CN115215732A - Method and equipment for purifying ethylene glycol - Google Patents
Method and equipment for purifying ethylene glycol Download PDFInfo
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- CN115215732A CN115215732A CN202210810786.8A CN202210810786A CN115215732A CN 115215732 A CN115215732 A CN 115215732A CN 202210810786 A CN202210810786 A CN 202210810786A CN 115215732 A CN115215732 A CN 115215732A
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- ethylene glycol
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- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 title claims abstract description 114
- 238000000034 method Methods 0.000 title claims abstract description 19
- 239000007788 liquid Substances 0.000 claims abstract description 56
- 238000001914 filtration Methods 0.000 claims abstract description 48
- 238000000746 purification Methods 0.000 claims abstract description 16
- 239000011552 falling film Substances 0.000 claims abstract description 11
- 239000000047 product Substances 0.000 claims abstract description 11
- 238000002425 crystallisation Methods 0.000 claims abstract description 10
- 230000008025 crystallization Effects 0.000 claims abstract description 10
- 239000012535 impurity Substances 0.000 claims abstract description 10
- 239000012043 crude product Substances 0.000 claims abstract description 9
- 238000000926 separation method Methods 0.000 claims abstract description 7
- 238000001179 sorption measurement Methods 0.000 claims abstract description 7
- 238000002844 melting Methods 0.000 claims abstract description 6
- 230000008018 melting Effects 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 239000007787 solid Substances 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims abstract description 3
- 238000000967 suction filtration Methods 0.000 claims description 15
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 14
- 239000000155 melt Substances 0.000 claims description 6
- 239000012528 membrane Substances 0.000 claims description 5
- 238000000108 ultra-filtration Methods 0.000 claims description 5
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- 238000003828 vacuum filtration Methods 0.000 claims description 4
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 abstract description 3
- 239000000706 filtrate Substances 0.000 description 7
- 239000012071 phase Substances 0.000 description 5
- 239000002245 particle Substances 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical class [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000005984 hydrogenation reaction Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 238000010000 carbonizing Methods 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- 239000013043 chemical agent Substances 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000004042 decolorization Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 230000032258 transport Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
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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
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D29/00—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor
- B01D29/01—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor with flat filtering elements
- B01D29/03—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor with flat filtering elements self-supporting
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D29/00—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor
- B01D29/50—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor with multiple filtering elements, characterised by their mutual disposition
- B01D29/56—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor with multiple filtering elements, characterised by their mutual disposition in series connection
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0059—General arrangements of crystallisation plant, e.g. flow sheets
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/02—Crystallisation from solutions
-
- 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
-
- 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
- C07C29/78—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by condensation or crystallisation
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to the technical field of glycol purification, in particular to a method and equipment for purifying glycol, which comprises the following steps; s1, physical filtration: carrying out primary filtration on the ethylene glycol crude product by adopting an adsorption filtration device, and removing impurities and decoloring; s2, melt crystallization: putting the filtered product obtained in the step S1 into a falling film crystallizer, heating to melt, and then cooling to crystallize; s3, solid-liquid separation: carrying out solid-liquid separation on the crystallized product obtained in the step S2, and taking a solid; and S4, repeating the steps S2-S3 to obtain the high-purity ethylene glycol. The equipment comprises a filtering component, a melting crystallizer and a liquid conveying pipe for communicating the filtering component and the melting crystallizer. The method does not need to add other chemical reagents, combines physical filtration and a falling film crystallizer, accelerates the purification process and has better purification effect.
Description
Technical Field
The invention relates to the technical field of ethylene glycol purification, in particular to a method and equipment for purifying ethylene glycol.
Background
Ethylene glycol is an important chemical raw material, has wide application and can be used as an antifreezing agent and a raw material of polyester fibers. Due to the different technical routes of ethylene glycol production, the impurity types are also many, but the main substances which are generally accepted to influence the UV value of the product at present are compounds containing carbonyl or conjugated double bonds.
In order to purify the crude ethylene glycol, chinese patent CN107973698A discloses a method for purifying ethylene glycol. The method comprises the following steps: (1) physical adsorption: carrying out physical adsorption on the ethylene glycol crude product through an activated carbon bed layer to obtain a first material flow; (2) hydrofining: contacting the first material flow, hydrogen and a composite hydrogenation catalyst for reaction; the composite hydrogenation catalyst comprises: continuous phase carbon and dispersed phase Raney alloy particles, wherein the dispersed phase Raney alloy particles are uniformly or non-uniformly dispersed in the continuous phase carbon, and the continuous phase carbon is obtained by carbonizing a carbonizable organic matter or a mixture thereof. The method can realize high-efficiency purification and obviously improve the ultraviolet transmittance of the glycol.
However, the above techniques still have the following drawbacks: 1) The purification process is complex and involves various equipment and instruments; 2) Other chemical agents need to be added, and new impurities are easy to appear.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method and equipment for purifying ethylene glycol, which do not need to add other chemical reagents, combine physical filtration and a falling film crystallizer, accelerate the purification process and have better purification effect.
In order to solve the technical problems, the invention adopts the following technical scheme:
a method for purifying ethylene glycol comprises the following steps;
s1, physical filtration: carrying out primary filtration on the ethylene glycol crude product by adopting an adsorption filtration device, and removing impurities and decoloring;
s2, melt crystallization: putting the filtered product obtained in the step S1 into a falling film crystallizer, heating to melt, and then cooling to crystallize;
s3, solid-liquid separation: carrying out solid-liquid separation on the crystallized product obtained in the step S2, and taking a solid;
and S4, repeating the steps S2-S3 to obtain the high-purity ethylene glycol.
Preferably, the physical filtration in step S1 is vacuum filtration using nanoscale activated carbon.
Preferably, the melting temperature in step S2 is 80-100 ℃ and the crystallization temperature is-30 to-20 ℃.
The ethylene glycol purification equipment comprises a filtering component, a melt crystallizer and a liquid conveying pipe for communicating the filtering component and the melt crystallizer.
Preferably, the filtering assembly comprises a first filtering tank, a first liquid storage tank, a second filtering tank and a second liquid storage tank which are sequentially and continuously arranged, a liquid outlet of the first filtering tank is communicated with a liquid inlet of the first liquid storage tank, a liquid outlet of the first liquid storage tank is communicated with a liquid inlet of the second filtering tank, a liquid outlet of the second filtering tank is communicated with a liquid inlet of the second liquid storage tank, a liquid outlet of the second liquid storage tank is communicated with the melting crystallizer through a liquid conveying pipe, and a control valve is arranged on the liquid conveying pipe; the first filtration tank and the second filtration tank are respectively provided with a first filter plate and a second filter assembly, the first filtration tank and the second filtration tank are independently provided with vacuum pumps, and the first liquid storage tank and the second liquid storage tank are respectively provided with a liquid level sensor.
Preferably, the second filtering component comprises a supporting filter screen and a second filtering plate, the second filtering plate comprises an ultrafiltration membrane shell, and nano activated carbon is filled in the ultrafiltration membrane shell.
The invention has the beneficial effects that:
in the actual use scenario, the crude ethylene glycol product is firstly subjected to vacuum filtration to remove impurities such as particles and suspended matters, and then is subjected to multistage crystallization operation by using a falling film crystallizer to obtain high-purity ethylene glycol. The method does not need to add other chemical reagents, combines physical filtration and a falling film crystallizer, accelerates the purification process and has better purification effect.
Drawings
FIG. 1 is a schematic diagram of the apparatus of the present invention.
Reference numerals:
1-a filter assembly; 11-a first suction filtration tank; 111-a first filter plate; 12-a first reservoir; 13-a second suction filtration tank; 131-supporting a screen; 132-a second filter plate; 14-a second reservoir; 15-a vacuum pump; 16-a liquid level sensor; 2-a melt crystallizer; 3-transfusion tube.
Detailed Description
In order to facilitate understanding of those skilled in the art, the present invention is further described below with reference to the following examples and the accompanying drawings, which are not intended to limit the present invention.
Example 1
Physical filtration: and (3) preliminarily filtering the ethylene glycol crude product by adopting an adsorption filtering device, and removing impurities and decoloring. Putting the crude ethylene glycol raw material into a first suction filtration tank 11, starting a vacuum pump 15 on the first suction filtration tank 11 to perform suction filtration, allowing filtrate to flow into a first liquid storage tank 12 through an outlet of the first suction filtration tank 11 for temporary storage, and performing primary filtration to remove common particles and suspended impurities; when a certain amount of filtrate is stored, the filtrate is pumped to the second suction and filtration tank 13 through a pipeline which is communicated with the first liquid storage tank 12 and the second suction and filtration tank 13, and a liquid pump is arranged on the pipeline and can be manually controlled to open and close, or a circuit can be designed to be connected with a central controller for automatic control; the second suction filtration tank 13 is opened to carry out suction filtration again on the primary filtrate, the filtrate flows into the second liquid storage tank 14 through the outlet of the second suction filtration tank 13 for temporary storage, and the secondary suction filtration is carried out for decolorization and filtration of macromolecules through the adsorption of an ultrafiltration membrane and nanoscale activated carbon; the liquid level sensor 16 is used to monitor the liquid level in the first liquid storage tank 12 and the second liquid storage tank 14 at any time, which facilitates the adjustment of the process progress in time.
Example 2
Melting and crystallizing: and (3) putting the filtered product obtained in the previous step into a falling film crystallizer to be heated and melted, and then cooling and crystallizing. Conveying the filtrate subjected to secondary filtration to a falling film crystallizer through a blood conveying pipe 3, preheating the falling film crystallizer to 80-100 ℃, and enabling the filtrate of the ethylene glycol crude product to be in a molten state to evaporate water; cooling the molten ethylene glycol crude product to the crystallization temperature of the ethylene glycol crude product of-20 ℃ at the speed of 10 ℃/h to crystallize the ethylene glycol crude product; then the solid-liquid separation is carried out by a falling film crystallizer, and then the operation of melt crystallization is carried out again on the solid phase product, so as to obtain the high-purity ethylene glycol after multi-stage crystallization.
The mode of earlier through vacuum filtration with the ethylene glycol crude gets rid of impurity such as granule wherein and suspended solid, then utilizes the falling liquid film crystallizer to carry out multistage crystallization operation, acquires high-purity ethylene glycol, compares in single purification mode among the traditional technical scheme, and two kinds of modes cooperate, can effectively save the process time, and whole journey need not to add other chemical reagent, has prevented secondary impurity, and whole process need not artifical contact and transports, and the operating environment is cleaner. The purity of the obtained product is as high as 99.95 percent.
All technical features in the embodiment can be subjected to appearance modification according to actual needs.
The above embodiments are preferred implementations of the present invention, and the present invention can be implemented in other ways without departing from the spirit of the present invention.
Claims (6)
1. A method for purifying ethylene glycol is characterized in that: comprises the following steps;
s1, physical filtration: preliminarily filtering the ethylene glycol crude product by adopting an adsorption filtering device, and removing impurities and decoloring;
s2, melt crystallization: putting the filtered product obtained in the step S1 into a falling film crystallizer, heating to melt, and then cooling to crystallize;
s3, solid-liquid separation: carrying out solid-liquid separation on the crystallized product obtained in the step S2, and taking a solid;
and S4, repeating the steps S2-S3 to obtain the high-purity ethylene glycol.
2. The method for purifying ethylene glycol according to claim 1, wherein: and the physical filtration in the step S1 adopts nanoscale active carbon for vacuum filtration.
3. The method for purifying ethylene glycol according to claim 1, wherein: the melting temperature in the step S2 is 80-100 ℃, and the crystallization temperature is-30 to-20 ℃.
4. An ethylene glycol purification apparatus of an ethylene glycol purification method according to any one of claims 1 to 3, characterized in that: comprises a filtering component (1), a melt crystallizer (2) and a liquid conveying pipe (3) for communicating the filtering component (1) and the melt crystallizer (2).
