CN114272636A - Device and method for separating ethylene glycol monomethyl ether and water through melt crystallization - Google Patents
Device and method for separating ethylene glycol monomethyl ether and water through melt crystallization Download PDFInfo
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- CN114272636A CN114272636A CN202111638497.6A CN202111638497A CN114272636A CN 114272636 A CN114272636 A CN 114272636A CN 202111638497 A CN202111638497 A CN 202111638497A CN 114272636 A CN114272636 A CN 114272636A
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Abstract
The invention discloses a device and a method for separating glycol methyl ether from water by melt crystallization, which comprises a falling film melt crystallizer and an external crystallizer heat exchanger, wherein the top of the external crystallizer heat exchanger is connected with a heat exchanger hot salt water outlet pipeline and a heat exchanger cold salt water inlet pipeline, the bottom of the external crystallizer heat exchanger is connected with a heat exchanger hot salt water inlet pipeline and a heat exchanger cold salt water inlet pipeline, the external crystallizer heat exchanger is connected with a crystallizer shell pass water circulating pump, the top end inside the falling film melt crystallizer is provided with a falling film melt crystallizer distributor, the top of the falling film melt crystallizer is connected with a 15% glycol methyl ether aqueous solution feeding pipeline, the bottom of the falling film melt crystallizer is respectively connected with a material circulating pump, a crystallizer residual liquid tank and a falling film melt crystallizer water tank, the invention has no external solvent and reduces the operation cost, environment-friendly, no three wastes are generated, and moe aqueous solution with the content of 40 percent is recycled.
Description
Technical Field
The invention relates to the field of chemical reagent purification, in particular to a device and a method for separating ethylene glycol monomethyl ether and water by melt crystallization.
Background
Ethylene glycol monomethyl ether (abbreviated as MOE), also called as ethylene glycol monomethyl ether, is an important solvent for furan phenol reaction; is a colorless transparent liquid, and is mixed and dissolved with water, alcohol, acetic acid, acetone and DMF; MOE is used as an important solvent, and widely used as a solvent for various oils and fats, cellulose acetate, cellulose nitrate, alcohol-soluble dyes and synthetic resins;
MOE and water are subjected to azeotropy, and a common rectification method is not suitable for separating ethylene glycol monomethyl ether from water; and in the furan phenol reaction section, MOE is used as a solvent, and the mass fraction of water in the MOE is required to be lower than 0.1 wt%. The prior art directly pumps the waste water solution containing 85 wt% of MOE into a rectifying tower, 15 wt% of MOE water solution is extracted from the top of the rectifying tower and is burnt in an incinerator, 0.1 wt% of MOE water solution is extracted from a tower kettle and is conveyed to a reaction working section to be used as a solvent, the process has high treatment cost, and the MOE waste is serious; the traditional process adopts desiccant anhydrous calcium chloride for dehydration, the amount of the anhydrous calcium chloride accounts for about 10 wt% of the wastewater amount of the MOE, the water content in the MOE can be reduced to be below 0.1 wt%, and then front fraction is removed through rectification to obtain a product; the method has the disadvantages that the anhydrous calcium chloride absorbs water and simultaneously absorbs a certain amount of MOE to form jelly, the recovery is difficult, the environment is polluted by the waste, dangerous solid waste is formed, the treatment cost is high, and the cost for drying and dehydrating is also high; therefore, the device and the method for separating the ethylene glycol monomethyl ether and the water by melt crystallization are provided.
Disclosure of Invention
The invention aims to solve the problems of the prior art by providing a device and a method for separating ethylene glycol monomethyl ether from water by melt crystallization.
In order to achieve the purpose, the invention provides the following technical scheme: a device for separating glycol methyl ether and water by melt crystallization comprises a falling film melt crystallizer and an external heat exchanger of the crystallizer, the top of the external heat exchanger of the crystallizer is connected with a hot brine outlet pipeline of the heat exchanger and a cold brine inlet pipeline of the heat exchanger, the bottom of the external heat exchanger of the crystallizer is connected with a hot brine inlet pipeline of the heat exchanger and a cold brine inlet pipeline of the heat exchanger, the crystallizer external heat exchanger is connected with a crystallizer shell pass water circulating pump, the top end in the falling film melting crystallizer is provided with a falling film melting crystallizer distributor, the top of the falling film melting crystallizer is connected with a 15 percent ethylene glycol methyl ether aqueous solution feeding pipeline, the bottom of the falling film melting crystallizer is respectively connected with a material circulating pump, a crystallizer residual liquid tank and a falling film melting crystallizer water tank, the crystallizer residual liquid tank is connected with a residual liquid extraction pump, and the falling film melting crystallizer water tank is connected with a water extraction pump.
