CN2536587Y - Methyl acetate hydrolyzer - Google Patents
Methyl acetate hydrolyzer Download PDFInfo
- Publication number
- CN2536587Y CN2536587Y CN 02213024 CN02213024U CN2536587Y CN 2536587 Y CN2536587 Y CN 2536587Y CN 02213024 CN02213024 CN 02213024 CN 02213024 U CN02213024 U CN 02213024U CN 2536587 Y CN2536587 Y CN 2536587Y
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- tubulation
- tower
- section
- tower tray
- reaction rectification
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The utility model discloses a methyl acetate hydrolysis device used for reaction rectification of methyl acetate hydrolysis, belonging to universal chemical equipment. The utility model comprises a cylindrical tower body divided into a reaction rectification section and a stripping section; a reaction rectification structure unit in the reaction rectification section comprises a tube provided and a tray; gel-type positive ion exchange resin is filled in the tube; one to ten layer reaction rectification structure units are arranged in the reaction rectification section, and the stripping section is connected with the reaction rectification section by the cylindrical tower body. The utility model is a cylindrical tower and comprises the reaction rectification section and the stripping section, the hydrolysis reaction intakes place in the reaction rectification section. The reaction rectification structure unit in the reaction rectification section combines the catalyst filling device, the liquid distributor, the overflow pipe and the steam-liquid contact device. The utility model has the advantages of compact structure and high equipment efficiency.
Description
Technical field:
The utility model relates to the used equipment of methyl acetate hydrolysis reactive distillation process, belongs to the universalization construction equipment.
Background technology:
The a large amount of ritalin of by-product in polyvinyl alcohol (PVA) is produced, at present PVA producer mostly adopts stationary cation bed hydrolysis process that ritalin is resolved into methyl alcohol and acetic acid and is recycled, the main drawback of fixed bed hydrolysis process is that the methyl acetate hydrolysis rate is low, a large amount of unhydrolysed ritalins need circulate, cause equipment huge, the energy consumption height.In reactants water ester mol ratio is 0.95～1.0 o'clock, and general percent hydrolysis can only reach 23%～25%.There are patent and bibliographical information to adopt the new hydrolysis process of catalytic distillation at present.
Adopting the gordian technique of catalysis rectification hydrolysis technique is the filling method of catalyzer (Zeo-karb) in reaction unit.The Japan special permission communique (JP8207259) and day disclosure are speciallyyed permit (JP05212290) and document, and (CA 96164550n) has reported the filling method of two kinds of catalyzer.A kind of is Zeo-karb to be made fibrous, is wrapped on the sticking plaster, in the tower of packing into then.Another kind is to use inert plastic as binding agent, and ion-exchange resin particles is molded into the cylinder shape catalyst filler with high density polyethylene(HDPE) under heating and melting, then is filled in the tower.The type of feed of these two kinds of catalyzer all has the trouble of making, and the shortcoming of difficulty is changed and reclaimed to catalyzer.Especially the second method loss that can come off after catalyzer uses for some time causes catalyst loss.The patent (WO9620912) of the Kim Ki-Joo of Korea S also is to adopt above-mentioned second kind of type of feed.Chinese patent (ZL97101306.3) adopts the mode of " tying up bag ", the Zeo-karb corrosion resistant Bu Baonei that packs into is made catalyst filling, pack into then and react in the tower, solved the shortcoming that the catalyst particles abscission runs off like this, but the manufacturing of catalyst pack is still cumbersome.The replacing of catalyzer is still inconvenient with activation.
Summary of the invention:
The purpose of this utility model provide a kind of with Zeo-karb be catalyzer ritalin equipment.
The utility model task is: the equipment of methyl acetate hydrolysis, comprise a cylindrical tower body, tower is divided into reactive distillation section and stripping section, reactive distillation structural unit in the reactive distillation section is made of tubulation that the gel type cation exchange resin is housed and tower tray, 1～10 layer of reactive distillation structural unit is housed in the reactive distillation section, and wherein stripping section links to each other by cylindrical tower body with rectifying section.
The invention has the advantages that (1) catalyst loading, activation, replacing are very convenient, the efficient height of catalyzer.(2) liquid dispenser, upflow tube tower tray are organically combined compact construction, device space utilization ratio height.
