CN102898305B - Dimethyl oxalate rectifying equipment - Google Patents
Dimethyl oxalate rectifying equipment Download PDFInfo
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- CN102898305B CN102898305B CN201210424137.0A CN201210424137A CN102898305B CN 102898305 B CN102898305 B CN 102898305B CN 201210424137 A CN201210424137 A CN 201210424137A CN 102898305 B CN102898305 B CN 102898305B
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- dimethyl oxalate
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Abstract
The invention discloses dimethyl oxalate rectifying equipment, which relates to chemical product rectifying equipment. Due to the adoption of the rectifying equipment, dimethyl oxalate can be prevented from being crystallized and blocking a pipeline when dimethyl oxalate tower bottoms are discharged discontinuously or discharge is stopped due to abnormal production. The dimethyl oxalate rectifying equipment comprises a rectifying tower, a reboiler and a dimethyl oxalate storing groove, wherein the tower bottoms outlet of the rectifying tower is connected with the inlet of the dimethyl oxalate storing groove through the dimethyl oxalate conveying pipeline; the dimethyl oxalate conveying pipeline is further connected with the inlet of a first pipeline, and the joint is a first node; the outlet of the first pipeline is connected with the inlet of the reboiler; the outlet of the reboiler is connected with a steam inlet pipe at the bottom of the rectifying tower; a first valve is arranged on a part of the dimethyl oxalate conveying pipeline which is positioned between the first node and the inlet of the dimethyl oxalate storage groove; a nitrogen gas conveying pipeline is connected to a part of the dimethyl oxalate conveying pipeline which is positioned between the first valve and the inlet of the dimethyl oxalate storage groove; and a second valve is arranged on the nitrogen gas conveying pipeline.
Description
Technical field
The present invention relates to a kind of Chemicals rectifying device, particularly relate to a kind of dimethyl oxalate rectifying device.
Background technology
Dimethyl oxalate is with synthetic gas methyl alcohol, NO, CO and O
2intermediate product during for waste ethylene glycol, its molecular formula is (COOCH
3)
2, the fusing point of dimethyl oxalate is 57 ℃, boiling point is 164.5 ℃, is solid under normal temperature.The reactions steps of preparing dimethyl oxalate comprises that esterification (obtains methyl nitrite CH
3oNO) and oxonation (acquisition dimethyl oxalate) two portions, its main chemical reactions formula is as follows:
2NO+2CH
3OH+1/2O
2→2CH
3ONO+H
2O （1）
2CH
3ONO+2CO→(COOCH
3)
2+2NO （2）
Step (2) gained dimethyl oxalate feed liquid will pass in rectifying tower separates the methyl alcohol mixing in dimethyl oxalate and by product methylcarbonate, and gained sterling dimethyl oxalate enters hydrogenation process hydrogenation again and obtains ethylene glycol crude product.The present institute of applicant operation technique is: 1) dimethyl oxalate feed liquid enters rectifying tower 1 ', carries out separation under certain temperature and pressure; 2) gained rectifying tower 1 ' tower bottoms enters dimethyl oxalate transport pipe 3 ', and by thermosiphon principle, enter the thermosyphon reboiler 2 ' entrance communicating with dimethyl oxalate transport pipe 3 ', in reboiler 2 ' with high-temperature steam heat exchange, liquid phase descending in gained tower bottoms steam and rectifying tower 1 ' is carried out heat and mass transport, tower reactor temperature reaches after certain temperature, completes separated tower bottoms and by dimethyl oxalate transport pipe 3 ', enters dimethyl oxalate storage tanks 4 ' mutually.
Dimethyl oxalate will crystallization when 55 ℃ of left and right, and the technology of using now according to applicant is being produced tower bottom of rectifying tower liquid continuous pulp discharge while stablize, now due to feed liquid is mobile and also rectifying tower reactor liquid temp more than 100 ℃, dimethyl oxalate is non-crystallizable.If but run into some special statuss, as: when the temperature in inlet amount change, rectifying tower, pressure, liquid level etc. change, the dimethyl oxalate liquid phase of continuous pulp discharge can not reach required purity, now just needs the discontinuous discharge of tower reactor.At tower bottoms not in the gap of discharge, feed liquid in whole dimethyl oxalate transport pipe 6 ' is with regard to stop motion, and temperature also slowly declines, and the dimethyl oxalate resting in dimethyl oxalate transport pipe 6 ' is easy to crystallization, blocking pipe, thus the carrying out of subsequent production affected.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of dimethyl oxalate rectifying device, and this rectifying device, when carrying out the discontinuous discharge of dimethyl oxalate tower bottoms or when production abends discharge, can be avoided dimethyl oxalate Crystallization Plugging pipeline.
Dimethyl oxalate rectifying device of the present invention, comprise rectifying tower, reboiler and dimethyl oxalate storage tanks, the outlet of tower bottom of rectifying tower liquid is connected with dimethyl oxalate storage tanks entrance by dimethyl oxalate transport pipe, dimethyl oxalate transport pipe is also connected with the first entrance, connecting place is first node, the first pipe outlet is connected with reboiler entrance, reboiler outlet is connected with the steam inlet tube of rectifier bottoms, dimethyl oxalate transport pipe is provided with the first valve at first node to the part between dimethyl oxalate storage tanks entrance, dimethyl oxalate transport pipe is connected with nitrogen gas delivery-line at the first valve to the part between dimethyl oxalate storage tanks entrance, the second valve is installed in nitrogen gas delivery-line.
Dimethyl oxalate rectifying device of the present invention, wherein said dimethyl oxalate transport pipe is provided with trace pipe outward.
Dimethyl oxalate rectifying device of the present invention, also comprise recooler and isolate storage tanks, described rectifying tower inside is positioned at tower top to the part of the top packing section first condenser that has been fixedly connected sequentially from top to bottom, liquid header and liquid distributor, wherein the pneumatic outlet of the first condenser and the material inlet of recooler are connected, the material outlet of recooler is connected with isolate storage tanks entrance, liquid header is collected the phlegma from the first condenser, liquid header liquid exit is parallel with second pipe entrance and the 3rd entrance, second pipe outlet is connected with the liquid inlet of liquid distributor, the 3rd pipe outlet communicates with isolate storage tanks, the 3rd entrance place of liquid header is provided with flowrate control valve.Liquid header and liquid distributor all adopt the technology in existing rectifying device.
The using method of dimethyl oxalate rectifying device of the present invention is as follows:
1, the dimethyl oxalate feed liquid of 63 ~ 67 ℃ of temperature is passed into rectifying tower, wherein dimethyl oxalate feed liquid contains the dimethyl oxalate of mass concentration 30 ~ 40%, the methylcarbonate of the methyl alcohol of mass concentration 63 ~ 67% and mass concentration 1.5% left and right and other impurity of trace;
2, tower bottom of rectifying tower liquid enters dimethyl oxalate transport pipe, by thermal siphon, enter thermosyphon reboiler again, it in reboiler, is the steam heat-exchanging of 175 ~ 185 ℃ with temperature, in gained tower bottoms steam and rectifying tower, descending liquid phase is carried out heat and mass transport, tower reactor temperature reaches after 140 ~ 150 ℃, the first valve open, the dimethyl oxalate in dimethyl oxalate transport pipe enters dimethyl oxalate storage tanks;
3, rectifying tower top gaseous phase in the first condenser with the recirculated cooling water heat exchange condensation of 28 ~ 32 ℃ of temperature, condensation gained liquid flows out the first condenser, through liquid header, collect, part phlegma passes through second pipe, after entering liquid distributor as the phegma of rectifying tower tower top, evenly spray, carry out heat and mass transport with the gas rising in rectifying tower, keep 50 ~ 60 ℃ of tower top temperatures, another part phlegma is by the 3rd pipeline, as overhead extraction liquid, enter isolate storage tanks, the 3rd entrance is provided with flowrate control valve, control tower top produced quantity, a small amount of uncooled gas continues to enter recooler, with temperature be the chilled brine heat exchange condensation of-4 ~ 6 ℃, condensation gained liquid enters isolate storage tanks,
4, when tower bottom of rectifying tower is not temporarily during discharge, the first valve closes, open the second valve, to passing into the nitrogen that normal temperature, pressure are 0.4 ~ 0.5MPa in dimethyl oxalate transport pipe, liquid phase dimethyl oxalate in dimethyl oxalate transport pipe is emptying, prevent that the crystallization of liquid phase dimethyl oxalate from resulting in blockage.
Dimethyl oxalate rectifying device difference from prior art of the present invention is: on dimethyl oxalate transport pipe, connect nitrogen gas delivery-line, when the discontinuous discharge of tower bottom of rectifying tower or need to temporarily stop dimethyl oxalate discharge time, close the first valve, slowly open the second valve, with nitrogen, the dimethyl oxalate in dimethyl oxalate transport pipe is pressed in storage tanks, after having feed liquid to discharge, do not close again the second valve family of power and influence in dimethyl oxalate transport pipe, after production is stable, in the time of need to carrying out normal continuous pulp discharge, open the first valve, can prevent like this dimethyl oxalate Crystallization Plugging pipeline residual in dimethyl oxalate transport pipe, not only guaranteed the continuous and steady operation of producing, also reduced workman's labour intensity simultaneously.
Dimethyl oxalate rectifying device of the present invention, trace pipe can be piping insulation when dimethyl oxalate transport pipe continuous pulp discharge, prevents dimethyl oxalate Crystallization Plugging pipeline.
Dimethyl oxalate rectifying device of the present invention, is arranged on the first condenser in rectifying tower, can save space, simultaneously because condenser is arranged on tower top, can more effective adjusting tower top temperature, and prevent that heavy component from steaming from tower top, guaranteed product quality.
Below in conjunction with accompanying drawing, dimethyl oxalate rectifying device of the present invention is described further.
Accompanying drawing explanation
Fig. 1 is the structural representation of dimethyl oxalate rectifying device of the present invention.
Embodiment
As shown in Figure 1, dimethyl oxalate rectifying device of the present invention, comprise rectifying tower 1, reboiler 2 and dimethyl oxalate storage tanks 4, rectifying tower 1 tower bottoms outlet is connected with dimethyl oxalate storage tanks 4 entrances by dimethyl oxalate transport pipe 3, the outer trace pipe that is provided with of dimethyl oxalate transport pipe 3, dimethyl oxalate transport pipe 3 is also connected with the first pipeline 71 entrances, connecting place is first node 8, the first pipeline 71 outlets are connected with reboiler 2 entrances, reboiler 2 outlets are connected with the steam inlet tube of rectifying tower 1 bottom, dimethyl oxalate transport pipe 3 is provided with the first valve 91 at first node 8 to the part between dimethyl oxalate storage tanks 4 entrances, dimethyl oxalate transport pipe 3 is connected with nitrogen gas delivery-line 10 at the first valve 91 to the part between dimethyl oxalate storage tanks 4 entrances, the second valve 92 is installed in nitrogen gas delivery-line 10, dimethyl oxalate rectifying device, also comprise recooler 5 and isolate storage tanks 6, rectifying tower inside is positioned at tower top to the part of the top packing section first condenser 11 that has been fixedly connected sequentially from top to bottom, liquid header 12 and liquid distributor 13, wherein the pneumatic outlet of the first condenser 11 is connected with the material inlet of recooler 5, the material outlet of recooler 5 is connected with isolate storage tanks 6 entrances, the phlegma that liquid header 12 is collected from the first condenser 11, liquid header 12 liquid exits are parallel with second pipe 72 entrances and the 3rd pipeline 73 entrances, second pipe 72 outlets are connected with the liquid inlet of liquid distributor 13, the 3rd pipeline 73 outlets communicate with isolate storage tanks 6, the 3rd pipeline 73 ingress are provided with flowrate control valve 93.
Above-described embodiment is described the preferred embodiment of the present invention; not scope of the present invention is limited; design under the prerequisite of spirit not departing from the present invention; various distortion and improvement that those of ordinary skills make technical scheme of the present invention, all should fall in the definite protection domain of the claims in the present invention book.