As a preferable technical scheme of the invention, the falling film melting crystallizer distributor is connected with an external heat exchanger of the crystallizer through a pipeline.
As a preferable technical scheme of the invention, the crystallizer shell pass water circulating pump is respectively connected with the falling film melting crystallizer and the external heat exchanger of the crystallizer through pipelines.
As a preferable technical scheme of the invention, the material circulating pump is respectively connected with the top and the bottom of the falling film melting crystallizer through pipelines.
As a preferred technical scheme of the invention, the falling film melting crystallizer water tank is respectively connected with the falling film melting crystallizer and the water extraction pump through pipelines.
As a preferred technical scheme of the invention, the crystallizer residual liquid tank is respectively connected with the falling film melting crystallizer and the residual liquid extraction pump through pipelines.
A method for separating ethylene glycol monomethyl ether from water by melt crystallization comprises the following steps:
s1, liquid-phase feeding: adding an aqueous solution containing 15% of ethylene glycol methyl ether at normal temperature into a falling film melting crystallizer by using a feed pipeline; starting a material circulating pump to circulate materials, and distributing a film on the inner side of a crystallizer tube by using a falling film melting crystallizer distributor;
s2, cooling and crystallizing: starting a crystallizer shell pass water circulating pump, simultaneously controlling the inlet and outlet flows of a heat exchanger cold brine water inlet pipeline and a heat exchanger cold brine water inlet pipeline, controlling the temperature of cold brine to be-10 ℃, and reducing the crystallization rate of ethylene glycol monomethyl ether aqueous solution in the falling film melting crystallizer to be-5 ℃ by controlling the crystallization rate to be 0.02-0.3 ℃/min;
s3, heating and sweating: after 4-8 hours of crystallization, discharging residual liquid into a residual liquid tank of a crystallizer, slowly adding hot brine of a heat exchanger into cold brine to increase the temperature of the cold brine, controlling the temperature to be 0 ℃, increasing the temperature in the falling film melting crystallizer to-2 ℃ at 0.05-0.5 ℃/min, controlling the flow of shell side brine to keep the temperature inside the falling film melting crystallizer constant for 10-30min, obtaining the residual liquid and aqueous solution containing 40% moe of perspiration liquid, discharging the residual liquid and the perspiration liquid into a rectifying tower, and using after purification;
s4, stopping feeding of cold brine, heating hot brine in an external heat exchanger of the crystallizer to melt the materials, melting water into liquid after the temperature is increased to 5-10 ℃ to obtain moe water solution with 99% of water, and discharging the water solution out of the sewage treatment system.
The invention has the beneficial effects that: the method has the advantages of no additional solvent, reduced operation cost, environmental friendliness, no generation of three wastes, and recovery of moe aqueous solution containing 40%.
Drawings
FIG. 1 is a schematic structural diagram of the present invention.
In the figure: the system comprises a 15% ethylene glycol monomethyl ether aqueous solution feeding pipeline 1, a falling film melting crystallizer distributor 2, a falling film melting crystallizer 3, a material circulating pump 4, a raffinate extraction pump 5, a water extraction pump 6, a crystallizer external heat exchanger 7, a crystallizer shell pass water circulating pump 8, a crystallizer residual liquid tank 9, a falling film melting crystallizer water tank 10, heat exchanger hot brine outlet water 11, heat exchanger cold brine inlet water 12, heat exchanger hot brine inlet water 13 and heat exchanger cold brine inlet water 14.
Detailed Description
The following detailed description of the preferred embodiments of the present invention, taken in conjunction with the accompanying drawings, will make the advantages and features of the invention more readily understood by those skilled in the art, and thus will more clearly and distinctly define the scope of the invention.
Referring to fig. 1, the present invention provides a technical solution: a device for separating glycol methyl ether and water by melt crystallization comprises a falling film melting crystallizer 3 and an external crystallizer heat exchanger 7, wherein the top of the external crystallizer heat exchanger 7 is connected with a heat exchanger hot brine water outlet pipeline 11 and a heat exchanger cold brine water inlet pipeline 12, the bottom of the external crystallizer heat exchanger 7 is connected with a heat exchanger hot brine water inlet pipeline 13 and a heat exchanger cold brine water inlet pipeline 14, the external crystallizer heat exchanger 7 is connected with a crystallizer shell pass water circulating pump 8, the top end inside the falling film melting crystallizer 3 is provided with a falling film melting crystallizer distributor 2, the top of the falling film melting crystallizer 3 is connected with a 15% glycol methyl ether aqueous solution feeding pipeline 1, the bottom of the falling film melting crystallizer 3 is respectively connected with a material circulating pump 4, a crystallizer residual liquid tank 9 and a falling film melting crystallizer water tank 10, the crystallizer residual liquid tank 9 is connected with a residual liquid extraction pump 5, the falling film melting crystallizer water tank 10 is connected with the water extraction pump 6.
The falling film melting crystallizer distributor 2 is connected with an external heat exchanger 7 of the crystallizer through a pipeline.
And the crystallizer shell pass water circulating pump 8 is respectively connected with the falling film melting crystallizer 3 and the external heat exchanger 7 of the crystallizer through pipelines.
The material circulating pump 4 is respectively connected with the top and the bottom of the falling film melting crystallizer 3 through pipelines.
The falling film melting crystallizer water tank 10 is respectively connected with the falling film melting crystallizer 3 and the water extraction pump 6 through pipelines.
The crystallizer residual liquid tank 9 is respectively connected with the falling film melting crystallizer 3 and the residual liquid extraction pump 5 through pipelines.
A method for separating ethylene glycol monomethyl ether from water by melt crystallization comprises the following steps:
s1, liquid-phase feeding: adding an aqueous solution containing 15% of ethylene glycol monomethyl ether at normal temperature into the falling film melt crystallizer 3 by using a feed pipeline; starting a material circulating pump 4 to circulate materials, and utilizing a falling film melting crystallizer distributor 2 to distribute films on the inner side of a crystallizer tube;
s2, cooling and crystallizing: starting a crystallizer shell pass water circulating pump 8, controlling the inlet and outlet flows of a heat exchanger cold brine water inlet pipeline 12 and a heat exchanger cold brine water inlet pipeline 14 at the same time, controlling the temperature of cold brine to be-10 ℃, and reducing the temperature of ethylene glycol monomethyl ether aqueous solution in the falling film melting crystallizer to be-5 ℃ by controlling the crystallization rate to be 0.02-0.3 ℃/min;
s3, heating and sweating: after 4-8 hours of crystallization, discharging residual liquid into a crystallizer residual liquid tank 9, slowly adding hot brine of a heat exchanger into cold brine to increase the temperature of the cold brine, controlling the temperature to be 0 ℃, increasing the temperature in the falling film melting crystallizer 3 to-2 ℃ at 0.05-0.5 ℃/min, controlling the flow of shell side brine to keep the temperature inside the falling film melting crystallizer 3 constant for 10-30min, obtaining the residual liquid and aqueous solution containing 40% moe of sweat, discharging the residual liquid and the sweat into a rectifying tower, and using after purification;
s4, stopping feeding of cold brine, heating hot brine in the external heat exchanger 7 of the crystallizer to melt the materials, melting water into liquid after the temperature is increased to 5-10 ℃ to obtain moe water solution with 99% of water, and discharging the water solution out of the sewage treatment system.
Example (b): a device for separating glycol methyl ether and water by melt crystallization and a method thereof comprise a 15% glycol methyl ether aqueous solution feed pipeline 1, a falling film melting crystallizer distributor 2, a falling film melting crystallizer 3, a material circulating pump 4, a raffinate extraction pump 5, a water extraction pump 6, a crystallizer external heat exchanger 7, a crystallizer shell pass water circulating pump 8, a crystallizer raffinate tank 9, a falling film melting crystallizer water tank 10, a heat exchanger hot brine water outlet pipeline 11, a heat exchanger cold brine water inlet pipeline 12, a heat exchanger hot brine water inlet pipeline 13 and a heat exchanger cold brine water inlet pipeline 14; at 1m3In a layer-type melt crystallizer of (1), 0.8m is charged3Cooling the 15 percent ethylene glycol monomethyl ether aqueous solution at a cooling rate of 0.1 ℃/min, wherein the cooling end point temperature is-5 ℃; after discharging the residual liquid, heating at the speed of 0.05 ℃/min to perform sweating, and keeping the temperature at-2 ℃ for 15min during sweating; after the discharged residual liquid and the generated sweat are treated in a rectifying tower, heating and melting; moe aqueous solution with 99 percent of water content is obtained and sent to a sewage treatment plant, and the once-through yield is 60 percent.
The above examples only show some embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention.
Claims (7)
1. The utility model provides a device of melt crystallization separation ethylene glycol methyl ether and water, includes falling film melt crystallizer (3) and crystallizer external heat exchanger (7), its characterized in that: the top of the external crystallizer heat exchanger (7) is connected with a heat exchanger hot brine water outlet pipeline (11) and a heat exchanger cold brine water inlet pipeline (12), the bottom of the external crystallizer heat exchanger (7) is connected with a heat exchanger hot brine water inlet pipeline (13) and a heat exchanger cold brine water inlet pipeline (14), the external crystallizer heat exchanger (7) is connected with a crystallizer shell pass water circulating pump (8), the top end of the interior of the falling film melting crystallizer (3) is provided with a falling film melting crystallizer distributor (2), the top of the falling film melting crystallizer (3) is connected with a 15% ethylene glycol monomethyl ether aqueous solution inlet pipeline (1), the bottom of the falling film melting crystallizer (3) is respectively connected with a material circulating pump (4), a crystallizer residual liquid tank (9) and a falling film melting crystallizer water tank (10), the crystallizer residual liquid tank (9) is connected with a residual liquid extraction pump (5), the falling film melting crystallizer water tank (10) is connected with a water extraction pump (6).
2. The apparatus for separating ethylene glycol methyl ether from water by melt crystallization according to claim 1, wherein: the falling film melting crystallizer distributor (2) is connected with an external heat exchanger (7) of the crystallizer through a pipeline.
3. The apparatus for separating ethylene glycol methyl ether from water by melt crystallization according to claim 1, wherein: and the crystallizer shell pass water circulating pump (8) is respectively connected with the falling film melting crystallizer (3) and the external heat exchanger (7) of the crystallizer through pipelines.
4. The apparatus for separating ethylene glycol methyl ether from water by melt crystallization according to claim 1, wherein: and the material circulating pump (4) is respectively connected with the top and the bottom of the falling film melting crystallizer (3) through pipelines.
5. The apparatus for separating ethylene glycol methyl ether from water by melt crystallization according to claim 1, wherein: the falling film melting crystallizer water tank (10) is respectively connected with the falling film melting crystallizer (3) and the water extraction pump (6) through pipelines.
6. The apparatus for separating ethylene glycol methyl ether from water by melt crystallization according to claim 1, wherein: the crystallizer residual liquid tank (9) is respectively connected with the falling film melting crystallizer (3) and a residual liquid extraction pump (5) through pipelines.
7. The method for separating ethylene glycol methyl ether from water by melt crystallization according to claim 1, wherein: the method comprises the following steps:
s1, liquid-phase feeding: adding an aqueous solution containing 15% of ethylene glycol methyl ether at normal temperature into the falling film melting crystallizer (3) by using a feed pipeline; starting a material circulating pump (4) for material circulation, and utilizing a falling film melting crystallizer distributor (2) to distribute films on the inner side of a crystallizer tube;
s2, cooling and crystallizing: starting a crystallizer shell pass water circulating pump (8), controlling the inlet and outlet flow rates of a heat exchanger cold brine water inlet pipeline (12) and a heat exchanger cold brine water inlet pipeline (14) at the same time, controlling the temperature of cold brine to be-10 ℃, and reducing the crystallization rate of the ethylene glycol monomethyl ether aqueous solution in the falling film melting crystallizer to be-5 ℃ by controlling the crystallization rate to be 0.02-0.3 ℃/min;
s3, heating and sweating: after 4-8 hours of crystallization, discharging residual liquid into a crystallizer residual liquid tank (9), slowly adding hot brine of a heat exchanger into cold brine to increase the temperature of the cold brine, controlling the temperature to be 0 ℃, increasing the temperature in the falling film melting crystallizer (3) to-2 ℃ at 0.05-0.5 ℃/min, controlling the flow of shell side brine to keep the temperature inside the falling film melting crystallizer (3) constant for 10-30min, obtaining residual liquid and aqueous solution containing 40% moe of sweat, discharging the residual liquid and the sweat into a rectifying tower, and purifying for use;
s4, stopping feeding of cold brine, feeding hot brine into an external heat exchanger (7) of the crystallizer to heat and melt the hot brine, heating the hot brine to 5-10 ℃, melting the hot brine into liquid to obtain moe aqueous solution with 99% of water, and discharging the aqueous solution out of the sewage treatment system.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115337662A (en) * | 2022-08-29 | 2022-11-15 | 烟台裕祥精细化工有限公司 | Equipment and method for purifying isophthaloyl dichloride through layered melt crystallization |
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Patent Citations (7)
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| JPH04306296A (en) * | 1991-04-04 | 1992-10-29 | Kao Corp | Production of liquid fatty acid and solid fatty acid |
| US20170349603A1 (en) * | 2014-12-23 | 2017-12-07 | Sk Innovation Co., Ltd. | Efficient Method for Producing and Purifying Anhydrous Sugar Alcohol |
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| CN115337662A (en) * | 2022-08-29 | 2022-11-15 | 烟台裕祥精细化工有限公司 | Equipment and method for purifying isophthaloyl dichloride through layered melt crystallization |
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