Below with reference to accompanying drawing embodiment of the present utility model is further described:
Fig. 1 process flow sheet of the present utility model
Fig. 2 reactive distillation modular construction of the present utility model front view
Fig. 3 reactive distillation modular construction of the present utility model vertical view
Fig. 4 I figure of the present utility model
Fig. 5 II figure of the present utility model
Fig. 6 III figure of the present utility model
Fig. 7 set ring structural representation of the present utility model
Among the figure: 1 is condenser; 2 is first preheater; 3 is first volume pump; 4 is vessel; 5 is second volume pump; 6 is second preheater; 7 is stripping section; Fig. 8 is cylindrical tower body; 9 is rectifying section, and 10 is thermometer; 11 is water coolant; 12 is nut, and 13 is seal washer; 14 is bolt; 15 is supporting cup; 16 is tower tray; 17 is upflow tube; 18 is tubulation; 19 is set ring; 20 is screen; 21 is leg; 22 is downtake; 23 is sieve aperture.
The utility model comprises a cylindrical tower body, and tower body is divided into reactive distillation section and stripping section; The reactive distillation section is made up of cylindrical shell and the reactive distillation structural unit that Zeo-karb is housed.Reaction zone is equipped with 1～10 reactive distillation structural unit.Fig. 2 is a reactive distillation structural unit front view.It is characterized by: Zeo-karb is housed as catalyzer in (1) tubulation, 0.2～2 meter of tubulation length, 10～200 millimeters of tubulation diameters, the lower end of tubulation is that 2～5 millimeters stainless steel plate is sealed with being drilled with diameter, survey in the pipe lower end and be lined with Stainless Steel Cloth and corrosion-resistant cloth, spill in order to prevent granules of catalyst.Tubulation hypomere side is drilled with diameter less than 0.5 millimeter aperture or do not hole.(2) tower tray of liquid distribution, overflow and vapour-liquid contact action has been equipped with in the tubulation upper end, the number liquid identical with tubulation is housed on the tower tray distributes upflow tube, plays the effect of evenly distributing liquid and overflow.Overfall tube diameter 5～50mm, upflow tube length overall 100～300mm.A upflow tube part is positioned at the tower tray upside, and a part is positioned at the tower tray downside.Upside exceeds tower tray 20～100mm, and there is the lance tooth of high 2～10mm the upflow tube upper edge, angle [alpha]=30～90 °.The upflow tube downside stretches into tubulation 10～30mm.(3) tubulation Stainless Steel Wire harness is placed on the screen 20, and tubulation is located with set ring 19.The internal diameter of set ring and tubulation bundle external diameter are complementary, and external diameter and tower cylinder internal diameter are complementary.Set ring is fixed on the cylinder inboard wall with screw.Screen supports with the leg 21 that is welded on the tower cylindrical shell.Tower tray is fastened on screw on the supporting cup 15 that is welded on the cylindrical shell, seals with seal washer 13 between tower tray and the supporting cup.Gas contacts with liquid on tower tray along rising on the tubulation gap.Liquid enters the catalyst zone that is contained in the tubulation and reacts along upflow tube toward current downflow.
Its reactive distillation structural unit,
1. the ion exchange resin as catalyzer is contained in the tubulation 18, and bottom, tubulation side is drilled with aperture or does not hole, and seal with the stainless steel plate that is drilled with aperture the tubulation bottom;
2. tubulation above tower tray 16 is housed, tower tray is a sieve plate, be uniform-distribution with on the tower tray and the same number of upflow tube 17 of tubulation, upflow tube 17 parts are positioned at the tower tray upside, a part is positioned at the tower tray downside, and upside exceeds tower tray 20～100mm, and there is lance tooth upflow tube 17 upper edges, angle [alpha]=30～90 °, upflow tube 17 downsides stretch into tubulation;
3. tubulation Stainless Steel Wire harness, be placed on the screen 20, tubulation is located with set ring 19, the internal diameter of set ring and tubulation bundle external diameter are complementary, external diameter and tower cylinder internal diameter are complementary, and set ring 19 usefulness screws are fixed on the cylinder inboard wall, and the leg 21 that screen 20 usefulness are welded on the tower cylindrical shell supports, tower tray 16 usefulness screws are fastened on the supporting cup 15 that is welded on the cylindrical shell, seal with seal washer 13 between tower tray 16 and the supporting cup 15.
Example of the present invention adopts described processing condition to carry out in described hydrolysis device, and wherein, ritalin, water are with measuring pump delivery, and quantity of reflux is measured with under meter.The tower still is the there-necked flask of 2000 milliliters of volumes, with electric mantle heating, tower body electrical heat tracing, intermittently extracts still liquid out to keep the tower bottoms position.The hydrolyzed solution of extracting out is analyzed with Varian GC3800 gas chromatograph.
The specific operation process of embodiment is: by the ritalin of proportioning metering or ritalin and carbinol mixture through second volume pump 5 be transported to continuously second preheater 6 be heated to preset temperature after from the top of hydrolysis tower or the bottom of hydrolysis tower reactive distillation section or the middle part of hydrolysis tower stripping section send into hydrolysis tower, simultaneously be transported to first preheater 2 through the water of metering continuously with first volume pump 3 and be heated to preset temperature and enter hydrolysis tower from cat head, reaction is hydrolyzed in reaction zone.By rectifying separation, volatile components (mainly being ritalin) is in cat head device 1 condensation that is condensed in tower for reaction product, and phlegma mixes with water after 2 heating of first preheater are sent the continuation of hydrolysis tower reaction zone back to and reacted.Reaction solution is extracted out continuously to keep the tower bottoms position from reboiler.The reaction solution of extracting out is with gas chromatograph for determination methyl alcohol and ritalin concentration wherein, with standard base (SB) titrimetry acetate concentration.Reaction process each component concentration of 3～8 hours afterreaction liquid of operation analysis continuously tends towards stability.Continue operation then and finished reaction in 3～5 hours.
Claims (2)
1, a kind of methyl acetate hydrolysis equipment, it is characterized in that: comprise a cylindrical tower body (8), tower is divided into reactive distillation section (9) and stripping section (7), reactive distillation structural unit in the reactive distillation section is made of tubulation that the gel type cation exchange resin is housed (18) and tower tray (16), 1～10 layer of reactive distillation structural unit is housed in the reactive distillation section, and wherein stripping section (7) links to each other by cylindrical tower body (8) with rectifying section (9).
2, the equipment of methyl acetate hydrolysis according to claim 2 is characterized in that: its reactive distillation structural unit:
1. the ion exchange resin as catalyzer is contained in the tubulation (18), and bottom, tubulation side is drilled with aperture or does not hole, and seal with the stainless steel plate that is drilled with aperture the tubulation bottom;
2. tubulation above tower tray (16) is housed, tower tray is a sieve plate, be uniform-distribution with on the tower tray and the same number of upflow tube of tubulation (17), upflow tube (a 17) part is positioned at the tower tray upside, a part is positioned at the tower tray downside, and upside exceeds tower tray 20～100mm, and there is lance tooth upflow tube (17) upper edge, angle [alpha]=30～90 °, upflow tube (17) downside stretches into tubulation;
3. tubulation Stainless Steel Wire harness, be placed on the screen (20), tubulation is located with set ring (19), the internal diameter of set ring and tubulation bundle external diameter are complementary, external diameter and tower cylinder internal diameter are complementary, and set ring (19) is fixed on the cylinder inboard wall with screw, and screen (20) supports with the leg (21) that is welded on the tower cylindrical shell, tower tray (16) is fastened on screw on the supporting cup (15) that is welded on the cylindrical shell, seals with seal washer (13) between tower tray (16) and the supporting cup (15).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02213024 CN2536587Y (en) | 2002-03-01 | 2002-03-01 | Methyl acetate hydrolyzer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02213024 CN2536587Y (en) | 2002-03-01 | 2002-03-01 | Methyl acetate hydrolyzer |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN2536587Y true CN2536587Y (en) | 2003-02-19 |
Family
ID=33692609
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 02213024 Expired - Fee Related CN2536587Y (en) | 2002-03-01 | 2002-03-01 | Methyl acetate hydrolyzer |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN2536587Y (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012164573A2 (en) | 2011-05-27 | 2012-12-06 | Reliance Industries Ltd., | Hydrolysis and esterification with acid catalysts |
| CN104152598A (en) * | 2014-08-26 | 2014-11-19 | 南通赛孚机械设备有限公司 | High-pressure reverse-flow continuous hydrolysis kettle for preparation of aliphatic acid |
-
2002
- 2002-03-01 CN CN 02213024 patent/CN2536587Y/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012164573A2 (en) | 2011-05-27 | 2012-12-06 | Reliance Industries Ltd., | Hydrolysis and esterification with acid catalysts |
| CN104152598A (en) * | 2014-08-26 | 2014-11-19 | 南通赛孚机械设备有限公司 | High-pressure reverse-flow continuous hydrolysis kettle for preparation of aliphatic acid |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |