CN1271721A - Process for pressure separation of mathanol and dimethyl carbonate azeotrope - Google Patents
Process for pressure separation of mathanol and dimethyl carbonate azeotrope Download PDFInfo
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- CN1271721A CN1271721A CN 00107115 CN00107115A CN1271721A CN 1271721 A CN1271721 A CN 1271721A CN 00107115 CN00107115 CN 00107115 CN 00107115 A CN00107115 A CN 00107115A CN 1271721 A CN1271721 A CN 1271721A
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Abstract
A process for the pressure separation of methanol-dimethyl carbonate azeotrope features that the pressure generated by material itself in pressure rectification tower is used to separate methanol and small quantity of dimethyl carbonate at tower top and the dimethyl carbonate with purity of over 97% is separated at tower bottom and then further rectified in rectifying tower for higher purity. Its advantages are low investment to equipment, low power consumption, few control units, easily controlled pressure in tower, and wide range of pressure.
Description
The invention belongs to the methylcarbonate separation technology field of (being called for short DMC), specifically a kind of method of pressurize separation of methanol and dimethyl carbonate azeotrope.
The industrial process of methylcarbonate (DMC) mainly contains liquid phase methanol carbonyl oxidation style, gas-phase methanol carbonyl oxidation style, ester-interchange method etc., and wherein ester-interchange method is the simplest on flow process.Domestic production DMC mainly adopts ester-interchange method at present.But no matter adopt which kind of method, methyl alcohol all can not transform fully during industrial production DMC, and initial products obtained therefrom all is the mixture of methyl alcohol and DMC.Under atmospheric pressure,, adopt common rectificating method, want to separate purification DMC and be difficult to accomplish because DMC and methyl alcohol formation binary constant boiling mixture (DMC30%, methyl alcohol 70%) by weight.At present the separating technology of prior art bibliographical information has: extractive distillation method, azeotropic distillation, membrane separation process, utilize rare gas element pressure distillation method and freeze crystallization etc.Wherein that is that all right is ripe for membrane separation technique, does not see the industrialization report.The extraction and fractionation method, the extraction agent consumption is big, reclaims the energy consumption height of extraction agent, and the rate of recovery of DMC is low.Though azeotropic distillation has superior part than the extractive distillation method, the nonvariant boiling reagent loss is also inevitably arranged, the quality of DMC is difficult to guarantee that operating process is long that control unit is many.Utilize rare gas element pressure distillation method to avoid many inadvisable parts in extractive distillation method and the azeotropic distillation, formed self simple and convenient characteristic, the DMC quality product of ester-interchange method production, material energy consumption level are stepped on a new stage.But utilize rare gas element pressurization isolation technique that shortcoming is also arranged: the working pressure of (1) system must be relatively stable, allow fluctuation range narrower, thereby operation easier is big.(2) the saturated branch of overhead fraction forces down, and condensing temperature requires low, and phlegma is hung oneself and is heated to the bubble point backflow, and a cold heat energy consumption is high.(3) need acquire inert gas compressor, surge tank equal pressure container, routine maintenance expense height, power consumption is big, and gas purity requires high.
The object of the present invention is to provide a kind of methyl alcohol of novelty and the separation method of dimethyl carbonate azeotrope, the pressure that it utilizes material reaction self to produce makes system's pressurization, thereby methyl alcohol is separated with DMC, and in order to obtain highly purified DMC, this separation method also comprises the treating process of DMC.
Accompanying drawing is a process flow sheet of the present invention.
Among the figure, T1, T2 are respectively compression rectification tower and DMC treating tower, and H1, H2 are respectively the tower still reboilers of compression rectification tower and treating tower, and C1, C2 are respectively the overhead condensers of compression rectification tower and treating tower, V1 is the tundish of DMC and methanol azeotrope, and P1 is a force (forcing) pump.
Distillation process carries out in the compression rectification tower, and whole rectifying column is divided into two sections, and epimere is rectifying section, and hypomere is stripping section, the midsection charging. For guaranteeing the separating effect of methyl alcohol and DMC, the theoretical cam curve of compression rectification tower should be greater than 15, preferably should be between 25～30. Continuous feed in the tower, the tower reactor continuous discharge, the overhead reflux ratio is 1～6, is preferably 3～5, and the pressure that produces because of material reaction self in the tower can reach 1.0～1.8MPa, and feeding temperature is about 150 ℃. Dimethyl carbonate for ester-interchange method production, add rectifying column T1 from transesterification reactor or reaction fractionating tower azeotropic mixture out through force (forcing) pump P1 curve 1, after the rectifying of T1 tower separates, a large amount of methyl alcohol and a small amount of DMC after the C1 condensation by line 3 Returning reacting systems, the DMC warp 2 of the content 97%～98% that the bottom tower reactor obtains enters DMC treating column T2, behind the highly purified DMC that purification obtains, leaving system's can by line 5 dispatches from the factory, a small amount of methyl alcohol of T2 cat head and the azeotropic mixture of DMC enter pans V1 by line 4 after the C2 condensation, in order to continue circulation, the rate of recovery of DMC can reach more than 90%. Treating column T2 is atmospheric tower.
