CN114797145A - Differential pressure thermal coupling rectification process for coal-to-ethylene glycol byproduct - Google Patents

Differential pressure thermal coupling rectification process for coal-to-ethylene glycol byproduct Download PDF

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CN114797145A
CN114797145A CN202210480247.2A CN202210480247A CN114797145A CN 114797145 A CN114797145 A CN 114797145A CN 202210480247 A CN202210480247 A CN 202210480247A CN 114797145 A CN114797145 A CN 114797145A
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tower
pressure
low
pipeline
reboiler
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CN114797145B (en
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陈学青
武涵
王�琦
张继军
姚红果
张超
李蓓
杨敬辉
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Hebei University of Technology
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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
    • B01D3/143Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
    • B01D3/146Multiple effect distillation
    • 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
    • B01D3/143Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
    • B01D3/148Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step in combination with at least one evaporator
    • 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
    • B01D3/32Other features of fractionating columns ; Constructional details of fractionating columns not provided for in groups B01D3/16 - B01D3/30
    • B01D3/322Reboiler specifications
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/74Separation; Purification; Use of additives, e.g. for stabilisation
    • C07C29/76Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
    • C07C29/80Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/10Process efficiency

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Abstract

The invention relates to a differential pressure thermal coupling rectification process for a coal-to-ethylene glycol byproduct. The process organically combines a light component removal tower, a high-pressure tower, a low-pressure tower, a light component removal tower thermal coupling reboiler (E1) and a low-pressure tower thermal coupling reboiler (E2), wherein one part of materials extracted from the top of the low-pressure tower returns to the high-pressure tower, one part of materials returns to the light component removal tower, and the discharged materials are not more than 1%. The ratio of the operating pressure of the high-pressure tower to the operating pressure of the low-pressure tower is generally not less than 10, the operating pressure of the high-pressure tower is not higher than 80kpa, the operating pressure of the low-pressure tower is not lower than 1kpa, and meanwhile, the azeotropic composition content change of the top of the high-pressure tower and the top of the low-pressure tower is ensured to be more than 5%, and the upper limit of system operation is not less than 120%. The invention realizes the separation and purification of the ethylene glycol and the 1, 2-butanediol in the coal-to-ethylene glycol byproduct; by using the differential pressure thermal coupling device, the secondary heat source can be fully utilized, the energy consumption is reduced, and the energy consumption can be reduced by about 30-35%.

Description

Differential pressure thermal coupling rectification process for coal-to-ethylene glycol byproduct
Technical Field
The invention relates to the field of chemical product rectification, in particular to a differential pressure thermal coupling rectification process for a coal-to-ethylene glycol byproduct.
Background
China has the resource characteristics of abundant coal resources and relatively lack of petroleum and natural gas, and the technology for preparing ethylene glycol from coal is widely popularized in China due to the advantages of low production cost, short flow and the like based on the development requirements of modern coal chemical industry.
At present, domestic enterprises only adopt reduced pressure rectification to extract part of ethylene glycol in the byproducts, when 1, 2-butanediol in the byproducts is increased to about 20 percent and the ethylene glycol is reduced to 60-70 percent, the ethylene glycol is not further processed and sold at a low value. More than 30-40 ten thousand tons of byproducts are generated every year, downstream manufacturers only further recover ethylene glycol or use the ethylene glycol as fuel after simple treatment, and qualified products of 1, 2-butanediol and ethylene glycol are not produced because the change rule of the ethylene glycol and the 1, 2-butanediol along with pressure is not mastered, differential pressure rectification is not adopted, reduced pressure rectification is only used, and the product purity is influenced because light components in the raw materials are not thoroughly removed. In 2017, the Shell company in the United states of America proposes a process for separating ethylene glycol and 1, 2-butanediol aiming at the mixture of ethylene glycol, 1, 2-butanediol and the like generated by hydrogenolysis of raw materials containing sugar or sugar alcohol, only can obtain ethylene glycol with higher purity, but cannot obtain a1, 2-butanediol product with high purity, and the material recovery rate is not high enough. The invention (US2017/0174596A1) only relates to a low-pressure tower and a high-pressure tower, and has large external discharge and low product yield; although the operation pressure of the high-pressure tower can be 50-150kpa, because the material has obvious heat sensitivity and is easy to generate side reactions such as polymerization and the like at high temperature, reduced pressure rectification is mostly adopted in actual production, namely the operation pressure is not more than 100 kpa.
Disclosure of Invention
The invention aims to provide a differential pressure thermal coupling rectification process for a coal-to-ethylene glycol byproduct, aiming at the defects in the prior art. The process is based on three tower flows of a light component removal tower, a high pressure tower and a low pressure tower, a light component removal tower thermal coupling reboiler (E1) and a low pressure tower thermal coupling reboiler (E2) are configured, a high temperature heat source and low temperature materials are utilized for heat exchange, and the low temperature materials are heated, so that the consumption of primary steam is reduced, the consumption of circulating water is reduced, the energy consumption is obviously reduced, and the operation cost is saved. The invention realizes the separation and purification of the ethylene glycol and the 1, 2-butanediol in the coal-to-ethylene glycol byproduct; by using the differential pressure thermal coupling device, the secondary heat source can be fully utilized, the energy consumption is reduced, and the energy consumption can be reduced by about 30-35%.