Claims (2)
1. a dimethyl oxalate rectifying device, comprise rectifying tower (1), reboiler (2) and dimethyl oxalate storage tanks (4), it is characterized in that: the outlet of rectifying tower (1) tower bottoms is connected with dimethyl oxalate storage tanks (4) entrance by dimethyl oxalate transport pipe (3), dimethyl oxalate transport pipe (3) is also connected with the first pipeline (71) entrance, connecting place is first node (8), the first pipeline (71) outlet is connected with reboiler (2) entrance, reboiler (2) outlet is connected with the steam inlet tube of rectifying tower (1) bottom, dimethyl oxalate transport pipe (3) is positioned at first node (8), to the part between dimethyl oxalate storage tanks (4) entrance, the first valve (91) is installed, dimethyl oxalate transport pipe (3) is positioned at the first valve (91) and is connected with nitrogen gas delivery-line (10) to the part between dimethyl oxalate storage tanks (4) entrance, the second valve (92) is installed in nitrogen gas delivery-line (10), the outer trace pipe that is provided with of dimethyl oxalate transport pipe (3).
2. dimethyl oxalate rectifying device according to claim 1, it is characterized in that: also comprise recooler (5) and isolate storage tanks (6), rectifying tower inside is positioned at tower top to the part of the top packing section the first condenser (11) that has been fixedly connected sequentially from top to bottom, liquid header (12) and liquid distributor (13), wherein the pneumatic outlet of the first condenser (11) is connected with the material inlet of recooler (5), the material outlet of recooler (5) is connected with isolate storage tanks (6) entrance, liquid header (12) is collected the phlegma from the first condenser (11), liquid header (12) liquid exit is parallel with second pipe (72) entrance and the 3rd pipeline (73) entrance, second pipe (72) outlet is connected with the liquid inlet of liquid distributor (13), the 3rd pipeline (73) outlet communicates with isolate storage tanks (6), the 3rd pipeline (73) ingress is provided with flowrate control valve (93).
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|---|---|---|---|
| CN201210424137.0A CN102898305B (en) | 2012-10-30 | 2012-10-30 | Dimethyl oxalate rectifying equipment |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210424137.0A CN102898305B (en) | 2012-10-30 | 2012-10-30 | Dimethyl oxalate rectifying equipment |
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| CN102898305A CN102898305A (en) | 2013-01-30 |
| CN102898305B true CN102898305B (en) | 2014-07-16 |
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| CN112174821B (en) * | 2020-09-04 | 2023-08-18 | 中盐安徽红四方股份有限公司 | Rectification method of dimethyl oxalate |
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| CN202961932U (en) * | 2012-10-30 | 2013-06-05 | 安徽淮化股份有限公司 | Rectification equipment for dimethyl oxalate |
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| CN101190884B (en) * | 2006-11-21 | 2011-02-23 | 上海焦化有限公司 | Method for synthesizing dimethyl oxalate and coproducing dimethyl carbonate |
| CN101934210B (en) * | 2010-09-13 | 2013-01-09 | 安徽淮化股份有限公司 | Carbonylation reactor suitable for industrial production of ethylene glycol |
| CN202322670U (en) * | 2011-11-23 | 2012-07-11 | 安徽淮化股份有限公司 | Anti-curing device system for dimethyl oxalate in industrial production of glycol |
| CN202786065U (en) * | 2012-08-30 | 2013-03-13 | 安徽淮化股份有限公司 | Dimethyl oxalate treatment and recovery system |
| CN102807490B (en) * | 2012-08-30 | 2014-08-20 | 安徽淮化股份有限公司 | System for treating and recovering dimethyl oxalate |
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| CN202961932U (en) * | 2012-10-30 | 2013-06-05 | 安徽淮化股份有限公司 | Rectification equipment for dimethyl oxalate |
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Effective date of registration: 20210318 Address after: 201102 rooms 615-618, 6th floor, T1 / F, chengkai center, Lane 166, Minhong Road, Minhang District, Shanghai Patentee after: PUJING CHEMICAL INDUSTRY (SHA)LIMITED Address before: 232038 Anhui Huainan Tian Jia An District Quanshan Anhui Huaihua Limited by Share Ltd technology research and Development Center Patentee before: ANHUI HUAIHUA CHEMICAL GROUP Co.,Ltd. |