In industrial application, because each of tower section liquid load differs greatly, compression rectification tower and DMC treating tower adopt the stainless steel metal screen waviness packings.
Embodiment situation equipment structure:
Operational stage: two tower operate continuouslys, azeotrope inlet amount 800L/h
Operating result:
| The T1 tower | The T2 tower | |
| Internal diameter (mm) | ????800 | ????600 |
| Rectifying section height (m) | ????6 | ????4 |
| Stripping section height (m) | ????4 | ????4 |
| Rectifying section stage number (piece) | ????60 | ????40 |
| Stripping section stage number (piece) | ????40 | ????40 |
| Feeding temperature (℃) | Working pressure (MPa) | Reflux ratio | Reflux temperature (℃) | |
| Implement side 1 | ????145 | ????1.0 | ????3 | ????75 |
| Embodiment 2 | ????150 | ????1.5 | ????3 | ????76 |
| Embodiment 3 | ????155 | ????1.8 | ????4 | ????78 |
| The T1 top | The T1 still | T2 still DMC | |||
| Methyl alcohol | ??DMC | Methyl alcohol | DMC | ||
| Embodiment 1 | ?94％ | ??6％ | ??3％ | 97％ | ????99.5％ |
| Embodiment 2 | ?95％ | ??5％ | ??2％ | 98％ | ????99.8％ |
| Embodiment 3 | ?96％ | ??4％ | ?1.5％ | 98.5％ | ????99.9％ |
The present invention directly relies on the pressure of material id reaction generation and realizes separating of methyl alcohol and DMC, its advantage is: does not pressurize by inert gas (1), produce pressure but directly rely on material self, a cover inert gas generation, compression, voltage stabilizing interlock have been saved, save equipment investment, reduced power consumption. (2) drop temperature is easy to control at bubble point backflow, and energy consumption is low. (3) the tower internal pressure is easy to control, and allowable fluctuation range is wider, and is easy to operate. (4) control module is few, has stopped because of the quality problem of inert gas total system to be consisted of negative effect fully.
Claims (3)
1, a kind of method of pressurize separation of methanol and dimethyl carbonate azeotrope is characterized in that utilizing the pressure separation of methanol of material self generation and the azeotrope of methylcarbonate.
2, by the method for described a kind of pressurize separation of methanol and dimethyl carbonate azeotrope of claim 1, it is characterized in that the pressure that material self produces in the compression rectification tower reaches 1.0～1.8MPa, feeding temperature is about 150 ℃.
3,, it is characterized in that the content that obtains is that 97～98% methylcarbonate enters the normal pressure treating tower and purifies and obtain highly purified methylcarbonate from compression rectification tower bottom tower still by the method for claim 1 or 2 described a kind of pressurize separation of methanol and dimethyl carbonate azeotropes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00107115 CN1271721A (en) | 2000-04-17 | 2000-04-17 | Process for pressure separation of mathanol and dimethyl carbonate azeotrope |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00107115 CN1271721A (en) | 2000-04-17 | 2000-04-17 | Process for pressure separation of mathanol and dimethyl carbonate azeotrope |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1271721A true CN1271721A (en) | 2000-11-01 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 00107115 Pending CN1271721A (en) | 2000-04-17 | 2000-04-17 | Process for pressure separation of mathanol and dimethyl carbonate azeotrope |
Country Status (1)
| Country | Link |
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| CN (1) | CN1271721A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7799940B2 (en) | 2007-02-16 | 2010-09-21 | Sabic Innovative Plastics Ip B.V. | Process for manufacturing dimethyl carbonate |
| US7803961B2 (en) | 2007-02-16 | 2010-09-28 | Sabic Innovative Plastics Ip B.V. | Process for manufacturing dimethyl carbonate |
| CN104418751A (en) * | 2013-08-29 | 2015-03-18 | 张家港市国泰华荣化工新材料有限公司 | Single-tower atmospheric continuous dimethyl carbonate purification process and device |
| CN106699565A (en) * | 2017-03-23 | 2017-05-24 | 山东石大胜华化工集团股份有限公司 | Device and method for energy saving and consumption reduction of dimethyl carbonate device |
-
2000
- 2000-04-17 CN CN 00107115 patent/CN1271721A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7799940B2 (en) | 2007-02-16 | 2010-09-21 | Sabic Innovative Plastics Ip B.V. | Process for manufacturing dimethyl carbonate |
| US7803961B2 (en) | 2007-02-16 | 2010-09-28 | Sabic Innovative Plastics Ip B.V. | Process for manufacturing dimethyl carbonate |
| CN104418751A (en) * | 2013-08-29 | 2015-03-18 | 张家港市国泰华荣化工新材料有限公司 | Single-tower atmospheric continuous dimethyl carbonate purification process and device |
| CN104418751B (en) * | 2013-08-29 | 2016-05-11 | 张家港市国泰华荣化工新材料有限公司 | The continuous purifying technique of dimethyl carbonate list tower normal pressure and device |
| CN106699565A (en) * | 2017-03-23 | 2017-05-24 | 山东石大胜华化工集团股份有限公司 | Device and method for energy saving and consumption reduction of dimethyl carbonate device |
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| C10 | Entry into substantive examination | ||
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| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |