CN203247212U - Recovering device of by-product raffinate generated in production process of coal-based ethylene glycol - Google Patents

Recovering device of by-product raffinate generated in production process of coal-based ethylene glycol Download PDF

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Publication number
CN203247212U
CN203247212U CN 201320274546 CN201320274546U CN203247212U CN 203247212 U CN203247212 U CN 203247212U CN 201320274546 CN201320274546 CN 201320274546 CN 201320274546 U CN201320274546 U CN 201320274546U CN 203247212 U CN203247212 U CN 203247212U
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tower
recovery tower
condenser
evaporator
water treatment
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陆丁丁
隋然
何晓萍
迪建东
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Tianjin Zhongfu Taike Chemical Technology Co ltd
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Tianjin Tzfd Science & Technology Co Ltd
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Abstract

The utility model relates to a recovering device of by-product raffinate generated in production process of coal-based ethylene glycol. The recovering device comprises an evaporator, a recovery tower, a waste water treatment tower, a wiped film evaporator and the like, wherein the discharging port of the evaporator is connected with the charging port of a light component condenser; the discharging port of the light component condenser is connected with the charging port of a methanol recovery tower; the discharging port of the methanol recovery tower kettle is connected with the charging port of the methanol recovery tower; the discharging port of the methanol recovery tower kettle is connected with the charging port of a waste water treatment tower; the discharging port of the waste water treatment tower kettle and the discharging port of the bottom liquid phase of the evaporator are connected to the charging port of the wiped film evaporator; the discharging port of the bottom of the wiped film evaporator is connected to a heavy boiling object storage tank; the discharging port of the upper gas phase of the wiped evaporator is connected with the charging port of a heavy component condenser; the discharging port of a condenser is connected with the charging port of a 1,2-propanediol recovery tower; the discharging port of the 1,2-propanediol recovery tower kettle is connected with the charging port of a ethylene glycol recovery tower. The recovering device is a high-efficiency and environmental-friendly recovering and separating device and makes economic and social benefits.

Description

The retrieving arrangement of by-product raffinate in the coal-ethylene glycol production process
Technical field
The utility model belongs to the processing method of chemical separation process, says further the retrieving arrangement that relates to by-product raffinate in the coal-ethylene glycol production process.
Background technology
Ethylene glycol is the simplest and most important aliphatic dihydroxy alcohol, it also is a kind of important petrochemical complex basic organic material, be widely used in producing trevira, frostproofer, lubricant, softening agent, nonionogenic tenside and explosive etc., high-purity ethylene glycol can be used as solvent and the medium of ammonium pertorate, also can be used for producing the special solvent glycol ether.Chemical enterprise all adopts producing glycol by virtue of hydration of ethylene oxide both at home and abroad at present; but in recent years be subject to the impact of oil crisis; the researcher all puts into take coal in the research of raw material production ethylene glycol both at home and abroad; for the present situation of nearly 40% import of the present ethylene glycol demand of China, domestic research unit and enterprise all drop into a large amount of energy and are devoted in the research and development of coal-ethylene glycol technique.
At present domesticly prepare ethylene glycol take coal as raw material, mainly contain three operational paths:
1, direct method: with gasification producing synthesis gas (CO+H2), again by direct synthesizing glycol of one step of synthetic gas.The key of this technology is the selection of catalyzer, is difficult to realize industrialization within quite long period.
2, olefin processes: take coal as raw material, by obtaining synthetic gas after gasification, conversion, the purification, synthetic through methyl alcohol, methanol-to-olefins (MTO) obtains ethene, finally obtains ethylene glycol through ethylene epoxidizing, ethylene oxide hydration and product exquisiteness again.This process combines olefin hydrocarbon making by coal with traditional petroleum path ethylene glycol, technology is comparatively ripe, but cost is relatively high.
3, barkite method: take coal as raw material, by obtaining respectively CO and H2 behind gasification, conversion, purification and the separating-purifying, wherein CO by catalytic coupling the synthetic and refining barkite of producing, again through carrying out hydrogenation reaction and the process by acquisition polyester grade ethylene glycol after refining with H2.This technical process is short, and cost is low, is the present domestic coal-ethylene glycol technology that receives publicity the highest, and usually said " coal-ethylene glycol " is exactly to refer in particular to this technique.
The a large amount of ethylene glycol raffinates of meeting by-product in the ethylene glycol production process, industrial scale according to 50,000 ton/years, the annual raffinate that approximately produces 3%-5%, it is rich in methyl alcohol, ethanol, 1, the components such as 2-propylene glycol, ethylene glycol and Diethylene Glycol, enterprise all sells it as cheap solvent at present, has caused the waste of resource.If can adopt rational separating technology that it is recycled, must greatly strengthen the recycling of this by-product waste liquid, therefore the utility model proposes and a kind ofly process this Chemical Manufacture waste liquid by luwa evaporator and high-efficiency and precision rectifying integrated separation technique.
Summary of the invention
The purpose of this utility model provides the retrieving arrangement of by-product raffinate in a kind of coal-ethylene glycol production process, adopts this device can effectively reclaim ethylene glycol and produces methyl alcohol in the raffinate, ethanol, 1,2-PD, ethylene glycol, the products such as Diethylene Glycol, thereby the comprehensive utilization of resources that improves raffinate.
The technical solution of the utility model is as follows:
The retrieving arrangement of the raffinate of coal-ethylene glycol of the present utility model, by vaporizer, light constituent condenser, methanol distillation column, the ethanol recovery tower, waste-water treatment tower, luwa evaporator, the thing storage tank heavily boils, restructuring minute condenser, 1,2-PD recovery tower and glycol recovery tower form; The outlet of vaporizer gaseous phase materials connects light constituent condenser material inlet, light constituent condenser material outlet connects the methanol distillation column material inlet, the Methanol Recovery column overhead obtains methanol product, methanol distillation column tower reactor material outlet connects ethanol recovery tower material inlet, ethanol recovery tower cat head obtains alcohol product, ethanol recovery tower tower reactor material outlet connects the waste-water treatment tower material inlet, the wastewater treatment column overhead obtains reaching the waste water of emission standard, waste-water treatment tower tower reactor material outlet connects base of evaporator liquid phase material outlet conduit, base of evaporator liquid phase material outlet conduit connects the luwa evaporator material inlet, luwa evaporator bottom liquid phases material outlet connects the thing storage tank that heavily boils, luwa evaporator upper gaseous phase material outlet connects restructuring minute condenser material inlet, restructuring minute condenser material outlet connects 1,2-propylene glycol recovery tower material inlet, 1,2-propylene glycol recovery tower cat head obtains 1,2-propylene glycol product, 1,2-propylene glycol recovery tower tower reactor material outlet connects glycol recovery tower material inlet, the glycol recovery column overhead obtains the ethylene glycol product, and tower reactor obtains the Diethylene Glycol product.
Each above-mentioned column overhead is provided with condenser, and tower reactor is provided with reboiler.
According to said apparatus, can proceed as follows:
The ethylene glycol raffinate at first enters vaporizer, under condition of normal pressure, operate, the vaporizer top is discharged gaseous phase materials and is entered the light constituent condenser, after the light constituent condenser condenses, enter methanol distillation column, the Methanol Recovery column overhead obtains methanol product after rectification process, methanol distillation column tower reactor material enters the ethanol recovery tower, ethanol recovery tower cat head obtains alcohol product, ethanol recovery tower tower reactor material enters waste-water treatment tower, the wastewater treatment column overhead obtains reaching the waste water of emission standard, waste-water treatment tower tower reactor material enters luwa evaporator, base of evaporator liquid effluent phase materials also enters luwa evaporator, luwa evaporator bottom liquid phases material enters the thing storage tank that heavily boils, luwa evaporator top gaseous phase materials enters restructuring minute condenser, after restructuring minute condenser condenses, enter 1,2-propylene glycol recovery tower, 1,2-propylene glycol recovery tower cat head obtains 1,2-propylene glycol product, 1,2-propylene glycol recovery tower tower reactor material enters the glycol recovery tower, and the glycol recovery column overhead obtains the ethylene glycol product, and tower reactor obtains the Diethylene Glycol product.
Luwa evaporator 22 bottom liquid phases material outlets connect the thing storage tank 24 that heavily boils.
Described high boiler material is high boiling polyol compound in the luwa evaporator, is roughly the contour solidifying high boiling material material of the oligopolymer that produces in the ethylene glycol production process, and it can be used as fuel and sells outward.