The invention is realized by adopting the following technical scheme:
a coal-to-ethylene glycol byproduct differential pressure thermal coupling rectification system comprises a lightness-removing column LPT1, a high pressure column HPT and a low pressure column LPT 2; the feed pump P1 is connected with the feed inlet of a light component removal tower LPT1 through a pipeline 1; the top steam outlet of the lightness-removing column LPT1 is connected with a top reflux tank V1 of the lightness-removing column through a condenser CX1, the outlet of the reflux tank V1 is connected with a reflux pump P2, and the outlet of the reflux pump P2 is respectively connected with the top of the extraction pipeline 3 and the top of the lightness-removing column LPT 1; the kettle of the light component removal tower LPT1 is respectively connected with a reboiler RB1, a light component removal tower thermal coupling reboiler E1 and a feed pump P3; the reboiler RB1 and the lightness-removing column thermal coupling reboiler E1 are respectively connected with the column bottom of a lightness-removing column LPT1, and the feed pump P3 is connected with the feed inlet of a high pressure column HPT;
the top of the high-pressure tower HPT is respectively connected with a condenser CX2 at the top of the high-pressure tower and a thermal coupling reboiler E2 at the low-pressure tower; the top condenser CX2 is connected with the high-pressure column reflux tank V2, and the condensate outlet of the low-pressure column thermal coupling reboiler E2 is connected with the high-pressure column reflux tank V2; a discharge port of the high-pressure tower reflux tank V2 is respectively connected with a top of a high-pressure tower HPT and a feed port of a low-pressure tower LPT2 through a high-pressure tower reflux pump P4; the outlet of the high-pressure tower HPT tower is divided into two parts, one part is connected with the bottom of the high-pressure tower HPT tower through a high-pressure tower reboiler RB2, and the other part is connected with an ethylene glycol product tank V3 through a high-pressure tower discharge pump P5, a thin film evaporator TFE1, a light component removal tower thermal coupling reboiler E1, an ethylene glycol product start condenser CX3 in sequence;
the top of the low-pressure tower LPT2 is sequentially connected with a low-pressure tower top condenser CX4, a low-pressure tower reflux tank V4 and a low-pressure tower reflux pump P6, an outlet of the low-pressure tower reflux pump P6 is connected with three pipelines, one pipeline is connected with the top of the low-pressure tower LPT2 through a pipeline 8, the second pipeline is connected with a light component extraction outlet through a pipeline 9, and the third pipeline is respectively connected with a high-pressure tower HPT feed inlet and a light component removal tower LPT1 feed inlet through a pipeline 10 and a pipeline 11; the tower kettle of the low-pressure tower LPT2 is connected with three pipelines, one pipeline is connected with the bottom of a low-pressure tower LPT2 through a low-pressure tower start reboiler RB3, the second pipeline is connected with the bottom of a low-pressure tower LPT2 through a low-pressure tower thermal coupling reboiler E2, and the third pipeline is connected with a1, 2-butanediol extraction outlet through a low-pressure tower discharge pump P7, a low-pressure tower thin-film evaporator TFE2, a1, 2-butanediol product condenser CX5, a1, 2-butanediol product tank V5 and a pipeline 12 in sequence;
the light component removal tower LPT1, the high pressure tower HPT and the low pressure tower LPT2 are all packed towers; the number of theoretical plates of the light component removal tower LPT1 is 40-60, and the feeding position is 30-40; the theoretical plate number of the high pressure column HPT is 70-90, and the feeding position is 53-68; theoretical plate number of low pressure column LPT2 is 50-75, feeding position is 35-41;
the reboilers RB1, RB2 and RB3 can be selected from a thermosyphon reboiler, a forced circulation reboiler, a falling film reboiler or a plate evaporator, and are preferably falling film reboilers;
the thermally coupled reboilers E1 and E2 are the same and may be selected from thermosyphon reboilers, forced circulation reboilers, falling film reboilers or plate evaporators, preferably falling film reboilers.
