CN115155091A - Polyethylene glycol separation system and separation method - Google Patents

Polyethylene glycol separation system and separation method Download PDF

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Publication number
CN115155091A
CN115155091A CN202210853427.0A CN202210853427A CN115155091A CN 115155091 A CN115155091 A CN 115155091A CN 202210853427 A CN202210853427 A CN 202210853427A CN 115155091 A CN115155091 A CN 115155091A
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Prior art keywords
teg
tower
peg
polyethylene glycol
materials
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CN202210853427.0A
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Inventor
张军
朱文杰
温学剑
张伟杰
张进
殷明亮
黄佳琴
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Sanjiang Letian Chemical Co ltd
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Sanjiang Letian Chemical Co ltd
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Priority to CN202210853427.0A priority Critical patent/CN115155091A/en
Publication of CN115155091A publication Critical patent/CN115155091A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/14Fractional distillation or use of a fractionation or rectification column
    • B01D3/141Fractional distillation or use of a fractionation or rectification column where at least one distillation column contains at least one dividing wall
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C41/00Preparation of ethers; Preparation of compounds having groups, groups or groups
    • C07C41/01Preparation of ethers
    • C07C41/34Separation; Purification; Stabilisation; Use of additives
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C41/00Preparation of ethers; Preparation of compounds having groups, groups or groups
    • C07C41/01Preparation of ethers
    • C07C41/34Separation; Purification; Stabilisation; Use of additives
    • C07C41/40Separation; Purification; Stabilisation; Use of additives by change of physical state, e.g. by crystallisation
    • C07C41/42Separation; Purification; Stabilisation; Use of additives by change of physical state, e.g. by crystallisation by distillation

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention discloses a polyethylene glycol separation system and a separation method, which comprises a TEG tower, a TEG storage tank, a cooler, a tower kettle pump, a reboiler, a separation unit, a PEG storage tank and a PEG delivery pump, wherein materials at the bottom of the TEG tower pass through the tower kettle pump, one part of materials are sent to the reboiler, the other part of materials are sent to the separation unit, the materials are separated into partial PEG materials and partial TEG materials through the separation unit, the separated partial PEG materials are sent to the PEG storage tank and are pumped out of the world for storage through the PEG delivery pump, and the separated partial TEG materials are sent to the cooler for cooling and then are sent to the TEG storage tank. According to the invention, impurities in the polyethylene glycol are removed by controlling the resin adsorption selectivity at a certain flow rate, temperature and pressure, and then the triethylene glycol product with higher purity can be separated by an evaporation system, and the yield of the triethylene glycol product can be increased.

Description

Polyethylene glycol separation system and separation method
Technical Field
The invention belongs to the field of ethylene glycol production, relates to separation of ethylene glycol byproduct polyethylene glycol, and particularly relates to a polyethylene glycol separation system and a separation method.
Background
In the traditional glycol separation technical route, a mixture of monoethylene glycol, diethylene glycol and polyethylene glycol is separated in an MEG tower, the product MEG is discharged from the side line of the tower, the tower top is dehydrated, and the tower bottom discharge mainly comprises MEG, DEG and TEG. And (3) feeding the tower bottom discharge of the MEG tower into an MEG recovery tower for next-step separation, wherein the tower top of the MEG recovery tower mainly produces MEG and a small amount of DEG, and the tower bottom discharge mainly comprises DEG and TEG. And discharging the material from the tower kettle of the MEG recovery tower into a DEG tower for next-step separation, ejecting DEG products out of the DEG tower, and discharging TEG from the tower kettle.
The dividing wall rectifying tower is one kind of completely heat integrated tower with new structure and with one vertical wall in the middle part to divide the tower into four parts, including upper section, lower section, rectifying feeding section and rectifying extracting section separated with partition board. The three-component mixture is separated into pure products by the dividing wall rectifying tower, only one tower, one reboiler, one condenser and one reflux distributor are needed, and energy consumption and equipment investment can be reduced.
Therefore, applications of the divided wall rectification column have been increasing in recent years. UOP company has applied several new processes using dividing wall distillation columns, such as the dividing wall distillation column technology for alkylbenzene production (US 6417420) and the dividing wall distillation technology for whole fraction gasoline desulfurization (US 6540907 and US 20030116474).
In addition, US20050211541 and US20050245037 disclose a dividing wall rectification technique for separating a solvent used in the production of propylene oxide; US7132038B2 discloses a method for purifying 1,3 butadiene from a crude 1,3 butadiene mixed liquor using a divided wall rectification column separation; the Jiangsu institute of labor saving applies for a device and a method (CN 101723793A) for separating crude glycol from pyrolysis gasoline; at present, more than about 70 dividing wall rectifying towers are operated commercially all over the world.
The existing glycol device adopts a traditional separation technical route, and has the problems of complex separation process of a mixture system of mono-glycol, di-glycol and polyethylene glycol, low separation purity, large investment and high energy consumption.
Disclosure of Invention
In order to solve the problems, the invention provides a polyethylene glycol separation system and a separation method, which aim to improve the separation rate of polyethylene glycol (a mixture of ethylene glycol, diethylene glycol, triethylene glycol and polyethylene glycol) which is a byproduct of an ethylene oxide/ethylene glycol device, separate the triethylene glycol in the polyethylene glycol more efficiently, reduce energy consumption, improve the yield and quality of high-purity triethylene glycol products, increase the additional value of the products, save energy, reduce consumption and improve comprehensive benefits.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention firstly provides a polyethylene glycol separation system, which comprises a TEG tower, a TEG storage tank, a cooler, a tower kettle pump, a reboiler, a separation unit, a PEG storage tank and a PEG delivery pump, wherein materials at the bottom of the TEG tower pass through the tower kettle pump, part of materials at the bottom of the TEG tower are sent to the reboiler, the other part of materials at the bottom of the TEG tower are sent to the separation unit and are separated into partial PEG materials and partial TEG materials by the separation unit, the separated partial PEG materials are sent to the PEG storage tank and are sent out of the world for storage by the PEG delivery pump, and the separated partial TEG materials are sent to the cooler for cooling and then are sent to the TEG storage tank.
As a preferred embodiment of the present invention, the feed to the reboiler section is in the range of 1/4 to 1/2.
As a preferable scheme of the invention, the TEG tower is internally provided with 3 sections of packed beds, the top of the TEG tower is provided with a condenser, and a liquid collecting tank is arranged below the condenser.
As a preferable scheme of the invention, the TEG tower comprises a feed filter, enters the TEG tower, is filtered by the feed filter and then enters a space between a first section of packed bed and a second section of packed bed of the TEG tower, and a TEG product is collected from a side line.
As a preferable aspect of the present invention, the present invention further includes a reflux pump, and the reflux pump is connected to the TEG tower and the cooler, respectively.
As a preferable scheme of the invention, the TEG storage tank also comprises a TEG delivery pump, and the TEG in the TEG storage tank is pumped out of the external storage through the TEG delivery pump.
As a preferable aspect of the present invention, the separation unit includes a resin separation system.
The invention also provides a polyethylene glycol separation method adopting the separation system, and the polyethylene glycol separation method comprises the following steps: the material from the DEG tower bottom enters the TEG tower after being filtered, TEG products are extracted from the side line of the TEG tower, part of the material at the bottom of the TEG tower is sent to a reboiler to reflux, part of the material is sent to a separation unit to be separated into partial PEG material and partial TEG material, the separated partial PEG material is sent to a PEG storage tank and is sent out of the outside by a PEG conveying pump to be stored, and the separated partial TEG material is sent to a cooler to be cooled and then is sent to the TEG storage tank.
As a preferred embodiment of the present invention, the temperature of the separation unit is 90 ℃, the flow rate is 10m/h, and the pressure is 0.2MPa.
Compared with the prior art, the invention has the following beneficial effects:
1) According to the invention, a separation unit is added in the existing ethylene oxide/ethylene glycol device, a byproduct polyethylene glycol material of the existing device is introduced into the separation unit, impurities in the polyethylene glycol are removed by controlling a certain flow rate, temperature and pressure through resin adsorption selectivity, a triethylene glycol product with higher purity can be separated through an evaporation system, and the yield of the triethylene glycol product can be increased.
2) The impurities in the materials are separated through resin adsorption, so that the separation difficulty of a downstream evaporation system can be reduced, the steam consumed by evaporation separation is reduced, the maintenance frequency of a triethylene glycol evaporation system can be reduced, and the comprehensive benefit is fully improved.
3) The method can ensure that impurities in the polyethylene glycol are removed, improve the cleanliness of materials, increase the treatment efficiency and effect of a subsequent evaporation analysis system, and improve the quality and yield of a triethylene glycol product.
4) The method can ensure that the components of the polyethylene glycol entering the triethylene glycol evaporation separation system are more single, and greatly reduce the steam consumption of the triethylene glycol evaporation separation.
5) By the method, the separation rate of the triethylene glycol product in the polyethylene glycol byproduct can be improved by 10%; the yield of the triethylene glycol is increased, and the yield of the triethylene glycol can be increased by 11 tons every year; the steam consumption of the evaporation separation system can be reduced, and the steam consumption can be reduced by about 50kg/h.
Drawings
FIG. 1 is a schematic of the present invention.
In the figure, 1.Teg column; 2. a reboiler; 3. a condenser; a TEG storage tank; 5. a separation unit; 6, PEG storage tank; 7. a cooler; 8. a tower kettle pump; 9. a feed filter; 10. a reflux pump; a PEG delivery pump; TEG transfer pump.
Detailed Description
For a further understanding of the present invention, reference will now be made in detail to the embodiments illustrated in the drawings.
The present application will be described in further detail with reference to the following drawings and examples. It is to be understood that the specific embodiments described herein are merely illustrative of the relevant invention and not restrictive of the invention. It should be noted that, for convenience of description, only the portions related to the present invention are shown in the drawings. The terms first, second, and the like in the present invention are provided for convenience of describing the technical solution of the present invention, and have no specific limiting effect, but are all generic terms, and do not limit the technical solution of the present invention. It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc., indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience of description and simplicity of description, but do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance. Unless expressly stated or limited otherwise, the terms "mounted," "connected," and "connected" are intended to be inclusive and mean, for example, that they may be fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in a specific case to those of ordinary skill in the art. The technical solutions in the same embodiment and the technical solutions in different embodiments can be arranged and combined to form a new technical solution without contradiction or conflict, and the technical solutions are within the scope of the present invention.
Referring to fig. 1, the present invention first provides a polyethylene glycol separation system, which comprises a TEG column 1, a reboiler 2, a condenser 3, a TEG storage tank 4, a separation unit 5, a peg storage tank 6, a cooler 7, a column bottom pump 8, a feed filter 9, a reflux pump 10, a peg transfer pump 11 and a TEG transfer pump 12.
The TEG tower 1 has 3 packed beds at an operating pressure of 1.33KPa, a condenser 3 is provided in the TEG tower 1, and a liquid collecting tank (not shown) is installed below the condenser 3 for collecting condensate to facilitate reflux.
The material received by the TEG tower 1 is from the material of the DEG tower kettle, the material is filtered by a feeding filter 9 and then enters between the 1 st section filler and the 2 nd section filler of the TEG tower 1, the TEG product is extracted from the side line, one part of the TEG product is sent to the TEG tower 1 through a reflux pump 10 for reflux, the other part of the TEG product is sent to a cooler 7 for cooling, and then the TEG product is collected in a TEG storage tank 4 and finally sent out for external storage through a TEG conveying pump 12.
And (3) feeding a part of the material from the bottom of the TEG tower 1 into a reboiler 2 through a tower kettle pump 8, heating and returning the material to the TEG tower 1, feeding the other part of the material into a separation unit 5 for separation to obtain a part of PEG material and a part of TEG material, feeding the separated part of PEG material into a PEG storage tank 6, and finally, feeding the part of PEG material out of the tower through a PEG conveying pump 11 to an evaporation and separation system in the next step.
And sending the separated TEG part material into a cooler 7 for cooling, collecting the cooled TEG part material in a TEG storage tank 4, and finally sending the TEG part material out of the outside for storage through a TEG conveying pump 12.
The separation unit 5 is a resin separation system, which employs a resin that can be directly commercially available for removing impurities from polyethylene glycol.
It may also be a resin prepared by the following method: adding 120 parts by weight of styrene, 12 parts by weight of divinylbenzene, 2 parts by weight of dichloroethane, 3 parts by weight of ZIF-8 nano material and 45 parts by weight of isobutanol into a reaction kettle, reacting at 80 ℃ for 5 hours, heating to 90 ℃ for reaction for 3 hours, and heating to 98 ℃ for reaction for 5 hours to obtain a polymeric white ball; and carrying out sulfonation reaction on the obtained polymeric white balls to obtain the resin.
Example 1
Referring to fig. 1, the method for separating polyethylene glycol provided in this embodiment includes: the material from the DEG tower kettle enters the TEG tower after being filtered, TEG products are extracted from the side line of the TEG tower, 1/2 of the material at the bottom of the TEG tower is sent to a reboiler for backflow, the rest part of the material is sent to a separation unit to be separated into partial PEG material and partial TEG material, the separated partial PEG material is sent to a PEG storage tank and is sent out of the outside for storage by a PEG conveying pump, and the separated partial TEG material is sent to the cooler for cooling and then is sent to the TEG storage tank.
The resins used in the separation unit are commercially available directly in the following types: YJ-1.
The temperature of the separation unit was 90 ℃, the flow rate 10m/h, and the pressure 0.2MPa.
The formaldehyde content of the triethylene glycol is 3ppm by on-line analysis, and a high-purity triethylene glycol product is obtained, wherein the product purity (wt%) is as follows: 99.6 percent, 23 percent of chroma, 78 percent of chroma of cobalt and molybdenum and the recovery rate of the high-purity triethylene glycol product.
Example 2
Referring to fig. 1, the method for separating polyethylene glycol provided in this embodiment includes: the material from the DEG tower kettle enters the TEG tower after being filtered, TEG products are extracted from the side line of the TEG tower, 1/3 of the material at the bottom of the TEG tower is sent to a reboiler for backflow, the rest part of the material is sent to a separation unit to be separated into partial PEG material and partial TEG material, the separated partial PEG material is sent to a PEG storage tank and is sent out of the outside for storage by a PEG conveying pump, and the separated partial TEG material is sent to the cooler for cooling and then is sent to the TEG storage tank.
The resin used in the separation unit is prepared by the above method.
The temperature of the separation unit was 90 ℃, the flow rate 10m/h, and the pressure 0.2MPa.
The formaldehyde content of the triethylene glycol is 3ppm through on-line analysis, and a high-purity triethylene glycol product is obtained, wherein the product purity (wt%) is as follows: 97.8 percent, 23 percent of chroma of cobalt and molybdenum, and 76 percent of recovery rate of high-purity triethylene glycol products.
Comparative example 1, triethylene glycol from an existing ethylene oxide/ethylene glycol co-production plant.
The formaldehyde content of the triethylene glycol is 5ppm by on-line analysis, and a high-purity triethylene glycol product is obtained, wherein the product purity (wt%) is as follows: 93.6 percent, 26 percent of chroma, cobalt molybdenum chroma and 65 percent of recovery rate of triethylene glycol products.
Therefore, the invention adds a separation unit in the existing ethylene oxide/ethylene glycol device, leads the by-product polyethylene glycol material of the existing device to the separation unit, removes impurities in the polyethylene glycol by controlling certain flow rate, temperature and pressure through resin adsorption selectivity, and can separate a triethylene glycol product with higher purity through an evaporation system and improve the yield of the triethylene glycol product.
The impurities in the materials are separated through resin adsorption, the separation difficulty of a downstream evaporation system can be reduced, the steam consumed by evaporation separation is reduced, the overhaul frequency of the triethylene glycol evaporation system can be reduced, the comprehensive benefit is fully improved, the high-pressure steam consumption of the triethylene glycol evaporation system can be reduced by about 50kg/h, the steam consumption is reduced by about 400t every year, the steam price per ton is about 240 yuan, and the steam cost can be saved by 9.6 ten thousand yuan every year.
While the invention has been described with respect to a preferred embodiment, it will be understood by those skilled in the art that the foregoing and other changes, omissions and deviations in the form and detail thereof may be made without departing from the scope of this invention. Those skilled in the art can make various changes, modifications and equivalent arrangements, which are equivalent to the embodiments of the present invention, without departing from the spirit and scope of the present invention, and which may be made by utilizing the techniques disclosed above; meanwhile, any changes, modifications and variations of the above-described embodiments, which are equivalent to those of the technical spirit of the present invention, are within the scope of the technical solution of the present invention.

