CN202139179U - Device for producing ethylene glycol by dimethyloxalate with hydrogenation - Google Patents
Device for producing ethylene glycol by dimethyloxalate with hydrogenation Download PDFInfo
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- CN202139179U CN202139179U CN201120013217U CN201120013217U CN202139179U CN 202139179 U CN202139179 U CN 202139179U CN 201120013217 U CN201120013217 U CN 201120013217U CN 201120013217 U CN201120013217 U CN 201120013217U CN 202139179 U CN202139179 U CN 202139179U
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Abstract
The utility model discloses a device for producing ethylene glycol by dimethyloxalate with hydrogenation, which comprises a feed preheater, a feed heater, a primary purifier, a secondary purifier and a hydrogenation reactor, as well as a hydrogenation product cooler and a liquid-phase hydrogenation product tank; wherein the feed preheater, the feed heater, the primary purifier, the secondary purifier and the hydrogenation reactor are connected in sequence through pipelines; the hydrogenation reactor is connected with the feed preheater through the pipeline; the hydrogenation product cooler is connected with the feed preheater through the pipeline; and the liquid-phase hydrogenation product tank is connected with the hydrogenation product cooler through the pipeline. The device is energy-saving and environmental-protection and realizes the full utilization of heat energy of the system, the raw material hydrogen is circularly used under the premise of meeting technological conditions so as to realize maximized utilization of raw materials and effectively solve the problem of accumulation of inert gases (nitrogen, argon and the like) in a circulating gas phase, and simultaneously detrimental impurities in a liquid phase and the gas phase in the raw materials can be effectively removed, the trouble to the activity and the selectivity of a hydrogenation catalyst, caused by concentration accumulation of the detrimental impurities, and long-term stable running of hydrogenation working procedure, can be ensured.
Description
Technical field
The utility model relates to a kind of device of preparing ethylene glycol by using dimethyl oxalate plus hydrogen.
Background technology
Terepthaloyl moietie is a kind of important Organic Chemicals; Be mainly used in and produce trevira, frostproofer, unsaturated polyester resin, lubricant, softening agent, nonionogenic tenside and explosive etc.; Can be used for industries such as coating, soup, brake fluid and printing ink in addition; Solvent and medium as ammonium pertorate are used to produce special solvent glycol ether etc., and purposes very extensively.
Current, the suitability for industrialized production of domestic and international large-scale terepthaloyl moietie all adopts the oxyethane direct hydration, i.e. the legal operational path of pressurized water, and production technology is basically by English lotus Shell, U.S. Halcon-SD and the monopolization of U.S. UCC three companies.In addition, the research-and-development activity of the new synthetic technology of terepthaloyl moietie is also making progress always.The companies such as catalyzing epoxyethane hydration legal system terepthaloyl moietie production technology: Halcon-SD, UCC, Dow chemistry, Japanese catalyst chemistry and Mitsubishi Chemical that developed in succession like Shell company, UCC company, Moscow Mendelyeev chemical engineering institute, Oil of Shanghai Petrochemical Company institute etc. have developed NSC 11801 legal system terepthaloyl moietie production technology in succession: companies such as Dow chemistry have developed terepthaloyl moietie (EG) and methylcarbonate (DMC) coproduction preparing ethylene glycol production technology etc.
But the drawback of aforesaid method is to need the consumption of ethylene resource; And mainly lean on traditional petroleum resources refining for present ethene; And under the situation of following one section global oil price in period high-order operation for a long time; Replace oil production terepthaloyl moietie (non-petroleum path is the CO route again) with aboundresources, low-cost Sweet natural gas or coal, can possess the advantage of competing mutually with traditional ethene route.Wherein, synthetic gas synthesizes the EG new technology, may produce great influence to the innovation of EG production technique.With the carbon monoxide is the feedstock production dimethyl oxalate, and then the dimethyl oxalate hydrogenation reaction being prepared terepthaloyl moietie is a very attractive Coal Chemical Industry route.Now both at home and abroad to being that the research of feedstock production dimethyl oxalate has obtained good effect with the carbon monoxide, industrial production is ripe.And with preparation of ethanediol by dimethyl oxalate hydrogenation; Still have more need of work further investigation; Especially how effectively improve the permanent stability of dimethyl oxalate hydrogenation procedure technology device; Life of catalyst is the deciding factor that influences the production equipment cycle of operation, and the purity that facts have proved hydrogenation operation raw material is to influence activity of hydrocatalyst and important factor optionally, and the existence of detrimental impurity has directly influenced the work-ing life of hydrogenation catalyst in the raw material; Remove the impurity in the virgin gas, the purity that improves raw material is the important topic of hydrogenation operation scientific research.