A coal-to-ethylene glycol byproduct differential pressure thermal coupling rectification process comprises the following steps:
the raw material enters a feed inlet of a lightness-removing column LPT1 through a pipeline 1 by a feed pump P1; the steam at the top of the light component removal tower LPT1 enters a reflux tank V1 at the top of the light component removal tower after being condensed by a condenser CX1, flows into a reflux pump P2 from the reflux tank V1, is divided into two parts at the pump outlet, one part is taken as a light component through a pipeline 3, and the other part flows back to the top of an LPT1 tower through a pipeline 2; one material at the tower bottom of the light component removal tower LPT1 flows back to the tower bottom after heat exchange through a light component removal tower reboiler RB1, one material flows back to the tower bottom after heat exchange through a light component removal tower thermal coupling reboiler E1, and the other material serving as a raw material of the high-pressure tower is fed into an HPT feed inlet of the high-pressure tower through a pipeline 4 through a feed pump P3;
the steam at the top of the high-pressure tower HPT enters a low-pressure tower thermal coupling reboiler E2, the condensate enters a reflux tank V2, then flows into a reflux pump P4 and then is divided into two parts, one part flows back to the top of the high-pressure tower HPT through a pipeline 5, and the other part flows into a feed inlet of a low-pressure tower LPT2 through a pipeline 6; the material at the tower bottom of the high pressure tower HPT flows out in two ways, one way is heated by a high pressure tower reboiler RB2 and then flows back to the tower bottom, the other way is used as an ethylene glycol product and is connected with a high pressure tower discharge pump P5, the ethylene glycol product is vaporized and decolored by a film evaporator TFE1 and then exchanges heat with the material at the bottom of the light component removal tower in a heat coupling reboiler E1 of the light component removal tower, the material flows into an ethylene glycol product tank V3 after passing through an ethylene glycol product start condenser CX3, and the ethylene glycol product is extracted from the ethylene glycol product tank V3 through a pipeline 7;
the steam at the top of the low-pressure tower LPT2 flows into a low-pressure tower reflux tank V4 through a low-pressure tower top condenser CX4, flows into a low-pressure tower reflux pump P6 through a reflux tank V4, flows out in three strands, one strand of the steam flows back to the top of the low-pressure tower LPT2 through a pipeline 8, one strand of the steam is taken out as a light component through a pipeline 9, and the third strand of the steam is taken as a raw material and flows back to a high-pressure tower HPT feed port and a light component removal tower LPT1 feed port through a pipeline 10 and a pipeline 11 respectively; one product at the bottom of the low-pressure tower LPT2 reflows to the bottom of a low-pressure tower LPT2 after heat exchange by a low-pressure tower thermal coupling reboiler E2, the other outflow 1, 2-butanediol product is connected with a low-pressure tower discharge pump P7, is vaporized and decolored by a low-pressure tower thin film evaporator TFE2, is condensed by a1, 2-butanediol product condenser CX5 and then flows into a1, 2-butanediol product tank V5, and finally, the product 1, 2-butanediol is extracted from the product tank V5 through a pipeline 12;
the pressure at the top of the light component removal tower LPT1 is 15-35Kpa, the temperature at the top of the tower is 130-158 ℃, and the reflux ratio at the top of the tower is 40-80: the temperature of the tower kettle is 140-165 ℃; the feeding temperature of the lightness-removing tower through a pipeline 1 is 25-30 ℃, and the feeding temperature of a pipeline 11 is 84-130 ℃;
the top pressure of the high pressure tower HPT is 40-80Kpa, the top temperature is 164-187 ℃, and the top reflux ratio is 4-7; the temperature of the tower kettle is 170-190 ℃; the feeding temperature of the high-pressure tower through a pipeline 4 is 140-165 ℃, and the feeding temperature of a pipeline 10 is 84-130 ℃;
the pressure at the top of the low-pressure tower LPT2 is 1-10Kpa, the temperature at the top of the tower is 84-130 ℃, and the reflux ratio at the top of the tower is 3-7; the temperature of the tower kettle is 90-135 ℃; the feeding temperature of the low-pressure tower is 164-187 ℃.
The flow ratio of the pipeline 9, the pipeline 10 and the pipeline 11 is 0.001:0.899:0.1-0.01:0.79:0.2
The tube side temperature of the reboiler RB1 is 140-165 ℃, the tube side temperature of the reboiler RB2 is 170-190 ℃, and the tube side temperature of the reboiler RB3 is 90-135 ℃; the shell side temperature of the thermal coupling reboiler E1 is 170-190 ℃, and the tube side temperature is 140-165 ℃; the shell pass temperature of the thermal coupling reboiler E2 is 164-187 ℃, and the tube pass temperature is 90-135 ℃;
the raw material liquid comprises, by mass, 65% -85% of ethylene glycol, 10% -30% of 1-2-butanediol, 0.1% -3% of other butanediol (2, 3-butanediol), 0.1% -1.5% of 1, 2-propanediol, 0.01% -0.1% of esters (gamma-butyrolactone, ethylene carbonate and the like), and a small amount of methyl glycolate and dimethyl oxalate.
The invention has the substantive characteristics that:
in the prior art, the method for separating the ethylene glycol and the 1, 2-butanediol by differential pressure is reported in documents, the invention gropes out the system rule that the azeotropic composition changes along with the pressure, adds a light component removal tower, a light component removal tower thermal coupling reboiler (E1) and a low pressure tower thermal coupling reboiler (E2), changes the operating pressure (40-80 kpa of a high pressure tower and 1-10kpa of a low pressure tower), and is different from the literature report (100 kpa of the high pressure tower and 30kpa of the low pressure tower).
The pure differential pressure rectification system is an operation system which is relatively independent from upstream to downstream before a thermal coupling reboiler is introduced, condensation and evaporation of materials in the system are coupled together after the thermal coupling reboiler is introduced, particularly, the system is operated under vacuum, if the heat exchange effect does not meet the design requirement or the flow resistance is too large, the system pressure is directly disturbed until the system stops, and the stability of the system operation pressure is directly influenced by the design selection and the operation elasticity of a pipeline and equipment resistance and the thermal coupling reboiler, so that a high-purity product cannot be obtained; the operation temperature is higher than 190 ℃, the polymerization reaction is obvious, and the byproducts are more; operating pressures below 1kpa can result in excessive vacuum system and equipment investment; the adjustment of the material circulation distribution proportion is also the key for stabilizing the material balance of the system and effectively removing impurities and ensuring the product purity, so the optimization and determination of the operation parameters are limited in many aspects.
The differential pressure thermal coupling rectification system designed by the invention organically combines a light component removal tower, a high-pressure tower, a low-pressure tower, a light component removal tower thermal coupling reboiler (E1) and a low-pressure tower thermal coupling reboiler (E2), wherein one part of materials extracted from the top of the low-pressure tower returns to the high-pressure tower, one part returns to the light component removal tower, and the discharged materials are not more than 1%. The ratio of the operating pressure of the high-pressure tower to the operating pressure of the low-pressure tower is generally not less than 10, the operating pressure of the high-pressure tower is not more than 80kpa, the operating pressure of the low-pressure tower is not less than 1kpa, meanwhile, the azeotropic composition content change of the top of the high-pressure tower and the top of the low-pressure tower is ensured to be more than 5%, the upper limit of system operation is not less than 120%, and qualified ethylene glycol and 1, 2-butanediol products can be obtained.
The invention has the beneficial effects that:
the invention has scientific and reasonable design, uses the steam at the top of the high-pressure tower as the heating medium of the material at the bottom of the low-pressure tower, provides heat for the material at the bottom of the low-pressure tower through the low-pressure tower thermal coupling reboiler E2, simultaneously uses the ethylene glycol product at the bottom of the high-pressure tower for vaporization and decoloration through the film evaporator, and can perform partial heat exchange with the material at the bottom of the light component removal tower LPT1 in the light component removal tower thermal coupling reboiler E1, thereby realizing thermal coupling rectification, and uses the technical means of differential pressure thermal coupling to reduce the use of circulating water, fully utilizes the secondary heat source, reduces the steam quantity, greatly reduces the production cost and energy consumption, and saves the energy consumption by 30-35%.
Drawings
FIG. 1 is a schematic diagram of a coal-to-ethylene glycol byproduct differential pressure thermal coupling rectification system;
in the figure, LPT 1: a light component removal tower; HPT: a high pressure column; LPT 2: low pressure column
P1: a light component removal tower feed pump; p2: a reflux pump of the light component removal tower; p3: a high pressure column feed pump; p4: a high pressure column reflux pump; p5: a high pressure column discharge pump; p6: a low pressure column reflux pump; p7: a low pressure column discharge pump; CX 1: a condenser at the top of the light component removal tower; CX 2: a condenser at the top of the high-pressure tower; CX 3: the ethylene glycol product is started up to be in a condenser; CX 4: a condenser at the top of the low-pressure tower; CX 5: a1, 2-butanediol product condenser; v1: a light component removal tower reflux tank; v2: a high pressure column reflux drum; v3: a glycol product tank; v4: a low pressure column reflux drum; v5: a1, 2-butanediol product tank; RB 1: a light component removal tower reboiler; RB 2: a high pressure column kettle reboiler; RB 3: a low-pressure tower start-up reboiler; TFE 1: a thin film evaporator; TFE 2: a thin film evaporator; e1: a light component removal column thermally coupled reboiler; e2 low pressure column thermally coupled reboiler; SW 1: a flow valve; SW 2: a flow valve;
Detailed Description
The invention will now be further described, by way of example, with reference to figure 1. The following examples are illustrative only and not intended to be limiting, and are not intended to limit the scope of the invention.
A differential pressure thermal coupling rectification system for a coal-to-ethylene glycol byproduct comprises a lightness-removing column LPT1, a high pressure column HPT and a low pressure column LPT2, wherein raw materials enter a feed inlet of a lightness-removing column LPT1 through a pipeline 1 by a feed pump P1; the top steam outlet of the light component removal tower LPT1 is connected with a top reflux tank V1 of the light component removal tower through a condenser CX1, the outlet of the reflux tank V1 is connected with a reflux pump P2, and the outlet of the reflux pump P2 is respectively connected with the extraction pipeline 3 and the top of the light component removal tower LPT 1; the kettle of the light component removal tower LPT1 is respectively connected with a reboiler RB1, a heat coupling reboiler E1 of the light component removal tower and a feed pump P3; the reboiler RB1 and the lightness-removing column thermal coupling reboiler E1 are respectively connected with the column bottom of a lightness-removing column LPT1, and the feed pump P3 is connected with the feed inlet of a high pressure column HPT;
