3) in described reactive distillation column (1) comprise 2-10 section catalyst filling section, and the longitudinal direction along described reactive distillation column (1) from top to bottom sets gradually.
3. method according to claim 1, is characterized in that, described liquid has isolated rear raw material reaction liquid at least one catalyst filling section feeding from other except the described catalyst filling section needing to carry out catalyst regeneration process; The catalyst filling section that after described gas barrier completes, gas enters above except the described catalyst filling section needing to carry out catalyst regeneration process carries out catalyzed reaction, or enters top gas section (2) until enter condenser (8).
4. method according to claim 3, is characterized in that, described liquid has isolated the catalyst filling section feeding of rear raw material reaction liquid from the superiors or the second layer; After described gas barrier completes, gas enters an adjacent catalyst filling section above and carries out catalyzed reaction, or enters top gas section (2) until enter condenser (8).
5. the method according to any one of claim 1-4, it is characterized in that, described step (b) comprises the following steps: catalyst treatment agent arrives the described catalyst filling section of carrying out catalyst regeneration process that needs from catalyst treatment agent storage tank (16) through catalyst treatment agent feeding pipe (71) and carries out manipulation of regeneration to catalyzer, complete the catalyst treatment agent after manipulation of regeneration through catalyst treatment agent recycling pipeline (73) enter into catalyst treatment agent reclaim storage tank (17) reclaim.
6. method according to claim 5, is characterized in that, described step (c) comprises the following steps of carrying out successively:
P () closes the valve that valve that described catalyst treatment agent storage tank (16) and catalyst treatment agent reclaim storage tank (17) opens irrigation storage tank (19) and waste liquid tank (20) simultaneously;
The catalyst filling section completing catalyst regeneration process q () irrigation to arrive from described irrigation storage tank (19) through described catalyst treatment agent feeding pipe (71) described in is rinsed, and completes the waste liquid after flushing and enters waste liquid tank (20) through described catalyst treatment agent recycling pipeline (73).
7. method according to claim 6, is characterized in that, described step (d) comprises the following steps of carrying out successively:
R () stops completing the flushing after catalyst regeneration process;
S () has made the catalyst filling section of catalyst regeneration process recover to come into operation.
8. method according to claim 7, it is characterized in that, described step (r) is valve by closing irrigation storage tank (19) and the valve completed described in simultaneously gently closing on the catalyst treatment agent discharging bifurcations of the catalyst filling section correspondence of catalyst regeneration process, the branch inlet of liquid inlet opening and the branch outlet of liquid outlet opening or valve group realize.
9. method according to claim 7, it is characterized in that, described step (s) is that valve in raw material discharging bifurcations, reaction material feed back bifurcations, gas feed bifurcations and the gas discharge bifurcations by completing the catalyst filling section correspondence of catalyst regeneration process described in gently opening or valve group realize.
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| CN101786946A (en) * | 2010-04-01 | 2010-07-28 | 江苏恒茂机械制造有限公司 | Methylal preparation device |
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