The utility model content
In order to solve the problems of the technologies described above, the utility model provides a kind of device of preparing ethylene glycol by using dimethyl oxalate plus hydrogen efficiently, in order to preparation terepthaloyl moietie; This installs energy-conserving and environment-protective, has realized making full use of of system's heat energy, is satisfying under the prerequisite of processing condition; Raw hydrogen has obtained recycling, and has realized the maximum using of raw material, efficiently solves the accumulation problem of rare gas element in the circulation gas phase (nitrogen, argon gas etc.); Guaranteed the effective concentration of reactant gases; Simultaneously, the impurity of liquid phase feeding obtains effective elimination, and the concentration of detrimental impurity gas has obtained effective control in the circulation gas; Solved because harmful gas concentration is accumulated the puzzlement that activity and selectivity to hydrogenation catalyst cause, guaranteed the operation of hydrogenation operation long-term stability.
The device of the preparing ethylene glycol by using dimethyl oxalate plus hydrogen that the utility model provides; Comprise: the feed preheater that connects in order through pipeline, feed heater, one section cleaner, two sections cleaners and hydrogenator; Wherein, said hydrogenator is connected with said feed preheater through pipeline; The hydrogenation products water cooler is connected with said feed preheater through pipeline; And hydrogenation liquid product jar is connected with said product water cooler through pipeline.
The device of above-mentioned preparing ethylene glycol by using dimethyl oxalate plus hydrogen also comprises: compressor is connected with said hydrogenation products water cooler with said feed preheater respectively through pipeline; Pressure-swing absorption apparatus is connected with said hydrogenation products water cooler with said feed preheater respectively through pipeline.
Above-mentioned pressure-swing absorption apparatus comprises PWR PLT compressor and adsorption unit.
Above-mentioned feed preheater, said feed heater and said hydrogenation products water cooler are partition shell and tube heat exchanger or shell-and-plate(heat)exchanger.
Above-mentioned one section cleaner, two sections cleaners, hydrogenators are tubular fixed-bed reactor.
The beneficial effect that the utility model can reach is:
1, the use of feed preheater.Make the hydrogenator exit gas give the charging preheating as thermal source, efficient recovery system's heat energy, reduced heat energy input in system, practiced thrift heat energy consumption.
2, the use of feed heater is fully heated the raw material charging, reaches the temperature requirement of one section cleaner, has ensured reaction effect.
3, the use of one section, two sections cleaner.The impurity in the liquid phase feeding that utilized the chemical process effective elimination; Obnoxious flavoures such as the carbon monoxide in the circulation gas have been realized the thorough purification of hydrogenation reaction raw material, have effectively controlled the purity that gets into the hydrogenator raw material; The activity and the selectivity of hydrogenation catalyst have been guaranteed; Improve the production capacity of device, and guaranteed the work-ing life of hydrogenation catalyst, effectively guaranteed the long-term stability operation of production equipment; Once more, after hydrogenating materials purified, the by product in the hydrogenation reaction product reduced, and greatly reduced the working load that hydrogenation products separates the post.
4, the use of compressor makes the unreacted virgin gas hydrogen of hydrogenator play circulation in system, and virgin gas hydrogen is fully used; Once more, for the full cycle operation pressure guarantee is provided.
5, the rare gas element in the circulation gas has been got rid of in the use of pressure-swing absorption apparatus, and the concentration of reactant gases is controlled within the technic index, has guaranteed hydrogenation reaction efficient.
Description of drawings
Fig. 1 is the device synoptic diagram of the utility model preparing ethylene glycol by using dimethyl oxalate plus hydrogen;
Fig. 2 is the utility model preparing ethylene glycol by using dimethyl oxalate plus hydrogen process flow diagram.
Reference numeral:
1, feed preheater; 2, feed heater; 3, hydrogenation products water cooler; 4, one section cleaner; 5, two sections cleaners; 6, hydrogenator; 7, compressor; 8, pressure-swing absorption apparatus; 9, hydrogenation liquid product jar.
