CN2685336Y - Special internal circulating reactor for combining liquid phase carbo oxide into dimethylester carbonate - Google Patents
Special internal circulating reactor for combining liquid phase carbo oxide into dimethylester carbonate Download PDFInfo
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- CN2685336Y CN2685336Y CN 200320104432 CN200320104432U CN2685336Y CN 2685336 Y CN2685336 Y CN 2685336Y CN 200320104432 CN200320104432 CN 200320104432 CN 200320104432 U CN200320104432 U CN 200320104432U CN 2685336 Y CN2685336 Y CN 2685336Y
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- pipe
- reactor
- carbonate
- vapor
- dimethylester
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Abstract
The utility model discloses a special internal circulating reactor for combining liquid phase carbo oxide into dimethylester carbonate, comprising a pipe reactor, and a return pipe which is connected with the pipe reactor. The special internal circulating reactor for combining liquid phase carbo oxide into dimethylester carbonate is characterized in that the reaction pipe is sheathed with the return pipe. The inner pipe is the reaction pipe, the space between the inner pipe and the outer pipe is the return pipe, and the upper section enlargement pipe of the two pipes is the fallaway section of the vapor and the liquid. The upper end of the outer pipe of the two coaxial pipes is connected with the bottom of the fallaway section of the vapor and the liquid. Compared with the prior art, the special internal circulating reactor for combining liquid phase carbo oxide into dimethylester carbonate has the advantages of simple structure, easy manufacturing and installation, small occupation of land, good mass transfer and heat transfer, high reaction efficiency, convenient temperature control, and low manufacture energy consumption.
Description
The utility model belongs to chemical industry equipment and makes the field.Especially a kind of by liquid phase methyl alcohol CH
3OH, gas phase CO, O
2And under the condition of catalyzer existence, carry out the tubular reactor of gas-liquid-solid phase reaction.
With methyl alcohol CH
3OH, gas phase CO, O
2Be raw material, preparation methylcarbonate tubular reactor under the condition that catalyzer exists, Italian Enichem company and the Chinese Hubei chemical industry joint stock company that jumps has together all applied for patent.The patent No. of Italy Enichem company application is EP0460735A2, and the feature of this patent reactor is made up of a reaction tubes and a return line.Form two-tube outer circulation.Jump the together patent publication No. of chemical industry joint stock company application of China Hubei is CN1204644A, and the feature of this patent reactor is that reactor is made up of many reaction tubess and a return line.Also be outer circulation.The common feature of these two kinds of patent reactors is that the effusive gas-liquid mixture in reaction tubes upper end is the vapor-liquid separation section of reactor top is separated into vapour-liquid two parts owing to gravitational difference after, liquid all is back to reaction tubes by self gravitation, and return line is arranged on outside the reaction tubes; Reaction tubes and heating of return line peripheral hardware or cooling jacket.The main drawback of this structure is reactor processing, and trouble especially is installed, and floor space is big, and the phegma cycling distance is big, and heat dissipation capacity is big, adds and adopts chuck heating or cooling, and the temperature control hysteresis time is long, by contrast the production energy consumption height.
Above shortcoming in view of prior art, the purpose of this utility model is to improve at the deficiency of above-mentioned reactor, a kind of bubbling style single tube inner circulation reactor of liquid-phase oxidation carbonylation Synthesis of dimethyl carbonate is provided, it is simple in structure that it is had, and is easy to processing and installs, and takes up an area of and economize, mass transfer and conducting heat, the reaction efficiency height, temperature control is convenient, the advantage that production energy consumption is low.
The purpose of this utility model is to realize by following means.
The special-purpose inner circulation reactor of liquid-phase oxidation carbonylation Synthesis of dimethyl carbonate, mainly be made up of tubular reactor and the return line that is attached thereto, reaction tubes is nested with return line is coaxial, and interior pipe is a reaction tubes, gap between interior pipe and the outer tube is a return line, and the epimere enlarged tube of two pipes is the vapor-liquid separation section; Two coaxial valve outer tubes upper end links to each other with vapor-liquid separation section bottom, and the lower end is provided with material inlet and drain hole, and the vapor-liquid separation section has pneumatic outlet.
After adopting means as above, structure of reactor is simple, is easy to processing and installs, and take up an area of and economize, mass transfer and conducting heat, the reaction efficiency height, it is convenient that temperature is controlled, and production energy consumption is low.
Description of drawings is as follows:
Fig. 1 is the structure iron of liquid of the present utility model.
Below in conjunction with accompanying drawing structure of the present utility model is described in further detail.
Fig. 1 is the configuration diagram of the bubbling style single tube inner circulation reactor of liquid-phase oxidation carbonylation Synthesis of dimethyl carbonate of the present utility model.