5. The ethylene glycol purification apparatus according to claim 4, wherein: the filtering component (1) comprises a first suction filtration tank (11), a first liquid storage tank (12), a second suction filtration tank (13) and a second liquid storage tank (14) which are sequentially and continuously arranged, wherein a liquid outlet of the first suction filtration tank (11) is communicated with a liquid inlet of the first liquid storage tank (12), a liquid outlet of the first liquid storage tank (12) is communicated with a liquid inlet of the second suction filtration tank (13), a liquid outlet of the second suction filtration tank (13) is communicated with a liquid inlet of the second liquid storage tank (14), a liquid outlet of the second liquid storage tank (14) is communicated with the melt crystallizer (2) through a liquid conveying pipe (3), and a control valve is arranged on the liquid conveying pipe (3);
the device is characterized in that a first filtering plate (111) and a second filtering component are respectively arranged on the first filtering tank (11) and the second filtering tank (13), the first filtering tank (11) and the second filtering tank (13) are independently provided with a vacuum pump (15), and liquid level sensors (16) are respectively arranged in the first liquid storage tank (12) and the second liquid storage tank (14).
6. The ethylene glycol purification apparatus according to claim 5, wherein: the second filter component comprises a support filter screen (131) and a second filter plate (132), the second filter plate (132) comprises an ultrafiltration membrane shell, and nano activated carbon is filled in the ultrafiltration membrane shell.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210810786.8A CN115215732A (en) | 2022-07-11 | 2022-07-11 | Method and equipment for purifying ethylene glycol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210810786.8A CN115215732A (en) | 2022-07-11 | 2022-07-11 | Method and equipment for purifying ethylene glycol |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN115215732A true CN115215732A (en) | 2022-10-21 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210810786.8A Pending CN115215732A (en) | 2022-07-11 | 2022-07-11 | Method and equipment for purifying ethylene glycol |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106866371A (en) * | 2015-12-11 | 2017-06-20 | 上海沃凯生物技术有限公司 | A kind of method that utilization fusion-crystallization purifies ethylene glycol |
| CN206276116U (en) * | 2016-10-25 | 2017-06-27 | 青海省化工设计研究院有限公司 | A kind of fine chemical product filtering and impurity removing device |
| CN206714007U (en) * | 2017-01-19 | 2017-12-08 | 合肥志诚蜂业有限责任公司 | A kind of honey deep processing unit |
| CN107973699A (en) * | 2016-10-25 | 2018-05-01 | 中国石油化工股份有限公司 | The method of purifying ethylene glycol |
| CN107973698A (en) * | 2016-10-25 | 2018-05-01 | 中国石油化工股份有限公司 | The method for purifying ethylene glycol |
| CN110759813A (en) * | 2019-10-23 | 2020-02-07 | 太原理工大学 | Method for purifying coal-to-ethylene glycol based on static melt crystallization device |
| CN215462567U (en) * | 2020-12-31 | 2022-01-11 | 尚鼎环境科技（江苏）有限公司 | Active carbon adsorption experimental apparatus |
-
2022
- 2022-07-11 CN CN202210810786.8A patent/CN115215732A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106866371A (en) * | 2015-12-11 | 2017-06-20 | 上海沃凯生物技术有限公司 | A kind of method that utilization fusion-crystallization purifies ethylene glycol |
| CN206276116U (en) * | 2016-10-25 | 2017-06-27 | 青海省化工设计研究院有限公司 | A kind of fine chemical product filtering and impurity removing device |
| CN107973699A (en) * | 2016-10-25 | 2018-05-01 | 中国石油化工股份有限公司 | The method of purifying ethylene glycol |
| CN107973698A (en) * | 2016-10-25 | 2018-05-01 | 中国石油化工股份有限公司 | The method for purifying ethylene glycol |
| CN206714007U (en) * | 2017-01-19 | 2017-12-08 | 合肥志诚蜂业有限责任公司 | A kind of honey deep processing unit |
| CN110759813A (en) * | 2019-10-23 | 2020-02-07 | 太原理工大学 | Method for purifying coal-to-ethylene glycol based on static melt crystallization device |
| CN215462567U (en) * | 2020-12-31 | 2022-01-11 | 尚鼎环境科技（江苏）有限公司 | Active carbon adsorption experimental apparatus |
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