CN102807490B - System for treating and recovering dimethyl oxalate - Google Patents
System for treating and recovering dimethyl oxalate Download PDFInfo
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- CN102807490B CN102807490B CN201210314905.7A CN201210314905A CN102807490B CN 102807490 B CN102807490 B CN 102807490B CN 201210314905 A CN201210314905 A CN 201210314905A CN 102807490 B CN102807490 B CN 102807490B
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- dmo
- reaction system
- dimethyl oxalate
- nitrogen
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Abstract
The invention provides a system for treating and recovering dimethyl oxalate. The system comprises a carbonylation system, wherein the carbonylation system comprises a DMO (Dimethyl Oxalate) scrubber tower, a DMO recovering tower, a circular cooler, a recovering tower reboiler, a DMO product tank, a scrubber tower reboiler, a DMO crude product tank, a nitrogen gas heater and a DMO recovering tank, which are mutually communicated through a pipeline; an output end of the carbonylation system is connected with an input end of a hydrogenation reaction system; an input end of the carbonylation system is connected with an output end of a nitrogen gas header pipe for inputting nitrogen gas; an input port of the DMO recovering tank is respectively communicated with each device in the carbonylation system through pipelines; and a circulating pump is arranged on a connecting pipeline between the DMO recovering tank and the DMO crude product tank. According to the nitrogen gas heater disclosed by the invention, the whole system can be used for automatically treating a dimethyl oxalate crystalline and is very convenient and has no influence on the running of the whole process.
Description
Technical field
The present invention relates to processing and recovery system in ethylene glycol production technique, specifically a kind of system that can process dimethyl oxalate crystallization and recovery.
Background technology
It is as follows that synthetic gas is prepared ethylene glycol main technique: CO gas phase is under methyl nitrite participates in, coupling, regeneration, catalytic cycle dimethyl oxalate processed (being called for short DMO), DMO repeated hydrogenation generating glycol (being called for short EG), obtains purified ethylene glycol by rectifying separation.
Dimethyl oxalate reaction formula is
cO+2CH
3oNO-→ (COOCH
3)
2+ 2NO
It take CO as raw material, and under strong oxidizer MN participates in, temperature of reaction is 120-140 ℃, and normal pressure carries out, and catalyzer is Pd/Al
2o
3, reactor is fixed-bed reactor.
Side reaction Formed dimethyl phthalate (DMC), its equation is:
CO?+?2CH
3ONO?—→CH
3OCOOCH
3?+?2NO
In production, DMO, DMC, methyl alcohol, nitrogen, CO, NO, CH
3the gases such as ONO, after oxonation, enter DMO scrubber tower, and DMO, DMC and methyl alcohol separate with liquid form at tower bottom, and remaining gas goes out through tower head, and then DMO separates under DMO recovery tower.But in actual production, due to steam fluctuation etc. in operation, and pipeline adjoining pipe holding temperature is inadequate, especially at the bottom of scrubber tower, in methanol solution, DMO content is greater than more than 35%, often causes under DMO scrubber tower and recovery tower underground pipelines (comprising valve) DMO crystallization to such an extent as to device stop.At present, the normal treating method adopting has two kinds: 1, steam is from the heating of pipeline valve outer surface, and the treatment time is long; 2, connect steam and manage temporarily, with steam direct heating, blow down to recover, but DMO decomposes in hot steam, only have outer row's burning disposal.Though above-mentioned two kinds of methods can solve the problem of crystallization to a certain extent, but very inconvenient, had a strong impact on the normal operation of system, reduced the efficiency of producing ethylene glycol.
Summary of the invention
The object of the present invention is to provide a kind of dimethyl oxalate that can conveniently process the crystallization of ethylene glycol production mesoxalic acid dimethyl ester to process and recovery system.
The present invention has adopted following technical scheme: a kind of processing of dimethyl oxalate and recovery system, this system comprises carbonylation reaction system, described carbonylation reaction system comprises DMO scrubber tower, DMO recovery tower, recirculation cooler, recovery tower reboiler, DMO product groove, scrubber tower reboiler, DMO crude product groove, rare gas element well heater and DMO accumulator tank, between described each device, through pipeline, be interconnected, the output terminal of described carbonylation reaction system is connected with hydrogenation reaction system input terminus, the input terminus of described carbonylation reaction system with for inputting the output terminal of the nitrogen header pipe of nitrogen, be connected, described nitrogen heater is located on the connection line between nitrogen header pipe and described carbonylation reaction system, the input aperture of DMO accumulator tank is communicated with each device in described carbonylation reaction system respectively through pipeline, connection line between described DMO accumulator tank and DMO crude product groove is provided with recycle pump.
beneficial effect: the present invention adds after nitrogen heater and DMO accumulator tank in original carbonylation reaction system, under the effect of hot nitrogen, DMO fast liquefying is flowed in DMO crude product groove, pan tank, accumulator tank or tower, whole system can be processed the problem of dimethyl oxalate crystallization, very convenient and do not affect the running of whole technique.
Accompanying drawing explanation
Fig. 1 is connection diagram of the present invention.
In figure: 1, nitrogen header pipe, 2, nitrogen heater, 3, DMO scrubber tower, 4, scrubber tower reboiler, 5, recirculation cooler, 6, crude product groove, 7, DMO recovery tower, 8, recovery tower reboiler, 9, DMO product groove, 10, DMO accumulator tank, 11, hydrogenation reaction system
12, recycle pump a, 13, recycle pump b, 14, valve a, 15, valve b.