Reaction tubes is nested with return line is coaxial as shown in fig. 1, and interior pipe is a reaction tubes 1, and the gap between interior pipe and the outer tube 2 is a return line, and the epimere enlarged tube of two pipes is a vapor-liquid separation section 3; The lower end is connected with raw material gas inlet 6 and drain hole 7 with material benzenemethanol import 5.Traverse baffle 11 is housed in the vapor-liquid separation section.Pipe 1 inlet is equipped with gas distributor 8 and heating or spiral coil cooling tube 4.9 is pneumatic outlet.10 for pipe 1 with manage port between 2, and withdrawing fluid loops back by this port and flows in the reaction tubes 1.
After medium methyl alcohol, CO, O2 and the catalyzer of reaction system enters reactor and begins reaction, Gu after the gas band liquid-medium and risen to the vapor-liquid separation section, because of the diameter of vapor-liquid separation section amplifies medium generation gravity settling natural separation suddenly than reaction tubes.Isolating methyl alcohol-methylcarbonate-water saturation gas is drawn from vapor-liquid separation section upper side, and the liquid phase through obtaining after the vapor-liquid separation again after the condensation is thick product methyl-carbonate, and the gas of incoagulability uses as raw material CO after the circular treatment supercharging again.Liquid phase-solid phase and the minimal amounts of dissolved gas in liquid phase then flows downward from the annular space between two pipes because of density increases in the vapor-liquid separation section, enters reaction tubes from the reaction tubes bottom, finishes the circulation of liquid-solid phase or liquid phase medium.The catalyzer of loss is added mouth 12 from catalyzer and is added aborning, adds mouth and only opens when adding catalyzer.
Embodiment 1:
Adopt structure of reactor shown in the accompanying drawing of the present utility model, reaction tubes diameter of inner pipe 32mm, outer tube diameter 50mm, two length of tube are 800mm, and gas distributor is equipped with in interior pipe ingress, and sparger perforate aperture is 1.5mm, percentage of open area 40%; Vapor-liquid separation section diameter 100mm, length 400mm.In this reactor, be incorporated with liquid-phase oxidation carbonylation Synthesis of dimethyl carbonate special-purpose catalyst 100g, add methyl alcohol 800g with pump, starting the logical CO of compressor keeps about system pressure 1.2Mpa, make reaction solution rise to 120 ℃ toward the interior 0.3Mpa low-pressure steam that feeds of reactor heating coil, the Adjustment System pressure-stabilisation is at scope 2.0Mpa, feed O2 and begin reaction, keep O2 content 3%, tail gas air speed 350～600hr
-1Collect thick product methyl-carbonate in the separator behind gas condenser, CO gas after the separation is taken off recycling use again behind the CO2, after one hour, system enters steady state, the thick group of products that obtains in separator becomes: methyl alcohol 75.0%, methylcarbonate 16.0%, water 9.0%, other organic by-products total amount is less than 0.05%.This reactor operation is after 8 hours, and catalyst production is 1.02Kg.DMC/Kg.Cat.h, moves after 96 hours, and catalyst production is 0.57Kg.DMC/Kg.Cat.h, moves after 240 hours, and catalyst production is 0.57Kg.DMC/Kg.Cat.h.
Embodiment 2:
Adopt structure of reactor shown in the accompanying drawing of the present utility model, reaction tubes diameter of inner pipe 400mm, outer tube diameter 500mm, interior length of tube 10800mm, outer length of tube 12000mm, gas distributor is equipped with in interior pipe ingress, sparger perforate aperture is 2.5mm, percentage of open area 60%; Vapor-liquid separation section diameter 1600mm, length 4000mm.In this reactor, be incorporated with liquid-phase oxidation carbonylation Synthesis of dimethyl carbonate special-purpose catalyst 200Kg, add methyl alcohol 1600Kg with pump, make reaction solution rise to 120 ℃ toward the interior 0.3Mpa low-pressure steam that feeds of reactor heating coil, the Adjustment System pressure-stabilisation is at scope 1.8～2.5Mpa, feed CO/O2 and begin reaction, keep O2 content 3.5%, tail gas air speed scope 350～550hr
-1Collect thick product methyl-carbonate in the separator behind gas condenser, CO gas after the separation is taken off recycling use again behind the CO2,2.5 after hour, system enters steady state, the thick group of products that obtains in separator becomes: methyl alcohol 73.8%, methylcarbonate 17.10%, water 8.9%, other organic by-products total amount is less than 0.05%.This reactor operation is after 8 hours, and catalyst production is Kg.DMC/Kg.Cat.h, moves after 96 hours, and catalyst production is 0.66Kg.DMC/Kg.Cat.h, moves after 240 hours, and catalyst production is 0.59Kg.DMC/Kg.Cat.h.
Embodiment 3:
Adopt structure of reactor shown in the accompanying drawing of the present utility model, reaction tubes diameter of inner pipe 400mm, outer tube diameter 500mm, interior length of tube 10800mm, outer length of tube 12000mm, gas distributor is equipped with in interior pipe ingress, sparger perforate aperture is 2.5mm, percentage of open area 60%; Vapor-liquid separation section diameter 1600mm, length 4000mm.In this reactor, be incorporated with liquid-phase oxidation carbonylation Synthesis of dimethyl carbonate special-purpose catalyst 200Kg, add methyl alcohol 1600Kg with pump, make reaction solution rise to 120 ℃ toward the interior 0.3Mpa low-pressure steam that feeds of reactor heating coil, the Adjustment System pressure-stabilisation is at 1.8～2.5Mpa, feed CO/CO2/O2 and begin reaction, wherein CO2 content 12.6%.Keep O2 content 3.5%, tail gas air speed scope 350～550hr
-1Collect thick product methyl-carbonate in the separator behind gas condenser, CO gas after the separation is taken off recycling use again behind the CO2,2.5 after hour, system enters steady state, the thick group of products that obtains in separator becomes: methyl alcohol 75.10%, methylcarbonate 15.20%, water 9.70%, other organic by-products total amount is less than 0.05%.This reactor operation is after 8 hours, and catalyst production is 0.680Kg.DMC/Kg.Cat.h, moves after 96 hours, and catalyst production is 0.55Kg.DMC/Kg.Cat.h, moves after 240 hours, and catalyst production is 0.54Kg.DMC/Kg.Cat.h.
Claims (2)
1, the special-purpose inner circulation reactor of liquid-phase oxidation carbonylation Synthesis of dimethyl carbonate, mainly form by tubular reactor and the return line that is attached thereto, it is characterized in that, reaction tubes is nested with return line is coaxial, interior pipe is reaction tubes, gap between interior pipe and the outer tube is a return line, and the epimere enlarged tube of two pipes is the vapor-liquid separation section; Two coaxial valve outer tubes upper end links to each other with vapor-liquid separation section bottom, and the lower end is provided with material inlet and drain hole, and the vapor-liquid separation section has pneumatic outlet.
2, according to the special-purpose inner circulation reactor of the described liquid-phase oxidation carbonylation Synthesis of dimethyl carbonate of claim 1, end entrance is provided with gas distributor and catalyzer is added mouth under the reaction tubes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200320104432 CN2685336Y (en) | 2003-12-17 | 2003-12-17 | Special internal circulating reactor for combining liquid phase carbo oxide into dimethylester carbonate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200320104432 CN2685336Y (en) | 2003-12-17 | 2003-12-17 | Special internal circulating reactor for combining liquid phase carbo oxide into dimethylester carbonate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN2685336Y true CN2685336Y (en) | 2005-03-16 |
Family
ID=34661553
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200320104432 Expired - Lifetime CN2685336Y (en) | 2003-12-17 | 2003-12-17 | Special internal circulating reactor for combining liquid phase carbo oxide into dimethylester carbonate |
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| Country | Link |
|---|---|
| CN (1) | CN2685336Y (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101357890B (en) * | 2008-09-17 | 2011-06-01 | 西安交通大学 | Methyl carbonate synthesis and refining technique using heat pump technique and apparatus thereof |
-
2003
- 2003-12-17 CN CN 200320104432 patent/CN2685336Y/en not_active Expired - Lifetime
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101357890B (en) * | 2008-09-17 | 2011-06-01 | 西安交通大学 | Methyl carbonate synthesis and refining technique using heat pump technique and apparatus thereof |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C56 | Change in the name or address of the patentee |
Owner name: SOUTHWEST RESEARCH + DESIGN INSTITUTE OF CHEMICAL Free format text: FORMER NAME: SOUTHWEST RESEARCH + DESIGN INSTITUTE OF CHEMICAL INDUSTRY |
|
| CP01 | Change in the name or title of a patent holder |
Address after: 445 box 610229, South Airport Road, Sichuan, Chengdu Patentee after: Southwest Chemical Research & Design Institute Co., Ltd. Address before: 445 box 610229, South Airport Road, Sichuan, Chengdu Patentee before: Xinan Chemical Research & Design Inst. |
|
| C17 | Cessation of patent right | ||
| CX01 | Expiry of patent term |
Expiration termination date: 20131217 Granted publication date: 20050316 |