the top of the high-pressure tower HPT is respectively connected with a condenser CX2 (through a valve SW1) at the top of the high-pressure tower and a thermal coupling reboiler E2 (through a valve SW2) at the low-pressure tower; the top condenser CX2 is connected with the high-pressure tower reflux tank V2, and the condensate outlet of the low-pressure tower thermal coupling reboiler E2 is connected with the high-pressure tower reflux tank V2; the discharge port of the high-pressure tower reflux tank V2 is respectively connected with the feed ports of the top of the high-pressure tower HPT (through a pipeline 5) and the low-pressure tower LPT2 (through a pipeline 6) through a high-pressure tower reflux pump P4; the outlet of the tower bottom of the high-pressure tower HPT is divided into two parts, one part is connected with the bottom of the high-pressure tower HPT through a high-pressure tower reboiler RB2, and the other part is connected with an ethylene glycol product tank V3 through a high-pressure tower discharge pump P5, a thin film evaporator TFE1, a light component removal tower thermal coupling reboiler E1, an ethylene glycol product start condenser CX3 in sequence;
the top of the low-pressure tower LPT2 is sequentially connected with a low-pressure tower top condenser CX4, a low-pressure tower reflux tank V4 and a low-pressure tower reflux pump P6, an outlet of the low-pressure tower reflux pump P6 is connected with three pipelines, one pipeline is connected with the top of the low-pressure tower LPT2 through a pipeline 8, the second pipeline is connected with a light component extraction outlet through a pipeline 9, and the third pipeline is respectively connected with a high-pressure tower HPT feed inlet and a light component removal tower LPT1 feed inlet through a pipeline 10 and a pipeline 11; the tower kettle of the low-pressure tower LPT2 is connected with three pipelines, one pipeline is connected with the bottom of a low-pressure tower LPT2 through a low-pressure tower start reboiler RB3, the second pipeline is connected with the bottom of a low-pressure tower LPT2 through a low-pressure tower thermal coupling reboiler E2, and the third pipeline is connected with a1, 2-butanediol extraction outlet through a low-pressure tower discharge pump P7, a low-pressure tower thin-film evaporator TFE2, a1, 2-butanediol product condenser CX5, a1, 2-butanediol product tank V5 and a pipeline 12 in sequence;
the light component removal tower LPT1, the high pressure tower HPT and the low pressure tower LPT2 are all packed towers; the number of theoretical plates of the light component removal tower LPT1 is 40-60, and the feeding position is 30-40; the theoretical plate number of the high pressure column HPT is 70-90, and the feeding position is 53-68; theoretical plate number of low pressure column LPT2 is 50-75, feeding position is 35-41;
the reboilers RB1, RB2 and RB3 can be selected from a thermosyphon reboiler, a forced circulation reboiler, a falling film reboiler or a plate evaporator, and are preferably falling film reboilers;
the thermally coupled reboilers E1 and E2 are identical and can be selected from thermosyphon reboilers, forced circulation reboilers, falling film reboilers or plate evaporators, preferably falling film reboilers.
A coal-to-ethylene glycol byproduct differential pressure thermal coupling rectification process comprises the following steps:
the raw material enters a feed inlet of a lightness-removing column LPT1 through a feed pump P1 and a pipeline 1; the steam at the top of the light component removal tower LPT1 enters a reflux tank V1 at the top of the light component removal tower after being condensed by a condenser CX1, flows into a reflux pump P2 from the reflux tank V1, is divided into two parts at the pump outlet, one part is taken as a light component through a pipeline 3, and the other part flows back to the top of an LPT1 tower through a pipeline 2; the material at the tower bottom of the light component removal tower LPT1 flows out in three strands, one strand flows into a reboiler RB1 for heating at the initial start-up stage and then flows back to the tower bottom of the light component removal tower LPT1, the other strand flows back to the tower bottom after heat exchange through a heat coupling reboiler E1 of the light component removal tower after the start-up is stable, and the other strand is used as a raw material and is sent into a feeding hole of the high pressure tower HPT through a pipeline 4 by a feeding pump P3;
the pressure at the top of the light component removal tower LPT1 is 15-35Kpa, the temperature at the top of the tower is 130-158 ℃, and the reflux ratio at the top of the tower is 40-80: the temperature of the tower kettle is 140-165 ℃; the feeding temperature of the light component removing tower through a pipeline 1 is 25-30 ℃, the feeding temperature of a pipeline 11 is 84-130 ℃, and the discharging temperature at the top of the tower is 130-158 ℃; the discharging temperature of the tower kettle is 140-165 ℃;
the top pressure of the high pressure tower HPT is 40-80Kpa, the top temperature is 164-187 ℃, and the top reflux ratio is 4-7; the temperature of the tower kettle is 170-190 ℃; the feeding temperature of the high-pressure tower through a pipeline 4 is 140-165 ℃, the feeding temperature of a pipeline 10 is 84-130 ℃, and the discharging temperature at the top of the tower is 164-187 ℃; the discharging temperature of the tower kettle is 170-190 ℃;
the pressure at the top of the low-pressure tower LPT2 is 1-10Kpa, the temperature at the top of the tower is 84-130 ℃, and the reflux ratio at the top of the tower is 3-7; the temperature of the tower kettle is 90-135 ℃; the feeding temperature of the low-pressure tower is 164-187 ℃, the discharging temperature of the top of the tower is 84-130 ℃, and the discharging temperature of the bottom of the tower is 90-135 ℃.
The ratio of the pipelines 9, 10 and 11 is 0.001:0.899:0.1-0.01:0.79: 0.2;
the tube side temperature of the reboiler RB1 is 140-165 ℃, the tube side temperature of the reboiler RB2 is 170-190 ℃, and the tube side temperature of the reboiler RB3 is 90-135 ℃; the shell side temperature of the thermal coupling reboiler E1 is 170-190 ℃, and the tube side temperature is 140-165 ℃; the shell pass temperature of the thermal coupling reboiler E2 is 164-187 ℃, and the tube pass temperature is 90-135 ℃;
the high pressure tower HPT opens a valve SW1 at the initial start-up stage, SW2 is kept closed, the steam at the top of the high pressure tower flows into a high pressure tower reflux tank V2 through a high pressure tower top condenser CX2 at the initial start-up stage, flows into a high pressure tower reflux pump P4 from a reflux tank V2 and refluxes to the top of the high pressure tower HPT through a pipeline 5; after the start-up is stable, opening SW2, gradually closing SW1 to control the flow rate to be 1% -20%, allowing the steam at the top of the high-pressure tower to enter a low-pressure tower thermal coupling reboiler E2, allowing the condensate to enter a reflux tank V2, then flowing into a reflux pump P4, dividing into two parts, wherein one part flows back to the top of the high-pressure tower HPT through a pipeline 5, and the other part flows into a low-pressure tower LPT2 feeding hole through a pipeline 6; the material at the tower bottom of the high pressure tower HPT flows out in two ways, one way is heated by a high pressure tower reboiler RB2 and then flows back to the tower bottom, the other way is used as an ethylene glycol product and is connected with a high pressure tower discharge pump P5, the ethylene glycol product is vaporized and decolored by a film evaporator TFE1 and then exchanges heat with the material at the tower bottom of the light component removal tower in a light component removal tower thermal coupling reboiler E1, the material flows into an ethylene glycol product tank V3 after passing through an ethylene glycol product start condenser CX3, and the ethylene glycol product is extracted from the ethylene glycol product tank V3 through a pipeline 7;
the steam at the top of the low-pressure tower LPT2 flows into a low-pressure tower reflux tank V4 through a low-pressure tower top condenser CX4, flows into a low-pressure tower reflux pump P6 through a reflux tank V4, flows out in three strands, one strand of the steam flows back to the top of the low-pressure tower LPT2 through a pipeline 8, one strand of the steam is taken out as a light component through a pipeline 9, and the third strand of the steam is taken as a raw material and flows back to a high-pressure tower HPT feed port and a light component removal tower LPT1 feed port through a pipeline 10 and a pipeline 11 respectively; the product at the tower bottom of the low-pressure tower LPT2 flows out in three strands, one strand flows back to the bottom of the low-pressure tower LPT2 through a low-pressure tower start reboiler RB3 at the initial start-up stage, the other strand flows through a low-pressure tower thermal coupling reboiler E2 for heat exchange and then flows back to the bottom of the low-pressure tower LPT2 after stable start-up, the 1, 2-butanediol product flowing out in the third strand flows into a1, 2-butanediol product tank V5 after being connected with a low-pressure tower discharge pump P7 and vaporized and decolored through a low-pressure tower film evaporator TFE2 and then condensed through a1, 2-butanediol product condenser CX5, and finally the product 1, 2-butanediol is collected through a pipeline 12 from the product tank V5.
The light component is extracted through a pipeline 3, and the extracted matter is (part of ethylene glycol, 1, 2-butanediol, 2, 3-butanediol, 1, 2-propanediol, ethylene carbonate, gamma-butyrolactone, methyl glycolate and dimethyl oxalate for preparing antifreeze and alcohol-based fuel)
The light component is extracted by a pipeline 9 and is (part of ethylene glycol, 1, 2-butanediol, 2, 3-butanediol, 1, 2-propanediol, gamma-butyrolactone, methyl glycolate and dimethyl oxalate)
The initial start-up stage is that the whole device is just started, the operating temperature, the operating pressure, the public work consumption, the product purity and the like do not meet the design requirements, and the conditions of fluctuation or over-high or over-low exist; the stable operation is that the operation temperature, the operation pressure, the public engineering consumption, the product purity and the like reach the design requirements and reach a stable value; both state concepts are common general knowledge.
Example 1
The example of treating a coal-to-ethylene glycol byproduct feed solution of 3.6 tons per hour is described.
The raw material liquid includes (ethylene glycol 82%, 1-2 butanediol 17.6%, other butanediol (2, 3-butanediol) 0.2%, 1, 2-propanediol 0.1%, esters (gamma-butyrolactone, ethylene carbonate, etc.) 0.08%, a small amount of methyl glycolate and dimethyl oxalate).
A coal-to-ethylene glycol byproduct differential pressure thermal coupling rectification system is shown in figure 1, the temperature of a coal-to-ethylene glycol byproduct raw material liquid from a reaction tank area is 25 ℃, the pressure is increased to 300KPa through a light component removal tower feed pump P1, the raw material liquid is sent to a light component removal tower LPT1, the number of tower plates of the light component removal tower is 48, the feed position is 35, the operating pressure is 15KPa, the temperature at the top of the tower is 136 ℃, the temperature at the bottom of the tower is 144 ℃, the reflux ratio at the top of the tower is 60, the material entering the light component removal tower is heated through a reboiler, and the liquid at the bottom of the tower which meets the separation requirement flows into a high pressure tower HPT through a feed pump P3 as the raw material; after the start-up is stable, the material in the tower bottom of the light component removal tower LPT1 can exchange heat with the ethylene glycol product from the high-pressure tower HPT through vaporization and decoloration at the ethylene glycol