Embodiment
Below in conjunction with accompanying drawing, be described in further detail:
As shown in Figure 1, this system comprises carbonylation reaction system conventional in prior art, DMO described in the present invention is writing a Chinese character in simplified form of dimethyl oxalate, the input terminus of carbonylation reaction system is connected with hydrogenation reaction system 11 with nitrogen header pipe 1 respectively, carbonylation reaction system comprises DMO scrubber tower 3, scrubber tower reboiler 4, recirculation cooler 5, DMO crude product groove 6, DMO recovery tower 7, recovery tower reboiler 8 and DMO product groove 9, between each device, with pipeline, be interconnected, pipeline adopts aluminium section bar, on the connection line of each device, be equipped with 1 to 3 valve, this system also comprises gas heater and DMO accumulator tank 10, because other rare gas elementes are not easy to extract in industrial production, therefore use nitrogen heater 2 in actual production, nitrogen heater 2 is located on the pipeline between nitrogen header pipe 1 and carbonylation reaction system, DMO accumulator tank 10 through pipeline respectively with nitrogen heater 2, carbonylation reaction system is connected with hydrogenation reaction system 11, wherein DMO accumulator tank 10 is also provided with recycle pump a12 with on pipeline that in carbonylation reaction system, DMO crude product groove 6 is connected, on the connection line of DMO crude product groove 6 and recirculation cooler 5, be also provided with recycle pump b13, when causing pipeline or valve blockage because of DMO crystallization, while first squeezing into certain methyl alcohol in order to dissolving in DMO accumulator tank 10, use, open valve a14 and the valve b15 at nitrogen heater 2 two ends, through nitrogen header pipe 1 nitrogen out, enter and in nitrogen heater 2, be heated to 100 ~ 140 degree, pressure-controlling is to 0.5Mpa, DMO scrubber tower presses 3 to be 0.3Mpa, because DMO fusing point is 54 ℃, therefore only need operation respective valves, under the effect of hot nitrogen, DMO fast liquefying is flowed through DMO crude product groove 6, DMO product groove 9, DMO recovery tower 7 flows in DMO accumulator tank 10, because having methyl alcohol can dissolve rear recovery in DMO accumulator tank 10 continues to use, not only environmental protection but also cost-saving, single valve or a plurality of valve crystallization can be blown down crystallization with the nitrogen after heating by controlling the switch of corresponding valve, so just can solve very easily the problem of DMO crystallization in pipeline, reach the object of fast processing and recovery.
Claims (3)
1. the processing of a dimethyl oxalate and recovery system, this system comprises carbonylation reaction system, described carbonylation reaction system comprises DMO scrubber tower, DMO recovery tower, recirculation cooler, recovery tower reboiler, DMO product groove, scrubber tower reboiler and DMO crude product groove, between described each device, through pipeline, be interconnected, the output terminal of described carbonylation reaction system is connected with hydrogenation reaction system input terminus, the input terminus of described carbonylation reaction system with for inputting the output terminal of the nitrogen header pipe of nitrogen, be connected, it is characterized in that: this system also comprises nitrogen heater and DMO accumulator tank, described nitrogen heater is located on the connection line between nitrogen header pipe and described carbonylation reaction system, the input aperture of DMO accumulator tank is connected with each device and described nitrogen heater in described carbonylation reaction system respectively through pipeline, connection line between described DMO accumulator tank and DMO crude product groove is provided with recycle pump, on connection line between described nitrogen heater and DMO accumulator tank and each device, be equipped with valve.
2. the processing of dimethyl oxalate according to claim 1 and recovery system, is characterized in that: described nitrogen heater thermal source is 0.8 ~ 1Mpa.
3. the processing of dimethyl oxalate according to claim 1 and 2 and recovery system, is characterized in that: the pressure of described scrubber tower and recovery tower is 0.2 ~ 0.4Mpa.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201210314905.7A CN102807490B (en) | 2012-08-30 | 2012-08-30 | System for treating and recovering dimethyl oxalate |
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|---|---|---|---|
| CN201210314905.7A CN102807490B (en) | 2012-08-30 | 2012-08-30 | System for treating and recovering dimethyl oxalate |
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| CN102807490A CN102807490A (en) | 2012-12-05 |
| CN102807490B true CN102807490B (en) | 2014-08-20 |
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| CN201210314905.7A Active CN102807490B (en) | 2012-08-30 | 2012-08-30 | System for treating and recovering dimethyl oxalate |
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| CN102898305B (en) * | 2012-10-30 | 2014-07-16 | 安徽淮化股份有限公司 | Dimethyl oxalate rectifying equipment |
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|---|---|---|---|---|
| US4629806A (en) * | 1981-01-23 | 1986-12-16 | Union Carbide Corporation | Vapor state formation of diesters of oxalic acid |
| EP0802175A1 (en) * | 1996-04-16 | 1997-10-22 | Ube Industries, Ltd. | Process for preparation of dialkyl oxalate |
| JP2003073333A (en) * | 2001-08-31 | 2003-03-12 | Ube Ind Ltd | Method for producing carbonic acid ester and oxalic acid ester |
| 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 |
| CN101381309B (en) * | 2008-10-24 | 2012-10-24 | 华东理工大学 | Method for separating low concentration dimethyl carbonate by double-column process in dimethyl oxalate process |
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Effective date of registration: 20210317 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 Province, Huainan city tianjia'an District Quanshan Patentee before: ANHUI HUAIHUA CHEMICAL GROUP Co.,Ltd. |