According to 50,000 ton/years industrial scale, the annual raffinate that approximately produces 3%-5%, approximately obtain 285 tons of methanol product, 266 tons of alcohol products, 209 tons of 1,2-PD products, 741 tons of ethylene glycol products, 190 tons of Diethylene Glycol products every year after this device is processed.
The utility model has the advantage of that described ethylene glycol raffinate reclaims technique and can effectively reclaim methyl alcohol in the ethylene glycol raffinate, ethanol, 1,2-PD, ethylene glycol, the products such as Diethylene Glycol are a kind of recovery separating technologies of efficient and environmental protection.Not only create good economic benefit, also created good social benefit.
Description of drawings
Fig. 1: the device for continuously recycling schematic diagram of ethylene glycol by-product raffinate.
Wherein: 1-ethylene glycol raffinate, 2-vaporizer, gaseous phase materials is discharged at 3-vaporizer top, 4-light constituent condenser, 5-light constituent phlegma, 6-methanol distillation column, 7-methanol distillation column condenser, 8-methanol product, 9-methanol distillation column reboiler, 10-methanol distillation column tower reactor material, 11-ethanol recovery tower, 12-ethanol recovery tower condenser, 13-alcohol product, 14-ethanol recovery tower reboiler, 15-ethanol recovery tower tower reactor material, 16-waste-water treatment tower, 17-waste-water treatment tower condenser, 18-reach the waste water of emission standard, 19-waste-water treatment tower reboiler, 20-waste-water treatment tower tower reactor material, 21-base of evaporator liquid effluent phase materials, 22-luwa evaporator, 23-heavily things that boil, 24-heavily thing storage tanks that boil, 25-luwa evaporator top gaseous phase materials, 26-restructuring minute condenser, 27-restructuring minute phlegma, 28-1,2-PD recovery tower, 29-1,2-propylene glycol recovery tower condenser, 30-1,2-PD product, 31-1,2-propylene glycol recovery tower reboiler, 32-1,2-PD recovery tower tower reactor material, 33-glycol recovery tower, 34-glycol recovery tower condenser, 35-ethylene glycol product, 36-glycol recovery tower reboiler, 37-Diethylene Glycol
Embodiment
Below in conjunction with embodiment, further specify the utility model, but the utility model is not limited to embodiment.
Equipment of the present utility model as shown in the figure, the outlet of vaporizer 2 gaseous phase materials connects light constituent condenser 4 material inlets, light constituent condenser 4 material outlets connect methanol distillation column 6 material inlets, methanol distillation column 6 cats head arrange methanol distillation column condenser 7, tower reactor arranges methanol distillation column reboiler 9, methanol distillation column 6 tower reactor material outlets connect ethanol recovery tower 11 material inlets, ethanol recovery tower 11 cats head arrange ethanol recovery tower condenser 12, tower reactor arranges ethanol recovery tower reboiler 14, ethanol recovery tower 11 tower reactor material outlets connect waste-water treatment tower 16 material inlets, waste-water treatment tower 16 cats head arrange waste-water treatment tower condenser 17, tower reactor arranges waste-water treatment tower reboiler 19, waste-water treatment tower 16 tower reactor material outlets connect vaporizer 2 bottom liquid phases material outlet pipelines, vaporizer 2 bottom liquid phases material outlet pipelines connect luwa evaporator 22 material inlets, luwa evaporator 22 bottom liquid phases material outlets connect the thing storage tank 24 that heavily boils, luwa evaporator 22 upper gaseous phase material outlets connect restructuring minute condenser 26 material inlets, restructuring minute condenser 26 material outlets connect 1,2-propylene glycol recovery tower 28 material inlets, 1,2-propylene glycol recovery tower 28 cats head arrange 1,2-propylene glycol recovery tower condenser 29, tower reactor arranges 1,2-propylene glycol recovery tower reboiler 31,1,2-propylene glycol recovery tower 28 tower reactor material outlets connect glycol recovery tower 33 material inlets, glycol recovery tower 33 cats head arrange glycol recovery tower condenser 34, and tower reactor arranges glycol recovery tower reboiler 36.