product condenser. The number of HPT plates of the high-pressure tower is 70, the feeding position is 53, the feeding temperature is 144 ℃, the feeding pressure is 300Kpa, the temperature at the top of the tower is 172 ℃, the reflux ratio at the top of the tower is 4.8, the temperature at the bottom of the tower is 176.5 ℃, the operating pressure of the HPT of the high-pressure tower is 50Kpa, the mass fraction of ethylene glycol in the azeotropic composition of ethylene glycol and 1, 2-butanediol at the top of the tower is 40.6 percent, the steam at the top of the HPT of the high-pressure tower is condensed by a condenser CX2 at the top of the high-pressure tower at the initial stage of starting, then is sent back to the top of the high-pressure tower after passing through a reflux tank V2 of the high-pressure tower, after the start is stable, the flow of SW1 is reduced to 17%, the flow of SW2 is opened to 83%, the steam at the top of the high-pressure tower flows into a reflux tank V2 after exchanging heat with the materials at the bottom of the low-pressure tower LPT2 through a low-pressure tower thermal coupling reboiler E2, then flows into a reflux tank V2 after being divided into two parts through a high-pressure tower reflux pump P4, one part flows back to the top of the high-pressure tower HPT, and the other part flows into the low-pressure tower LPT2 as a raw material; the materials in the tower bottom of the high-pressure tower are heated by a reboiler RB2 of the high-pressure tower, the ethylene glycol product meeting the separation requirement is vaporized and decolored by a thin film evaporator TFE1 and then exchanges heat with the materials in the tower bottom of a light component removal tower LPT1 in a heat coupling reboiler E1 of the light component removal tower, the ethylene glycol product is condensed by a condenser CX3 of the start of the ethylene glycol product and then flows into an ethylene glycol product tank V3, the ethylene glycol product is extracted by a pipeline 7, the flow rate is 2.92t/h, and the purity is more than 99%. The tower number of the low-pressure tower LPT2 is 60, the feeding position is 35, the feeding temperature is 172 ℃, the feeding pressure is 300Kpa, the tower top temperature is 114 ℃, the tower kettle temperature is 124 ℃, the operating pressure of the low-pressure tower LPT2 is 5Kpa, the tower top reflux ratio is 4, the mass fraction of ethylene glycol in the azeotropic composition of the ethylene glycol and 1, 2-butanediol at the tower top is 46.2%, and the material at the bottom of the low-pressure tower LPT2 and the steam at the top of the high-pressure tower HPT can exchange heat at a low-pressure tower thermal coupling reboiler E2 and then flow back to the bottom of the low-pressure tower; the steam at the top of the low-pressure tower LPT2 is condensed by a condenser at the top of the low-pressure tower and then flows back to a reflux tank V4 of the low-pressure tower, one part of the product in the reflux tank V4 flows into a light component removal tower LPT1 and a high-pressure tower HPT as raw materials through a reflux pump P6 of the low-pressure tower at the temperature of 114 ℃ and the pressure of 300Kpa, one part of the product flows back to the top of the low-pressure tower, the other part of the product flows out as light components, and the flow ratio of pipelines 9, 10 and 11 is 0.001:0.899: 0.1. The materials in the tower bottom of the low-pressure tower are heated by a low-pressure tower start reboiler RB3 at the start-up initial stage, after the start-up is stable, the 1, 2-butanediol product meeting the separation requirement flows into a thin film evaporator TFE2 through a low-pressure tower discharge pump P7 to be vaporized, decolored and condensed to obtain the 1, 2-butanediol product, the flow is 0.44t/h, and the purity is more than 98%. (qualified products can be obtained when the feeding amount fluctuates to 4.2t/h when the device is in stable operation)
In the above example, the operating pressure difference of the high-pressure tower and the low-pressure tower is set, so that the steam at the top of the high-pressure tower HPT exchanges heat with the tower kettle material of the low-pressure tower LPT2, and the steam at the top of the high-pressure tower is liquefied to release heat, which completely meets the heat demand of the tower kettle material of the low-pressure tower; meanwhile, the ethylene glycol product extracted from the tower bottom of the high-pressure tower HPT exchanges heat with the material in the tower bottom of the lightness-removing tower LPT1 after vaporization and decoloration, and the ethylene glycol product after vaporization and decoloration can provide part of heat for the material in the tower bottom of the lightness-removing tower LPT 1.
Example 2
The other steps are the same as example 1, except that the feeding amount is changed from 3.6t/h to 4.2t/h, the operating pressure of the light component removal tower is changed from 15Kpa to 35Kpa, the temperature at the top of the tower is changed from 136 ℃ to 158 ℃, the temperature at the bottom of the tower is changed from 144 ℃ to 165 ℃, the number of trays is changed from 48 to 55, and the feeding position is changed from 35 to 42; the operating pressure of the high-pressure tower is changed from 50Kpa to 80Kpa, the temperature of the top of the tower is changed from 172 ℃ to 187 ℃, the temperature of the bottom of the tower is changed from 176.5 ℃ to 190 ℃, the number of plates is changed from 70 to 82, the feeding position is changed from 53 to 66, the reflux ratio is changed from 4.8 to 4.2, 3.4t/h of glycol is extracted from the bottom of the tower, and the purity is more than 99 percent; the operating pressure of the low-pressure tower is changed from 5Kpa to 3Kpa, the temperature of the top of the tower is changed from 114 ℃ to 104 ℃, the reflux ratio is changed from 4 to 3.25, the number of the tower plates is changed from 60 to 61, the feeding position is changed from 35 to 39, the temperature of the bottom of the tower is changed from 124 ℃ to 117 ℃, 1, 2-butanediol is extracted from the bottom of the tower at 0.52t/h, and the purity is more than 98%; the energy is saved by 35 percent.
