CN102898305A - Dimethyl oxalate rectifying equipment - Google Patents
Dimethyl oxalate rectifying equipment Download PDFInfo
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- CN102898305A CN102898305A CN2012104241370A CN201210424137A CN102898305A CN 102898305 A CN102898305 A CN 102898305A CN 2012104241370 A CN2012104241370 A CN 2012104241370A CN 201210424137 A CN201210424137 A CN 201210424137A CN 102898305 A CN102898305 A CN 102898305A
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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 are (COOCH
3)
2, the fusing point of dimethyl oxalate is 57 ℃, boiling point is 164.5 ℃, is solid under the normal temperature.The reactions steps of preparation 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 the rectifying tower separates the methyl alcohol and the by product methylcarbonate that mix in the dimethyl oxalate, and gained sterling dimethyl oxalate enters the hydrogenation process hydrogenation again and obtains the ethylene glycol crude product.The present institute of applicant operation technique is: 1) the dimethyl oxalate feed liquid enters rectifying tower 1 ', separates under certain temperature and pressure; 2) gained rectifying tower 1 ' tower bottoms enters dimethyl oxalate transport pipe 3 ', and enter the thermosyphon reboiler 2 ' entrance that communicates with dimethyl oxalate transport pipe 3 ' by thermosiphon principle, in reboiler 2 ' with the high-temperature steam heat exchange, liquid phase descending in gained tower bottoms steam and the rectifying tower 1 ' is carried out heat and mass transport, after the tower reactor temperature reached certain temperature, the tower bottoms of finishing separation entered dimethyl oxalate storage tanks 4 ' by dimethyl oxalate transport pipe 3 ' mutually.
Dimethyl oxalate will crystallization when 55 ℃ of left and right sides, and the technology of using now according to the applicant is being produced tower bottom of rectifying tower liquid continuous pulp discharge when stablize, this moment since feed liquid is mobile and rectifying tower reactor liquid temp more than 100 ℃, dimethyl oxalate is non-crystallizable.If but run into some special statuss, as: when the temperature that inlet amount changes, rectifying tower is interior, pressure, liquid level etc. changed, the dimethyl oxalate liquid phase of continuous pulp discharge can not reach required purity, just needed the discontinuous discharge of tower reactor this moment.At tower bottoms not in the gap of discharge, feed liquid in the whole dimethyl oxalate transport pipe 6 ' is with regard to stop motion, and temperature also slowly descends, and the dimethyl oxalate that rests in the 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 provides a kind of dimethyl oxalate rectifying device, and this rectifying device can be avoided dimethyl oxalate Crystallization Plugging pipeline when carrying out the discontinuous discharge of dimethyl oxalate tower bottoms or production when abending discharge.
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 links to each other with dimethyl oxalate storage tanks entrance by the dimethyl oxalate transport pipe, the dimethyl oxalate transport pipe also links to each other with the first entrance, connecting place is first node, the first pipe outlet links to each other with the reboiler entrance, the reboiler outlet links to each other with the steam inlet tube of rectifier bottoms, the dimethyl oxalate transport pipe is equipped with the first valve at first node to the part between the dimethyl oxalate storage tanks entrance, the dimethyl oxalate transport pipe is connected with nitrogen gas delivery-line at the first valve to the part between the dimethyl oxalate storage tanks entrance, and the second valve is installed on the nitrogen gas delivery-line.
Dimethyl oxalate rectifying device of the present invention, wherein said dimethyl oxalate transport pipe is equipped 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 cat head 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 links to each other with the material inlet of recooler, the material outlet of recooler links to each other with isolate storage tanks entrance, liquid header is collected from the phlegma of the first condenser, the liquid header liquid exit is parallel with second pipe entrance and the 3rd entrance, the second pipe outlet links to each other with the liquid inlet of liquid distributor, the 3rd pipe outlet communicates with the isolate storage tanks, and the 3rd entrance place of liquid header is equipped with flowrate control valve.Liquid header and liquid distributor all adopt the technology in the existing rectifying device.
The using method of dimethyl oxalate rectifying device of the present invention is as follows:
1, the dimethyl oxalate feed liquid with 63 ~ 67 ℃ of temperature passes into rectifying tower, and wherein the 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 about 1.5% and other impurity of trace;
2, tower bottom of rectifying tower liquid enters the dimethyl oxalate transport pipe, enter thermosyphon reboiler by thermal siphon again, it in reboiler is 175 ~ 185 ℃ steam heat-exchanging with temperature, descending liquid phase is carried out heat and mass transport in gained tower bottoms steam and the rectifying tower, after the tower reactor temperature reaches 140 ~ 150 ℃, dimethyl oxalate in the first valve open, dimethyl oxalate transport pipe enters the 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, collect through liquid header, part phlegma passes through second pipe, evenly spray after entering liquid distributor as the phegma of rectifying tower cat head, carry out heat and mass transport with the gas that rises in the rectifying tower, keep 50 ~ 60 ℃ of tower top temperatures, another part phlegma is by the 3rd pipeline, enter the isolate storage tanks as overhead extraction liquid, the 3rd entrance is equipped with flowrate control valve, control cat head produced quantity, a small amount of uncooled gas continues to enter recooler, with temperature be-4 ~ 6 ℃ chilled brine heat exchange condensation, condensation gained liquid enters the isolate storage tanks;
4, when tower bottom of rectifying tower temporarily not during discharge, the first valve closes, open the second valve, pass into normal temperature in the dimethyl oxalate transport pipe, pressure is the nitrogen of 0.4 ~ 0.5MPa, liquid phase dimethyl oxalate in the 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: connect nitrogen gas delivery-line at the dimethyl oxalate transport pipe, when the discontinuous discharge of tower bottom of rectifying tower or need to temporarily stop the dimethyl oxalate discharge time, close the first valve, slowly open the second valve, with nitrogen the dimethyl oxalate in the dimethyl oxalate transport pipe is pressed in the storage tanks, after having feed liquid to discharge in the dimethyl oxalate transport pipe, do not close again the second valve family of power and influence, 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 the dimethyl oxalate transport pipe, not only guarantee 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 installed in the first condenser in the rectifying tower, can save the space, simultaneously because condenser is installed in cat head, can more effective adjusting tower top temperature, and prevent that heavy component from steaming from cat head, guaranteed product quality.
Below in conjunction with accompanying drawing dimethyl oxalate rectifying device of the present invention is described further.
Description of drawings
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, the outlet of rectifying tower 1 tower bottoms links to each other with dimethyl oxalate storage tanks 4 entrances by dimethyl oxalate transport pipe 3, the dimethyl oxalate transport pipe 3 outer trace pipes that are equipped with, dimethyl oxalate transport pipe 3 also links to each other with the first pipeline 71 entrances, connecting place is first node 8,71 outlets of the first pipeline link to each other with reboiler 2 entrances, reboiler 2 outlets link to each other with the steam inlet tube of rectifying tower 1 bottom, dimethyl oxalate transport pipe 3 is equipped 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 on the nitrogen gas delivery-line 10, the dimethyl oxalate rectifying device, also comprise recooler 5 and isolate storage tanks 6, rectifying tower inside is positioned at cat head 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 links to each other with the material inlet of recooler 5, the material outlet of recooler 5 links to each other with isolate storage tanks 6 entrances, liquid header 12 is collected from the phlegma of 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 link to each other with the liquid inlet of liquid distributor 13,73 outlets of the 3rd pipeline communicate with isolate storage tanks 6, and the 3rd pipeline 73 ingress are equipped with flowrate control valve 93.
Above-described embodiment is described preferred implementation of the present invention; be not that scope of the present invention is limited; design under the prerequisite of spirit not breaking away 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 claims of the present invention.
Claims (3)
1. 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 links to each other with dimethyl oxalate storage tanks (4) entrance by dimethyl oxalate transport pipe (3), dimethyl oxalate transport pipe (3) also links to each other with the first pipeline (71) entrance, connecting place is first node (8), the first pipeline (71) outlet links to each other with reboiler (2) entrance, reboiler (2) outlet links to each other with the steam inlet tube of rectifying tower (1) bottom, dimethyl oxalate transport pipe (3) is positioned at first node (8) and 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, and the second valve (92) is installed on the nitrogen gas delivery-line (10).
2. dimethyl oxalate rectifying device according to claim 1 is characterized in that: the outer trace pipe that is equipped with of dimethyl oxalate transport pipe (3).
3. dimethyl oxalate rectifying device according to claim 2, it is characterized in that: also comprise recooler (5) and isolate storage tanks (6), rectifying tower inside is positioned at cat head 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) links to each other with the material inlet of recooler (5), the material outlet of recooler (5) links to each other with isolate storage tanks (6) entrance, liquid header (12) is collected from the phlegma of 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 links to each other with the liquid inlet of liquid distributor (13), the 3rd pipeline (73) outlet communicates with isolate storage tanks (6), and the 3rd pipeline (73) ingress is equipped with flowrate control valve (93).
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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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| 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 true CN102898305A (en) | 2013-01-30 |
| CN102898305B CN102898305B (en) | 2014-07-16 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112174821A (en) * | 2020-09-04 | 2021-01-05 | 中盐安徽红四方股份有限公司 | Rectification method of dimethyl oxalate |
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|---|---|---|---|---|
| CN101190884A (en) * | 2006-11-21 | 2008-06-04 | 上海焦化有限公司 | Method for synthesizing dimethyl oxalate and coproducing dimethyl carbonate |
| CN101934210A (en) * | 2010-09-13 | 2011-01-05 | 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 |
| CN102807490A (en) * | 2012-08-30 | 2012-12-05 | 安徽淮化股份有限公司 | System for treating and recovering dimethyl oxalate |
| CN202786065U (en) * | 2012-08-30 | 2013-03-13 | 安徽淮化股份有限公司 | Dimethyl oxalate treatment and recovery system |
| CN202961932U (en) * | 2012-10-30 | 2013-06-05 | 安徽淮化股份有限公司 | Rectification equipment for dimethyl oxalate |
-
2012
- 2012-10-30 CN CN201210424137.0A patent/CN102898305B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101190884A (en) * | 2006-11-21 | 2008-06-04 | 上海焦化有限公司 | Method for synthesizing dimethyl oxalate and coproducing dimethyl carbonate |
| CN101934210A (en) * | 2010-09-13 | 2011-01-05 | 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 |
| CN102807490A (en) * | 2012-08-30 | 2012-12-05 | 安徽淮化股份有限公司 | System for treating and recovering dimethyl oxalate |
| CN202786065U (en) * | 2012-08-30 | 2013-03-13 | 安徽淮化股份有限公司 | Dimethyl oxalate treatment and recovery system |
| CN202961932U (en) * | 2012-10-30 | 2013-06-05 | 安徽淮化股份有限公司 | Rectification equipment for dimethyl oxalate |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112174821A (en) * | 2020-09-04 | 2021-01-05 | 中盐安徽红四方股份有限公司 | Rectification method of dimethyl oxalate |
| 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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| CN102898305B (en) | 2014-07-16 |
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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. |