Ethylene glycol raffinate 1 at first enters vaporizer 2, under condition of normal pressure, operate, vaporizer 2 tops are discharged gaseous phase materials 3 and are entered light constituent condenser 4, after 4 condensations of light constituent condenser, enter methanol distillation column 6, methanol distillation column 6 cats head obtain methanol product 8 after rectification process, methanol distillation column 6 tower reactor materials 10 enter ethanol recovery tower 11, ethanol recovery tower 11 cats head obtain alcohol product 13, ethanol recovery tower 11 tower reactor materials 15 enter waste-water treatment tower 16, waste-water treatment tower 16 cats head must reach the waste water 18 of emission standard, waste-water treatment tower 16 tower reactor materials 20 enter luwa evaporator 22, vaporizer 2 bottom liquid effluent phase materials 21 also enter luwa evaporator 22, luwa evaporator 22 bottom liquid phases materials 23 enter the thing storage tank 24 that heavily boils, luwa evaporator 22 top gaseous phase materials 25 enter restructuring minute condenser 26, after restructuring minute condenser condenses, enter 1,2-propylene glycol recovery tower 28,1,2-propylene glycol recovery tower 28 cats head obtain 1,2-propylene glycol product 30,1,2-propylene glycol recovery tower 28 tower reactor materials 32 enter glycol recovery tower 33, and glycol recovery tower 33 cats head obtain ethylene glycol product 35, and tower reactor obtains Diethylene Glycol product 37.
Embodiment 1
Ethylene glycol raffinate 1 enters vaporizer 2 with the flow velocity of 1700kg/h, the working pressure of vaporizer 2 is normal pressure, service temperature is 110 ℃, vaporizer 2 tops are discharged gaseous phase materials 3 and are entered light constituent condenser 4, enter methanol distillation column 6 through 4 condensations of light constituent condenser and after being cooled to 40 ℃, the theoretical plate number of methanol distillation column 6 is 35, working pressure is normal pressure, tower top temperature is 65 ℃, the tower reactor temperature is 100 ℃, methanol distillation column 6 cats head obtain 95% methanol product 8 after rectification process, methanol distillation column 6 tower reactor materials 10 enter ethanol recovery tower 11, the theoretical plate number of ethanol recovery tower 11 is 30, working pressure is normal pressure, tower top temperature is 80 ℃, the tower reactor temperature is 100 ℃, ethanol recovery tower 11 cats head obtain 95% alcohol product 13 after rectification process, ethanol recovery tower 11 tower reactor materials 15 enter waste-water treatment tower 16, the theoretical plate number of waste-water treatment tower 16 is 20, working pressure is normal pressure, tower top temperature is 100 ℃, the tower reactor temperature is 130 ℃, waste-water treatment tower 16 cats head must reach the waste water 18 of emission standard after rectification process, waste-water treatment tower 16 tower reactor materials 20 enter luwa evaporator 22, vaporizer 2 bottom liquid effluent phase materials 21 also enter luwa evaporator 22, the working pressure of luwa evaporator 22 is 20kPa, service temperature is 200 ℃, rotating speed is 200 rev/mins, luwa evaporator 22 bottom liquid phases materials 23 enter the thing storage tank 24 that heavily boils, luwa evaporator 22 top gaseous phase materials 25 enter restructuring minute condenser 26, enter 1 through restructuring minute condenser 26 condensations and after being cooled to 80 ℃, 2-propylene glycol recovery tower 28,1, the theoretical plate number of 2-propylene glycol recovery tower 28 is 30, working pressure is 20kPa, tower top temperature is 140 ℃, the tower reactor temperature is 170 ℃, after rectification process 1,2-propylene glycol recovery tower 28 cats head obtain 96%1,2-propylene glycol product 30,1,2-propylene glycol recovery tower 28 tower reactor materials 32 enter glycol recovery tower 33, the theoretical plate number of glycol recovery tower 33 is 35, working pressure is 20kPa, tower top temperature is 160 ℃, the tower reactor temperature is 190 ℃, and glycol recovery tower 33 cats head obtain 99% ethylene glycol product 35 after rectification process, and glycol recovery tower 33 tower reactors obtain 96% Diethylene Glycol product 37.
Embodiment 2
Ethylene glycol raffinate 1 enters vaporizer 2 with the flow velocity of 1700kg/h, the working pressure of vaporizer 2 is normal pressure, service temperature is 110 ℃, vaporizer 2 tops are discharged gaseous phase materials 3 and are entered light constituent condenser 4, enter methanol distillation column 6 through 4 condensations of light constituent condenser and after being cooled to 40 ℃, the theoretical plate number of methanol distillation column 6 is 40, working pressure is normal pressure, tower top temperature is 68 ℃, the tower reactor temperature is 105 ℃, methanol distillation column 6 cats head obtain 94% methanol product 8 after rectification process, methanol distillation column 6 tower reactor materials 10 enter ethanol recovery tower 11, the theoretical plate number of ethanol recovery tower 11 is 35, working pressure is normal pressure, tower top temperature is 85 ℃, the tower reactor temperature is 105 ℃, ethanol recovery tower 11 cats head obtain 96% alcohol product 13 after rectification process, ethanol recovery tower 11 tower reactor materials 15 enter waste-water treatment tower 16, the theoretical plate number of waste-water treatment tower 16 is 25, working pressure is normal pressure, tower top temperature is 103 ℃, the tower reactor temperature is 135 ℃, waste-water treatment tower 16 cats head must reach the waste water 18 of emission standard after rectification process, waste-water treatment tower 16 tower reactor materials 20 enter luwa evaporator 22, vaporizer 2 bottom liquid effluent phase materials 21 also enter luwa evaporator 22, the working pressure of luwa evaporator 22 is 25kPa, service temperature is 200 ℃, rotating speed is 250 rev/mins, luwa evaporator 22 bottom liquid phases materials 23 enter the thing storage tank 24 that heavily boils, luwa evaporator 22 top gaseous phase materials 25 enter restructuring minute condenser 26, enter 1 through restructuring minute condenser 26 condensations and after being cooled to 80 ℃, 2-propylene glycol recovery tower 28,1, the theoretical plate number of 2-propylene glycol recovery tower 28 is 35, working pressure is 25kPa, tower top temperature is 145 ℃, the tower reactor temperature is 175 ℃, after rectification process 1,2-propylene glycol recovery tower 28 cats head obtain 97%1,2-propylene glycol product 30,1,2-propylene glycol recovery tower 28 tower reactor materials 32 enter glycol recovery tower 33, the theoretical plate number of glycol recovery tower 33 is 40, working pressure is 25kPa, tower top temperature is 165 ℃, the tower reactor temperature is 195 ℃, and glycol recovery tower 33 cats head obtain 99% ethylene glycol product 35 after rectification process, and glycol recovery tower 33 tower reactors obtain 96% Diethylene Glycol product 37.
Embodiment 3
Ethylene glycol raffinate 1 enters vaporizer 2 with the flow velocity of 1700kg/h, the working pressure of vaporizer 2 is normal pressure, service temperature is 110 ℃, vaporizer 2 tops are discharged gaseous phase materials 3 and are entered light constituent condenser 4, enter methanol distillation column 6 through 4 condensations of light constituent condenser and after being cooled to 40 ℃, the theoretical plate number of methanol distillation column 6 is 45, working pressure is normal pressure, tower top temperature is 70 ℃, the tower reactor temperature is 110 ℃, methanol distillation column 6 cats head obtain 95% methanol product 8 after rectification process, methanol distillation column 6 tower reactor materials 10 enter ethanol recovery tower 11, the theoretical plate number of ethanol recovery tower 11 is 40, working pressure is normal pressure, tower top temperature is 90 ℃, the tower reactor temperature is 110 ℃, ethanol recovery tower 11 cats head obtain 95% alcohol product 13 after rectification process, ethanol recovery tower 11 tower reactor materials 15 enter waste-water treatment tower 16, the theoretical plate number of waste-water treatment tower 16 is 30, working pressure is normal pressure, tower top temperature is 105 ℃, the tower reactor temperature is 140 ℃, waste-water treatment tower 16 cats head must reach the waste water 18 of emission standard after rectification process, waste-water treatment tower 16 tower reactor materials 20 enter luwa evaporator 22, vaporizer 2 bottom liquid effluent phase materials 21 also enter luwa evaporator 22, the working pressure of luwa evaporator 22 is 30kPa, service temperature is 200 ℃, rotating speed is 300 rev/mins, luwa evaporator 22 bottom liquid phases materials 23 enter the thing storage tank 24 that heavily boils, luwa evaporator 22 top gaseous phase materials 25 enter restructuring minute condenser 26, enter 1 through restructuring minute condenser 26 condensations and after being cooled to 80 ℃, 2-propylene glycol recovery tower 28,1, the theoretical plate number of 2-propylene glycol recovery tower 28 is 40, working pressure is 30kPa, tower top temperature is 150 ℃, the tower reactor temperature is 180 ℃, after rectification process 1,2-propylene glycol recovery tower 28 cats head obtain 96%1,2-propylene glycol product 30,1,2-propylene glycol recovery tower 28 tower reactor materials 32 enter glycol recovery tower 33, the theoretical plate number of glycol recovery tower 33 is 45, working pressure is 30kPa, tower top temperature is 170 ℃, the tower reactor temperature is 200 ℃, and glycol recovery tower 33 cats head obtain 99% ethylene glycol product 35 after rectification process, and glycol recovery tower 33 tower reactors obtain 96% Diethylene Glycol product 37.
