CN105478062A - Method of filling maleic anhydride catalysts through benzene - Google Patents
Method of filling maleic anhydride catalysts through benzene Download PDFInfo
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- CN105478062A CN105478062A CN201510932260.7A CN201510932260A CN105478062A CN 105478062 A CN105478062 A CN 105478062A CN 201510932260 A CN201510932260 A CN 201510932260A CN 105478062 A CN105478062 A CN 105478062A
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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
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
- B01J8/06—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds in tube reactors; the solid particles being arranged in tubes
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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
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/0015—Feeding of the particles in the reactor; Evacuation of the particles out of the reactor
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D307/00—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
- C07D307/02—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings
- C07D307/34—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members
- C07D307/56—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D307/60—Two oxygen atoms, e.g. succinic anhydride
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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
- B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
- B01J2208/00743—Feeding or discharging of solids
- B01J2208/00752—Feeding
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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
- B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
- B01J2208/00743—Feeding or discharging of solids
- B01J2208/00769—Details of feeding or discharging
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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
- B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
- B01J2208/00796—Details of the reactor or of the particulate material
- B01J2208/00805—Details of the particulate material
- B01J2208/00814—Details of the particulate material the particulate material being provides in prefilled containers
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
Abstract
The invention aims at providing a method of filling maleic anhydride catalysts through benzene. The method comprises the steps of (1) preparation before filling of the catalysts, (2) filling of second-stage catalysts and (3) filling of first-stage catalysts. The filling method has the advantages that by measuring the heights and bed pressure drops of a secondary catalyst bed and a primary catalyst bed respectively, bridging of the catalysts can be prevented, the problem of non-uniform filling of the two-stage catalysts is solved, and then adverse effects on the catalytic reaction process are reduced.
Description
Technical field
The present invention relates to catalyst technical field, be specifically related to a kind of packing method of benzene method maleic anhydride catalyst.
Background technology
Maleic anhydride (being called for short " cis-butenedioic anhydride ") is important basic organic chemical industry raw material.Produce cis-butenedioic anhydride mainly with benzene, normal butane or butylene for raw material, be that unstripped gas fixes a catalytic oxidation cis-butenedioic anhydride existing many decades history at home and abroad at present with benzene, benzene oxidatoin method is the conventional production methods of production cis-butenedioic anhydride, and mature technology is reliable.
Cis-butenedioic anhydride is exothermic reaction, so usually adopt shell and tube reactor in course of reaction, this reactor loads catalyst usually in pipe, and shell side then passes to suitable thermophore.Although being seated in chemical products production process of catalyst is a routine operation, but Catalyst packing quality being uniformly distributed beds air-flow, the reduction of bed resistance, effective performance of catalyst efficiency, and normal production in the future, the prolongation in energy-saving and cost-reducing and even catalyst service life all bring direct impact, the filling quality of catalyst will be directly connected to whole course of reaction thus.For filling or more catalyst changeout, no matter be adopt traditional manual method or adopt special Catalyst packing equipment, this workload is all larger and complicated, easy neglected loading or filling uneven.The irregular stage raw material bias current that will induce reaction of Catalyst packing, gently then causes reaction effect to be deteriorated, weighs and then cause beds overtemperature to cause shut-down.In filling process, breakage rate must be reduced as far as possible, prevent " bridge formation " phenomenon from occurring.
Summary of the invention
Adopt two section bed benzene oxidatoin legal system in the technique of cis-butenedioic anhydride, the reactor adopted is tubular fixed-bed reactor, catalyst in this fixed-bed column reactor is made up of two kinds of catalyst of two sections different formulations, different size, the concrete preparation method of catalyst belongs to prior art, can be specifically CN101284242B see Authorization Notice No., the Chinese invention patent that name is called " catalyst of producing maleic anhydrid (e) by benzene gas-phase oxidation with high load and high yield ".
The technical problem to be solved in the present invention is to provide a kind of packing method of benzene method maleic anhydride catalyst, loads irregular problem to solve two section bed catalyst in prior art.
Technical scheme of the present invention is a kind of packing method of benzene method maleic anhydride catalyst, it is characterized in that comprising following step:
(1) preparation before Catalyst packing
After being cleaned out by reactor tubulation, bottom loads complex spring;
The filling of (2) two sections of catalyst
Beds is carried out not decile to divide, catalyst loads two-stage catalytic agent from down to up and is called two sections of catalyst and one section of catalyst, loader is adopted to load catalyst, two sections of catalyst are loaded in the hopper of loader, can load according to the reactor tubulation of loader tremie pipe number to respective numbers simultaneously.After filling, measure the loading height of two sections of catalyst, if the deviating height of two sections of catalyst exceeds the scope of permission, then use dust catcher sucking-off part two sections of catalyst; If the deviating height of two sections of catalyst in allowed limits, then Pressure Drop test is carried out to two sections of catalyst of each reaction tube, each pipe pressure is fallen and averages, if the Pressure Drop of two sections of catalyst higher than average pressure fall 106% time, then use the agent of dust catcher sucking-off partially catalyzed, if fall lower than average pressure 94% of two sections of catalyst, then should bleed off and re-start filling;
The filling of (3) one sections of catalyst
Two sections of catalyst packing heights and Pressure Drop are all within the range of permission, then carry out the filling of one section of catalyst, if the deviating height of one section of catalyst exceeds the scope of permission, then use dust catcher sucking-off part one section of catalyst, when one section of catalyst deviating height in allowed limits, then Pressure Drop test is carried out to the total bed of catalyst, the total pressure drop of column of each pipe catalyst is averaged, if the total pressure drop of column of catalyst higher than average pressure fall 106% time, then use dust catcher sucking-off part one section of catalyst, if the total bed layer pressure of catalyst be reduced to that average pressure falls 94%, then should bleed off and re-start filling.
Further, described reactor tubulation is length 3600mm, and diameter is the seamless steel pipe of Ф 25 × 2mm.
Further, the total bed height 3200 ~ 3300mm of described catalyst, in each reactor tubulation, catalyst total filling amount is 860 ± 5g.
Further, the loading height of described two sections of catalyst is 1950mm, deviating height should loading height ± 80mm.
Further, the loading height of described one section of catalyst is 1300mm, deviating height should loading height ± 50mm.
Further, the carrier of described catalyst selects corundum (α-Al
2o
3), one in carborundum (SiC), support shapes is annular.
Beneficial effect of the present invention is: by measuring height and the pressure drop of column of two sections of catalyst and one section of beds respectively, catalyst " bridge formation " phenomenon can be prevented, solve two section bed catalyst and load irregular problem, and then reduce the harmful effect to catalytic reaction process.
Detailed description of the invention
Below in conjunction with embodiment, brief description is made to the specific embodiment of the present invention.
Embodiment one:
The filling of two sections of catalyst: beds is carried out not decile and divide, catalyst loads two-stage catalytic agent from down to up and is called two sections of catalyst and one section of catalyst, loader is adopted to load catalyst, two sections of catalyst are loaded in the hopper of loader, can load according to the reactor tubulation of loader tremie pipe number to respective numbers simultaneously.After filling, measure the loading height of two sections of catalyst, if the deviating height of two sections of catalyst exceeds the scope of permission, then use dust catcher sucking-off part two sections of catalyst; If the deviating height of two sections of catalyst in allowed limits, then Pressure Drop test is carried out to two sections of catalyst of each reaction tube, each pipe pressure is fallen and averages, if the Pressure Drop of two sections of catalyst higher than average pressure fall 106% time, then use the agent of dust catcher sucking-off partially catalyzed, if fall lower than average pressure 94% of two sections of catalyst, then should bleed off and re-start filling.
Repeat 30 times to above-mentioned filling, and add up bed pressure drop, statistics is in table 1.
Two sections of beds pressure drop deviation statistics in table 1 embodiment one
Two sections of beds pressure drop deviations | Number of times is added up |
>106% | 4 |
94%~106% | 23 |
<94% | 3 |
Embodiment two:
The filling of one section of catalyst: two sections of catalyst packing heights and Pressure Drop are all within the range of permission, then carry out the filling of one section of catalyst, if the deviating height of one section of catalyst exceeds the scope of permission, then use dust catcher sucking-off part one section of catalyst, when one section of catalyst deviating height in allowed limits, then Pressure Drop test is carried out to the total bed of catalyst, the total pressure drop of column of each pipe catalyst is averaged, if the total pressure drop of column of catalyst higher than average pressure fall 106% time, then use dust catcher sucking-off part one section of catalyst, if the total bed layer pressure of catalyst be reduced to that average pressure falls 94%, then should bleed off and re-start filling.
Repeat 30 times to above-mentioned filling, and add up bed pressure drop, statistics is in table 2.
The total bed pressure drop deviation statistics of catalyst in table 2 embodiment two
The total bed pressure drop deviation of catalyst | Number of times is added up |
>106% | 6 |
94%~106% | 20 |
<94% | 4 |
Above one embodiment of the present of invention have been described in detail, but described content being only preferred embodiment of the present invention, can not being considered to for limiting practical range of the present invention.All equalizations done according to the present patent application scope change and improve, and all should still belong within patent covering scope of the present invention.
Claims (6)
1. a packing method for benzene method maleic anhydride catalyst, is characterized in that, comprises following step:
(1) preparation before Catalyst packing
After being cleaned out by reactor tubulation, bottom loads complex spring;
The filling of (2) two sections of catalyst
Beds is carried out not decile to divide, catalyst loads two-stage catalytic agent from down to up and is called two sections of catalyst and one section of catalyst, loader is adopted to load catalyst, two sections of catalyst are loaded in the hopper of loader, can load according to the reactor tubulation of loader tremie pipe number to respective numbers simultaneously.After filling, measure the loading height of two sections of catalyst, if the deviating height of two sections of catalyst exceeds the scope of permission, then use dust catcher sucking-off part two sections of catalyst; If the deviating height of two sections of catalyst in allowed limits, then Pressure Drop test is carried out to two sections of catalyst of each reaction tube, each pipe pressure is fallen and averages, if the Pressure Drop of two sections of catalyst higher than average pressure fall 106% time, then use the agent of dust catcher sucking-off partially catalyzed, if fall lower than average pressure 94% of two sections of catalyst, then should bleed off and re-start filling;
The filling of (3) one sections of catalyst
Two sections of catalyst packing heights and Pressure Drop are all within the range of permission, then carry out the filling of one section of catalyst, if the deviating height of one section of catalyst exceeds the scope of permission, then use dust catcher sucking-off part one section of catalyst, when one section of catalyst deviating height in allowed limits, then Pressure Drop test is carried out to the total bed of catalyst, the total pressure drop of column of each pipe catalyst is averaged, if the total pressure drop of column of catalyst higher than average pressure fall 106% time, then use dust catcher sucking-off part one section of catalyst, if the total bed layer pressure of catalyst be reduced to that average pressure falls 94%, then should bleed off and re-start filling.
2. the packing method of a kind of benzene method maleic anhydride catalyst according to claim 1, it is characterized in that: described reactor tubulation is length 3600mm, diameter is the seamless steel pipe of Ф 25 × 2mm.
3. the packing method of a kind of benzene method maleic anhydride catalyst according to claim 1, is characterized in that: the total bed height 3200 ~ 3300mm of described catalyst, in each reactor tubulation, catalyst total filling amount is 860g.
4. the packing method of a kind of benzene method maleic anhydride catalyst according to claim 1, is characterized in that: the loading height of described two sections of catalyst is 1950mm, deviating height should loading height ± 80mm.
5. the packing method of a kind of benzene method maleic anhydride catalyst according to claim 1, is characterized in that: the loading height of described one section of catalyst is 1300mm, deviating height should loading height ± 50mm.
6. the packing method of a kind of benzene method maleic anhydride catalyst according to claim 1, is characterized in that: the carrier of described catalyst selects the one in corundum, carborundum, and support shapes is annular.
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CN201510932260.7A CN105478062B (en) | 2015-12-14 | 2015-12-14 | A kind of packing method of benzene method maleic anhydride catalyst |
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Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH09141084A (en) * | 1995-11-27 | 1997-06-03 | Mitsubishi Rayon Co Ltd | Packing method of solid catalyst |
US5892108A (en) * | 1996-05-09 | 1999-04-06 | Mitsubishi Rayon Co., Ltd. | Method for packing with catalyst for synthesis of unsaturated aldehyde and unsaturated carboxylic acid |
CN1514803A (en) * | 2001-06-06 | 2004-07-21 | ά | Furnace and steam reforming process |
CN103816931A (en) * | 2014-02-10 | 2014-05-28 | 常州新日催化剂有限公司 | Catalyst for maleic anhydride preparation by benzene oxidation |
-
2015
- 2015-12-14 CN CN201510932260.7A patent/CN105478062B/en not_active Expired - Fee Related
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH09141084A (en) * | 1995-11-27 | 1997-06-03 | Mitsubishi Rayon Co Ltd | Packing method of solid catalyst |
US5892108A (en) * | 1996-05-09 | 1999-04-06 | Mitsubishi Rayon Co., Ltd. | Method for packing with catalyst for synthesis of unsaturated aldehyde and unsaturated carboxylic acid |
CN1514803A (en) * | 2001-06-06 | 2004-07-21 | ά | Furnace and steam reforming process |
CN103816931A (en) * | 2014-02-10 | 2014-05-28 | 常州新日催化剂有限公司 | Catalyst for maleic anhydride preparation by benzene oxidation |
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Effective date of registration: 20181226 Address after: 300 000 No. 499-1 Jinyuan Road, Dagang, Binhai New Area, Tianjin Patentee after: TIANJIN BOHUA ZHONGHE CHEMICAL Co.,Ltd. Address before: 300000 Jinyuan Road, Tianjin Binhai New Area (Dagang) Petrochemical Industrial Park (Tianjin Bohua Zhonghe Chemical Co., Ltd.) Patentee before: TIANJIN TIANHUAN INSTITUTE OF FINE CHEMICAL ENGINEERING |
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Granted publication date: 20180213 Termination date: 20211214 |