Embodiment
Below in conjunction with accompanying drawing and specific embodiment the utility model is described further so that those skilled in the art can better understand the utility model and implementing, but the embodiment that lifts not conduct to the qualification of the utility model.
As illustrated in fig. 1 and 2; Fresh hydrogen, dimethyl oxalate get into feed preheater 1 heat exchange with circulating hydrogen through pipeline; Feed preheater 1 is shell and tube heat exchanger or shell-and-plate(heat)exchanger; Its shell side thermal source is hydrogenator 6 outlet products, and tube side (or plate journey) is circulating hydrogen, fresh hydrogen and dimethyl oxalate liquid phase feeding.After the heat exchange; Circulating hydrogen, fresh hydrogen and dimethyl oxalate get into feed heater 2 and further heat; To reach the requirement of one section cleaner 4 temperature; Feed heater 2 is shell and tube heat exchanger or shell-and-plate(heat)exchanger, and its shell side thermal source is a MP steam, and tube side (or plate journey) is circulating hydrogen, fresh hydrogen and dimethyl oxalate.Behind circulating hydrogen, fresh hydrogen and the dimethyl oxalate heating and gasifying; Get into one section cleaner 4; Remove dimethyl oxalate and bring next impurity into; One section cleaner 4 is a tubular fixed-bed reactor, loads the solid granular scavenging agent in the tubulation, and shell side is the cold carrier (as: de-salted water) that reaction heat shifts out.One section cleaner 4 exit gas gets into two sections cleaners 5, and gas is carried out secondary-cleaned, and two sections cleaners 5 are tubular fixed-bed reactor, loads the solid granular scavenging agent in the tubulation, and shell side is the cold carrier (as: de-salted water) that reaction heat shifts out.The gas of two sections cleaner 5 outlets gets into hydrogenator 6 and carries out hydrogenation reaction, and hydrogenator 6 is a tubular fixed-bed reactor, loads solid granular catalyst in the tubulation, and shell side is the cold carrier (as: de-salted water) that reaction heat shifts out.Hydrogenator 6 outlet products get into feed preheater 1 and charge raw material heat exchange, and above-mentioned outlet product is cooled, and in hydrogenation products water cooler 3, carries out gas-liquid separation then; Hydrogenation products water cooler 3 is shell and tube heat exchanger or casing-structure heat-exchanger; Its shell side is recirculated water or refrigerated water, and tube side (or plate journey) is above-mentioned outlet product, and above-mentioned outlet product is cooled and is separated into liquid and gas; Liquid phase is the terepthaloyl moietie that hydrogenation reaction generates; Get into hydrogenation liquid product jar 9, gas phase is the mixed gas of hydrogen and small amounts of inert gas etc., and the above-mentioned mixed gas of volume percent 90-100% gets into compressor 7; Compressor 7 is for providing PWR PLT; Realize recycling of raw hydrogen, the above-mentioned mixed gas of volume percent 1-10% gets into pressure-swing absorption apparatus 8 and removes cumulative rare gas element in the system, and pressure-swing absorption apparatus comprises PWR PLT compressor, an adsorption device (containing sorbent material) (not shown); Realize separating of rare gas element and circulating hydrogen, remove and recycle after gas and compressor 7 exit gass behind the rare gas element converge.
The above embodiment is the preferred embodiment that proves absolutely that the utility model is lifted, and the protection domain of the utility model is not limited thereto.Being equal to that the technician in present technique field is done on the utility model basis substitutes or conversion, all within the protection domain of the utility model.The protection domain of the utility model is as the criterion with claims.
Claims (7)
1. the device of a preparing ethylene glycol by using dimethyl oxalate plus hydrogen is characterized in that, comprising:
The feed preheater that connects in order through pipeline, feed heater, one section cleaner, two sections cleaners and hydrogenator, wherein, said hydrogenator is connected with said feed preheater through pipeline;
The hydrogenation products water cooler is connected with said feed preheater through pipeline;
And hydrogenation liquid product jar is connected with said hydrogenation products water cooler through pipeline.
2. the device of preparing ethylene glycol by using dimethyl oxalate plus hydrogen according to claim 1 is characterized in that, also comprises: compressor is connected with said hydrogenation products water cooler with said feed preheater respectively through pipeline; Pressure-swing absorption apparatus is connected with said hydrogenation products water cooler with said feed preheater respectively through pipeline.
3. the device of preparing ethylene glycol by using dimethyl oxalate plus hydrogen according to claim 2 is characterized in that, said pressure-swing absorption apparatus comprises PWR PLT compressor and adsorption unit.
4. the device of preparing ethylene glycol by using dimethyl oxalate plus hydrogen according to claim 1 is characterized in that, said feed preheater is shell and tube heat exchanger or shell-and-plate(heat)exchanger.
5. the device of preparing ethylene glycol by using dimethyl oxalate plus hydrogen according to claim 1 is characterized in that, said feed heater is shell and tube heat exchanger or shell-and-plate(heat)exchanger.
6. the device of preparing ethylene glycol by using dimethyl oxalate plus hydrogen according to claim 1 is characterized in that, said hydrogenation products water cooler is shell and tube heat exchanger or shell-and-plate(heat)exchanger.
7. the device of preparing ethylene glycol by using dimethyl oxalate plus hydrogen according to claim 1 is characterized in that, said one section cleaner, two sections cleaners, hydrogenators are tubular fixed-bed reactor.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201120013217U CN202139179U (en) | 2011-01-17 | 2011-01-17 | Device for producing ethylene glycol by dimethyloxalate with hydrogenation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201120013217U CN202139179U (en) | 2011-01-17 | 2011-01-17 | Device for producing ethylene glycol by dimethyloxalate with hydrogenation |
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| Publication Number | Publication Date |
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| CN202139179U true CN202139179U (en) | 2012-02-08 |
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| CN201120013217U Expired - Lifetime CN202139179U (en) | 2011-01-17 | 2011-01-17 | Device for producing ethylene glycol by dimethyloxalate with hydrogenation |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102942446A (en) * | 2012-12-03 | 2013-02-27 | 大唐国际化工技术研究院有限公司 | Method for preparing ethanol via hydrogenation of acetic ester based on recirculating of recovered hydrogen |
| CN103804142A (en) * | 2012-11-07 | 2014-05-21 | 中国石油化工集团公司 | System and method used for preparing glycol via hydrogenation of oxalic ester |
| WO2015027897A1 (en) * | 2013-09-02 | 2015-03-05 | 东华工程科技股份有限公司 | Energy-saving ester hydrogenation process |
| CN109482107A (en) * | 2018-11-30 | 2019-03-19 | 华东理工大学 | The gasification method and vapourizing unit of dimethyl oxalate |
| CN111732497A (en) * | 2020-07-21 | 2020-10-02 | 濮阳永金化工有限公司 | Device for improving hydrogen-ester ratio and application method |
-
2011
- 2011-01-17 CN CN201120013217U patent/CN202139179U/en not_active Expired - Lifetime
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103804142A (en) * | 2012-11-07 | 2014-05-21 | 中国石油化工集团公司 | System and method used for preparing glycol via hydrogenation of oxalic ester |
| CN103804142B (en) * | 2012-11-07 | 2016-05-11 | 中国石油化工集团公司 | A kind of system and method for hydrogenation of oxalate for preparing ethylene glycol |
| CN102942446A (en) * | 2012-12-03 | 2013-02-27 | 大唐国际化工技术研究院有限公司 | Method for preparing ethanol via hydrogenation of acetic ester based on recirculating of recovered hydrogen |
| CN102942446B (en) * | 2012-12-03 | 2015-09-23 | 大唐国际化工技术研究院有限公司 | A kind of method reclaiming the acetic ester preparation of ethanol by hydrogenating of hydrogen recirculation |
| WO2015027897A1 (en) * | 2013-09-02 | 2015-03-05 | 东华工程科技股份有限公司 | Energy-saving ester hydrogenation process |
| CN109482107A (en) * | 2018-11-30 | 2019-03-19 | 华东理工大学 | The gasification method and vapourizing unit of dimethyl oxalate |
| CN111732497A (en) * | 2020-07-21 | 2020-10-02 | 濮阳永金化工有限公司 | Device for improving hydrogen-ester ratio and application method |
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Legal Events
| Date | Code | Title | Description |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CX01 | Expiry of patent term | ||
| CX01 | Expiry of patent term |
Granted publication date: 20120208 |