CN115040882A - Device and method for removing ethylene glycol impurities - Google Patents

Device and method for removing ethylene glycol impurities Download PDF

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Publication number
CN115040882A
CN115040882A CN202210817796.4A CN202210817796A CN115040882A CN 115040882 A CN115040882 A CN 115040882A CN 202210817796 A CN202210817796 A CN 202210817796A CN 115040882 A CN115040882 A CN 115040882A
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Prior art keywords
glycol
ethylene glycol
pump
tower
product
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CN202210817796.4A
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Chinese (zh)
Inventor
蒋宇春
张军
顾冬磊
陆叶萍
时勤飞
方群聪
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Zhejiang Sanjiang Chemical New Material Co ltd
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Zhejiang Sanjiang Chemical New Material Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/007—Energy recuperation; Heat pumps
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/14—Fractional distillation or use of a fractionation or rectification column
    • B01D3/143—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D36/00—Filter circuits or combinations of filters with other separating devices
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J41/00—Anion exchange; Use of material as anion exchangers; Treatment of material for improving the anion exchange properties
    • B01J41/04—Processes using organic exchangers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J41/00—Anion exchange; Use of material as anion exchangers; Treatment of material for improving the anion exchange properties
    • B01J41/08—Use of material as anion exchangers; Treatment of material for improving the anion exchange properties
    • B01J41/12—Macromolecular compounds
    • B01J41/13—Macromolecular compounds obtained otherwise than by reactions only involving unsaturated carbon-to-carbon bonds
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
    • C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
    • C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
    • C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts

Abstract

The invention discloses a device and a method for removing glycol impurities, and the device comprises a glycol tower, a glycol product pump, a heat exchanger, a cooler, an impurity removal processing unit, an intermediate tank and a product conversion pump, wherein the glycol tower receives liquid glycol conveyed from a drying tower, the glycol tower is sequentially connected with the heat exchanger, the cooler and the impurity removal processing unit through the glycol product pump, the outlet of the impurity removal processing unit is connected with the inlet of the intermediate tank, the outlet of the intermediate tank is connected with the product conversion pump, and the product conversion pump is externally connected with a finished product tank. On the basis of the existing device and process, the invention adds an impurity removal processing unit on the glycol finished product extraction line, thereby improving the ultraviolet UV value of the glycol finished product.

Description

Device and method for removing ethylene glycol impurities
Technical Field
The invention belongs to the field of ethylene glycol production, relates to impurity removal of ethylene glycol, and particularly relates to a device and a method for removing ethylene glycol impurities.
Background
Ethylene glycol is an important organic chemical raw material, has wide application, is mainly used for producing polyester fibers, antifreeze, unsaturated polyester resin, lubricant, plasticizer, nonionic surfactant and the like, and can also be used in the industries of paint, photographic developing solution, brake fluid and printing ink.
At present, the production of large-scale ethylene glycol at home and abroad is a petroleum method, the main raw materials are ethylene and oxygen, a silver catalyst and methane or nitrogen are used as a stabilizing agent, the ethylene is directly oxidized into ethylene oxide, and then the ethylene glycol is regenerated. However, with the increasing exhaustion of petroleum resources, the ethylene glycol produced by the process has been completely unable to meet the increasing global demand for ethylene glycol.
In the existing ethylene oxide/ethylene glycol co-production device and process, a large amount of impurities are produced in the reaction process when the catalyst runs to the final stage along with the lapse of time, so that the ultraviolet UV values of ethylene glycol products at 220nm and 275nm are sharply reduced, the discontinuity of the ethylene glycol products cannot reach the enterprise-level qualified standard, and the unqualified products are re-refined, so that a large amount of resources are wasted.
Disclosure of Invention
In order to solve the problems, the invention provides a device and a method for removing glycol impurities, and by the device and the method, the ultraviolet UV value can be improved from the original 80-85 to 85-90, the ultraviolet UV value under 275nm can reach more than 95, and various analysis indexes of a glycol finished product produced at the final stage of catalyst operation can still be stably kept above the qualified standard.
In order to achieve the purpose, the invention adopts the following technical scheme:
the utility model provides a device of desorption ethylene glycol impurity, includes ethylene glycol tower, ethylene glycol product pump, heat exchanger, cooler, edulcoration processing unit, intermediate tank and product conversion pump, the ethylene glycol tower is received from the liquid ethylene glycol that the drying tower carried, the ethylene glycol tower pass through ethylene glycol product pump in proper order with the heat exchanger, the cooler and edulcoration processing unit connects, the export of edulcoration processing unit with the entry linkage of intermediate tank, the export of intermediate tank with the product conversion pump is connected, the external finished product jar of product conversion pump.
As a preferable scheme of the invention, the system further comprises a feeding filter, an overhead condenser and a reflux tank, wherein the feeding filter is connected with the ethylene glycol tower, the overhead condenser of the ethylene glycol tower is connected with the overhead condenser, and the overhead condenser is connected with the reflux tank.
The preferable scheme of the invention also comprises a reboiler, a reboiler circulating pump and a reboiling preheater, wherein the bottom of the ethylene glycol tower is sequentially connected with the reboiling preheater and the reboiler through the reboiler circulating pump.
As a preferable scheme of the invention, the system further comprises a tower bottom pump, and tower bottom liquid of the ethylene glycol tower is conveyed to an external separation tower through the tower bottom pump.
The invention also comprises a reflux pump, wherein the reflux tank is refluxed to the top of the ethylene glycol tower through the reflux pump.
As a preferable aspect of the present invention, the impurity removal processing unit includes a resin processor.
As a preferable scheme of the invention, the tower top condenser further comprises a condenser sewage pump, and the condenser sewage pump is connected with the tower top condenser.
The second aspect of the invention provides a method for removing glycol impurities by using the device.
As a preferred aspect of the present invention, the method comprises: before the finished ethylene glycol product is extracted, impurity removal treatment is carried out, wherein the impurity removal treatment comprises the following steps: and recovering waste heat of the crude glycol, cooling, treating by a processor to remove aldehyde, acid and iron impurities in the crude glycol, collecting the treated glycol in an intermediate tank, and storing to obtain the polyester-grade glycol.
As a preferable scheme of the invention, the ultraviolet UV value of the finished product of the glycol at 220nm is more than or equal to 85, and the ultraviolet UV value at 275nm is more than or equal to 95.
Compared with the prior art, the invention has the following beneficial effects:
1) on the basis of the existing device and process, the invention adds an impurity removal processing unit on the extraction line of the finished product of the glycol, thereby improving the ultraviolet UV value of the finished product of the glycol;
2) the ultraviolet UV value of the glycol product obtained by the device and the method of the invention under 220nm can be improved from the original 80-85 to 85-90, the ultraviolet UV value under 275nm can reach more than 95, and various analysis indexes of the glycol finished product produced at the final stage of the catalyst operation can still be stably kept above the qualified standard;
3) according to the method, the consumption of sulfuric acid, caustic soda and sodium bisulfite of the water treatment device can be reduced by about 15 tons each month compared with the original consumption;
4) in the whole catalyst service cycle, the waste water production of the device can be reduced by about 10 percent, thereby saving a large amount of steam and desalted water consumption and achieving the effects of energy conservation and consumption reduction.
Drawings
FIG. 1 is a schematic view of the apparatus of the present invention.
In the figure, 1. feed filter; 2. a condenser sewage pump; 3. an ethylene glycol column; 4. a reboiler; 5. a reboiling preheater; 6. a reboiler circulation pump; 7. a reflux pump; 8. a tower top condenser; 9. a tower bottom pump; 10. a glycol product pump; 11. a reflux tank; 12. a heat exchanger; 13. a cooler; 14. an impurity removal processing unit; 15. an intermediate tank; 16. and (4) a product switching 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 specific cases to those skilled 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 firstly provides a device for removing ethylene glycol impurities, based on the existing ethylene oxide/ethylene glycol co-production device of the applicant, an impurity removal processing unit is added on the existing production line, and comprises a feed filtration unit 1, a condenser sewage pump 2, an ethylene glycol tower 3, a reboiler 4, a reboiling preheater 5, a reboiler circulating pump 6, a reflux pump 7, an overhead condenser 8, a tower bottom pump 9, an ethylene glycol product pump 10, a reflux tank 11, a heat exchanger 12, a cooler 13, an impurity removal processing unit 14, an intermediate tank 15 and a product conversion pump 16, which are respectively connected through a pipeline.
Tower bottoms from a drying tower (not shown in the figure) are sent to an ethylene glycol tower 3 through a feeding filter 1, a 3-section packed bed is arranged in the ethylene glycol tower 3, a fiber-grade monoethylene glycol product is extracted through a liquid side line, the residual heat is recovered through a heat exchanger 12, then the fiber-grade monoethylene glycol product enters a cooler 13 for further cooling, passes through an impurity removal processing unit 14, is collected in an intermediate tank 15, and finally is sent to the outside of a boundary area for storage through a product conversion pump 16.
The reboiling heat of the ethylene glycol column 3 is provided by a reboiler preheater 5 and a reboiler 4, the heat source is from high pressure steam, and the reboiler preheater 5 and the reboiler 4 are circulated in series by a reboiler circulation pump 6.
The bottom liquid of the ethylene glycol tower 3 is sent to an external separation tower through a tower bottom pump 9.
The top of the ethylene glycol tower 3 is connected with a tower top condenser 8 for removing residual moisture and volatile impurities and reducing the concentration of aldehyde and UV impurities in the product, the steam at the top of the tower firstly enters the tower top condenser 8, most of gas phase is condensed after partial heat is condensed and recovered from tower bottom liquid from a stripping tower (not shown in the figure), and condensate is sent into a reflux tank 11 and sent into the top of the ethylene glycol tower 3 as reflux through a reflux pump 7.
The overhead condenser 8 discharges impurities through the condenser blow-down pump 2.
The impurity-removing raw materials in the invention are as follows:
H 2 COH-H 2 COH+R-HC＝O→(H 3 C-O) 2 CH-R+H 2 O.。
the impurity removal processing unit 14 is a resin processor, and the resin used may be a commercially available resin for removing impurities such as aldehyde, acid, and iron, or may 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, in the method for removing ethylene glycol impurities provided in this embodiment, before a finished ethylene glycol product is extracted, impurity removal processing is performed, where the impurity removal processing includes: recovering waste heat of the crude glycol, cooling, treating by a processor to remove aldehyde, acid and iron impurities in the crude glycol, collecting the treated glycol in an intermediate tank, and storing to obtain polyester-grade glycol, wherein the resin used in the processor is macroporous weakly-alkaline acrylic acid series anion exchange resin (D640).
Example 2
The only difference was that the resin used in the treater was the resin prepared as described above, as in example 1. Comparative example 1, ethylene glycol produced by an existing ethylene oxide/ethylene glycol co-production plant.
The ethylene glycol obtained in the initial stage and the final stage of the operation of the catalyst in example 1, example 2 and comparative example 1 respectively is analyzed and tested, the UV value and the chromaticity are tested, the test result is in accordance with the national standard, and the results are shown in the table 1 in the GB4649-2008 industrial ethylene glycol standard.
TABLE 1 test results
Figure BDA0003741557910000041
Therefore, the ultraviolet UV value of the ethylene glycol product obtained by the device and the method can be improved from 80-85 to 85-90 at 220nm, the ultraviolet UV value at 275nm can reach more than 95, and various analysis indexes of the ethylene glycol finished product produced at the final stage of catalyst operation can be still stably kept above the qualified standard.
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 (10)

1. The device for removing the ethylene glycol impurities is characterized by comprising an ethylene glycol tower, an ethylene glycol product pump, a heat exchanger, a cooler, an impurity removal processing unit, an intermediate tank and a product conversion pump, wherein the ethylene glycol tower receives liquid ethylene glycol conveyed from a drying tower, the ethylene glycol tower is sequentially connected with the heat exchanger, the cooler and the impurity removal processing unit through the ethylene glycol product pump, an outlet of the impurity removal processing unit is connected with an inlet of the intermediate tank, an outlet of the intermediate tank is connected with the product conversion pump, and the product conversion pump is externally connected with a finished product tank.
2. The apparatus according to claim 1, further comprising a feed filter, an overhead condenser and a reflux tank, wherein the feed filter is connected to the ethylene glycol tower, the overhead condenser of the ethylene glycol tower is connected to the overhead condenser, and the overhead condenser is connected to the reflux tank.
3. The apparatus for removing glycol impurities as claimed in claim 1, further comprising a reboiler, a reboiler circulating pump and a reboiling preheater, wherein the bottom of the glycol tower is sequentially connected with the reboiling preheater and the reboiler through the reboiler circulating pump.
4. The device for removing the ethylene glycol impurities according to claim 2, further comprising a bottom pump, wherein the bottom liquid of the ethylene glycol tower is conveyed to the external separation tower through the bottom pump.
5. The apparatus for removing glycol impurities as claimed in claim 2, further comprising a reflux pump, wherein the reflux tank is refluxed to the top of the glycol tower by the reflux pump.
6. The apparatus according to claim 1, wherein the impurity removal unit comprises a resin processor.
7. The apparatus of claim 2, further comprising a condenser blowdown pump, wherein the condenser blowdown pump is connected to the overhead condenser.
8. A method for removing ethylene glycol impurities, characterized in that the device according to any one of claims 1-7 is used.
9. The method for removing the ethylene glycol impurity as claimed in claim 8, wherein the method comprises: before the finished ethylene glycol product is extracted, impurity removal treatment is carried out, wherein the impurity removal treatment comprises the following steps: and recovering waste heat of the crude glycol, cooling, treating by a processor to remove aldehyde, acid and iron impurities in the crude glycol, collecting the treated glycol in an intermediate tank, and storing to obtain the polyester-grade glycol.
10. The method for removing the impurities in the glycol as claimed in claim 9, wherein the ultraviolet UV value of the finished glycol product at 220nm is not less than 85, and the ultraviolet UV value at 275nm is not less than 95.
CN202210817796.4A 2022-07-12 2022-07-12 Device and method for removing ethylene glycol impurities Pending CN115040882A (en)

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Citations (5)

* 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
CN203620271U (en) * 2014-02-27 2014-06-04 三江湖石化工有限公司 High-efficiency ethylene glycol product waste heat recovery device
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

Patent Citations (5)

* 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
CN203620271U (en) * 2014-02-27 2014-06-04 三江湖石化工有限公司 High-efficiency ethylene glycol product waste heat recovery device
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

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