The retrieving arrangement of by-product raffinate in the coal-ethylene glycol production process that the utility model proposes, be described by preferred embodiment, person skilled obviously can not break away from the utility model content, to equipment as herein described with the preparation method changes or suitably change and combination, realize the utility model technology in the spirit and scope.Special needs to be pointed out is, the replacement that all are similar and change are apparent to those skilled in the art, and they are deemed to be included in spirit of the present utility model, in scope and the content.

Claims (2)

1. the retrieving arrangement of by-product raffinate in the coal-ethylene glycol production process is characterized in that by vaporizer light constituent condenser, methanol distillation column, the ethanol recovery tower, waste-water treatment tower, luwa evaporator, the thing storage tank heavily boils, restructuring minute condenser, 1,2-PD recovery tower and glycol recovery tower form; The outlet of vaporizer gaseous phase materials connects light constituent condenser material inlet, light constituent condenser material outlet connects the methanol distillation column material inlet, methanol distillation column tower reactor material outlet connects ethanol recovery tower material inlet, ethanol recovery tower cat head obtains alcohol product, ethanol recovery tower tower reactor material outlet connects the waste-water treatment tower material inlet, waste-water treatment tower tower reactor material outlet connects base of evaporator liquid phase material outlet conduit, base of evaporator liquid phase material outlet conduit connects the luwa evaporator material inlet, luwa evaporator bottom liquid phases material outlet connects the thing storage tank that heavily boils, luwa evaporator upper gaseous phase material outlet connects restructuring minute condenser material inlet, restructuring minute condenser material outlet connects 1,2-propylene glycol recovery tower material inlet, 1,2-PD recovery tower tower reactor material outlet connects glycol recovery tower material inlet.
2. device as claimed in claim 1 is characterized in that described each column overhead is provided with condenser, and tower reactor is provided with reboiler.
CN 201320274546 2013-05-17 2013-05-17 Recovering device of by-product raffinate generated in production process of coal-based ethylene glycol Expired - Lifetime CN203247212U (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103254030A (en) * 2013-05-17 2013-08-21 天津天中福大科技发展有限公司 Device and method for recycling byproduct residual liquid in coal-to-ethylene-glycol production process
CN108434766A (en) * 2018-04-03 2018-08-24 烟台国邦化工机械科技有限公司 A kind of high-melting-point object system's recovery system and process
CN111825527A (en) * 2020-06-12 2020-10-27 神木市锦界安顺煤矿机电修造有限公司 Process for recovering residual ethylene glycol liquid by immersion, evaporation and adsorption

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103254030A (en) * 2013-05-17 2013-08-21 天津天中福大科技发展有限公司 Device and method for recycling byproduct residual liquid in coal-to-ethylene-glycol production process
CN108434766A (en) * 2018-04-03 2018-08-24 烟台国邦化工机械科技有限公司 A kind of high-melting-point object system's recovery system and process
CN111825527A (en) * 2020-06-12 2020-10-27 神木市锦界安顺煤矿机电修造有限公司 Process for recovering residual ethylene glycol liquid by immersion, evaporation and adsorption

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