Claims (9)

1. A polyethylene glycol separation system is characterized by comprising a TEG tower, a TEG storage tank, a cooler, a tower kettle pump, a reboiler, a separation unit, a PEG storage tank and a PEG conveying pump, wherein materials at the bottom of the TEG tower pass through the tower kettle pump, a part of materials at the bottom of the TEG tower are conveyed to the reboiler, the other part of materials at the bottom of the TEG tower are conveyed to the separation unit and are separated into partial PEG materials and partial TEG materials through the separation unit, the separated partial PEG materials are conveyed to the PEG storage tank and are conveyed out of the world for storage through the PEG conveying pump, and the separated partial TEG materials are conveyed to the cooler for cooling and are conveyed to the TEG storage tank.
2. The polyethylene glycol separation system of claim 1, wherein the feed to the reboiler section is in the range of 1/4 to 1/2.
3. The system as claimed in claim 1, wherein the TEG tower contains 3 packed beds, the TEG tower is provided with a condenser at the top, and a liquid collecting tank is arranged below the condenser.
4. The system for separating polyethylene glycol according to claim 3, further comprising a feed filter, wherein the TEG product enters the TEG tower and is filtered by the feed filter, and then enters between the first section packed bed and the second section packed bed of the TEG tower, and the TEG product is extracted from a side line.
5. The polyethylene glycol separation system of claim 1, further comprising a reflux pump, wherein the reflux pump is connected to the TEG tower and the cooler respectively.
6. The polyethylene glycol separation system of claim 1, further comprising a TEG transfer pump, wherein TEG in the TEG storage tank is pumped out of the external storage via the TEG transfer pump.
7. The polyethylene glycol separation system of claim 1, wherein the separation unit comprises a resin separation system.
8. A method for separating polyethylene glycol, wherein the method for separating polyethylene glycol employs the polyethylene glycol separation system according to any one of claims 1 to 7, and comprises: the material from the DEG tower bottom enters the TEG tower after being filtered, TEG products are extracted from the side line of the TEG tower, part of the material at the bottom of the TEG tower is sent to a reboiler to reflux, part of the material is sent to a separation unit to be separated into partial PEG material and partial TEG material, the separated partial PEG material is sent to a PEG storage tank and is sent out of the outside by a PEG conveying pump to be stored, and the separated partial TEG material is sent to a cooler to be cooled and then is sent to the TEG storage tank.
9. The process of claim 8, wherein the separation unit has a temperature of 90 ℃, a flow rate of 10m/h and a pressure of 0.2MPa.
CN202210853427.0A 2022-07-08 2022-07-08 Polyethylene glycol separation system and separation method Pending CN115155091A (en)

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Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA1330350C (en) * 1986-10-07 1994-06-21 Thomas Martin Schmitt Method for purification of ethylene glycol
JP2001031600A (en) * 1999-07-14 2001-02-06 Nippon Shokubai Co Ltd Production of highly pure monoethylene glycol
CN101058526A (en) * 2007-04-11 2007-10-24 江苏工业学院 Method of increasing quality of glycol
CN203370311U (en) * 2013-07-05 2014-01-01 三江化工有限公司 Efficient plate-type mono ethylene glycol (MEG) tower system
CN104649898A (en) * 2015-02-16 2015-05-27 曲靖众一合成化工有限公司 Method and device for producing 2-naphthol and coproducing 2,3 acid by solvent method continuous carbonization
CN105315132A (en) * 2014-07-23 2016-02-10 中国石化工程建设有限公司 System and method used for energy utilization between ethylene glycol device dehydrating tower and refining tower
CN106542975A (en) * 2016-10-17 2017-03-29 中石化上海工程有限公司 The method of continuous production high-purity triethylene glycol
CN109293475A (en) * 2018-11-15 2019-02-01 北京兴高化学技术有限公司 Coal-ethylene glycol refining methd and system
CN109956851A (en) * 2019-04-08 2019-07-02 宁波中科远东催化工程技术有限公司 The system and method for ethylene glycol rectifying in synthesis gas preparing ethylene glycol
CN212440073U (en) * 2020-03-13 2021-02-02 三江化工有限公司 Reboiling system of ethylene glycol tower
CN112321397A (en) * 2020-10-19 2021-02-05 中国石油化工股份有限公司 Novel method for increasing yield of triethylene glycol by EOEG device

Patent Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA1330350C (en) * 1986-10-07 1994-06-21 Thomas Martin Schmitt Method for purification of ethylene glycol
JP2001031600A (en) * 1999-07-14 2001-02-06 Nippon Shokubai Co Ltd Production of highly pure monoethylene glycol
CN101058526A (en) * 2007-04-11 2007-10-24 江苏工业学院 Method of increasing quality of glycol
CN203370311U (en) * 2013-07-05 2014-01-01 三江化工有限公司 Efficient plate-type mono ethylene glycol (MEG) tower system
CN105315132A (en) * 2014-07-23 2016-02-10 中国石化工程建设有限公司 System and method used for energy utilization between ethylene glycol device dehydrating tower and refining tower
CN104649898A (en) * 2015-02-16 2015-05-27 曲靖众一合成化工有限公司 Method and device for producing 2-naphthol and coproducing 2,3 acid by solvent method continuous carbonization
CN106542975A (en) * 2016-10-17 2017-03-29 中石化上海工程有限公司 The method of continuous production high-purity triethylene glycol
CN109293475A (en) * 2018-11-15 2019-02-01 北京兴高化学技术有限公司 Coal-ethylene glycol refining methd and system
CN109956851A (en) * 2019-04-08 2019-07-02 宁波中科远东催化工程技术有限公司 The system and method for ethylene glycol rectifying in synthesis gas preparing ethylene glycol
CN212440073U (en) * 2020-03-13 2021-02-02 三江化工有限公司 Reboiling system of ethylene glycol tower
CN112321397A (en) * 2020-10-19 2021-02-05 中国石油化工股份有限公司 Novel method for increasing yield of triethylene glycol by EOEG device

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