Comparative example 1
And (3) treating 3.6 tons of coal-to-ethylene glycol byproduct feed solution every hour, and regulating the pressure in the tower by using a common differential pressure rectification device (such as energy consumption, circulating water consumption and the like in the differential rectification device document (US2017/0174596A1) and in comparative example 1, the data are obtained by analog calculation without thermal coupling under the same material treatment capacity), so that a qualified ethylene glycol product is obtained by the reflux ratio.
The hot stream energy consumed in comparative example 1 was 12084KW, whereas the hot stream energy consumed in example 1 was 8040KW, an overall saving of energy consumption of about 33.4% was achieved in example 1 compared to the comparative example 1 apparatus. Meanwhile, the consumption of the circulating water is also obviously reduced, the consumption of the circulating water in example 1 is 819t/h, the consumption of the circulating water in comparative example 1 is 1330.6t/h, and the consumption of the circulating water in example 1 is reduced by 510.8t/h compared with that in comparative example 1.
The invention is not the best known technology.

Claims (6)

1. A coal-to-ethylene glycol byproduct differential pressure thermal coupling rectification process is characterized by comprising the following steps:
in a differential pressure thermal coupling rectification system for preparing the ethylene glycol by-product from coal, raw materials enter a feed inlet of a lightness-removing column LPT1 through a feed pump P1 and a pipeline 1; the steam at the top of the light component removal tower LPT1 enters a reflux tank V1 at the top of the light component removal tower after being condensed by a condenser CX1, flows into a reflux pump P2 from the reflux tank V1, is divided into two parts at the outlet of the pump, one part is taken as a light component through a pipeline 3, and the other part flows back to the top of the light component removal tower LPT1 through a pipeline 2; one material at the tower bottom of the light component removal tower LPT1 flows back to the tower bottom after heat exchange through a light component removal tower reboiler RB1, one material flows back to the tower bottom after heat exchange through a light component removal tower thermal coupling reboiler E1, and the other material serving as a raw material of the high-pressure tower is fed into an HPT feed inlet of the high-pressure tower through a pipeline 4 through a feed pump P3;
the steam at the top of the high-pressure tower HPT enters a low-pressure tower thermal coupling reboiler E2, the condensate enters a reflux tank V2, then flows into a reflux pump P4 and then is divided into two parts, one part flows back to the top of the high-pressure tower HPT through a pipeline 5, and the other part flows into a feed inlet of a low-pressure tower LPT2 through a pipeline 6; the material at the tower bottom of the high pressure tower HPT flows out in two ways, one way is heated by a high pressure tower reboiler RB2 and then flows back to the tower bottom, the other way is used as an ethylene glycol product and is connected with a high pressure tower discharge pump P5, the ethylene glycol product is vaporized and decolored by a film evaporator TFE1 and then exchanges heat with the material at the bottom of the light component removal tower in a heat coupling reboiler E1 of the light component removal tower, the material flows into an ethylene glycol product tank V3 after passing through an ethylene glycol product start condenser CX3, and the ethylene glycol product is extracted from the ethylene glycol product tank V3 through a pipeline 7;
the steam at the top of the low-pressure tower LPT2 flows into a low-pressure tower reflux tank V4 through a low-pressure tower top condenser CX4, flows into a low-pressure tower reflux pump P6 through a reflux tank V4 and flows out in three strands, one strand of the steam flows back to the top of the low-pressure tower LPT2 through a pipeline 8, the other strand of the steam is taken out as a light component through a pipeline 9, and the third strand of the steam is taken as a raw material and flows back to a high-pressure tower HPT feed port and a light component removal tower LPT1 feed port through a pipeline 10 and a pipeline 11 respectively; one stream of products at the tower bottom of the low-pressure tower LPT2 flows back to the tower bottom of the low-pressure tower LPT2 after heat exchange by a low-pressure tower thermal coupling reboiler E2, the other stream of the flowing 1, 2-butanediol products is connected with a low-pressure tower discharge pump P7, is vaporized and decolored by a low-pressure tower film evaporator TFE2, is condensed by a1, 2-butanediol product condenser CX5 and then flows into a1, 2-butanediol product tank V5, and finally the product 1, 2-butanediol is extracted from the product tank V5 through a pipeline 12;
the pressure at the top of the light component removal tower LPT1 is 15-35Kpa, the temperature at the top of the tower is 130-158 ℃, and the reflux ratio at the top of the tower is 40-80: the temperature of the tower kettle is 140-165 ℃; the feeding temperature of the light component removal tower LPT1 through a pipeline 1 is 25-30 ℃, the feeding temperature of a pipeline 11 is 84-130 ℃, and the discharging temperature at the top of the tower is 130-145 ℃;
the top pressure of the high pressure tower HPT is 40-80Kpa, the top temperature is 164-187 ℃, and the top reflux ratio is 4-7; the temperature of the tower kettle is 170-190 ℃; the feeding temperature of the high-pressure tower through a pipeline 4 is 140-165 ℃, the feeding temperature of a pipeline 10 is 84-130 ℃, and the discharging temperature at the top of the tower is 164-187 ℃;
the pressure at the top of the low-pressure tower LPT2 is 1-10Kpa, the temperature at the top of the tower is 84-130 ℃, and the reflux ratio at the top of the tower is 3-7; the temperature of the tower kettle is 90-135 ℃; the feeding temperature of the low-pressure tower is 164-187 ℃, and the discharging temperature at the top of the tower is 84-130 ℃;
the tube side temperature of the reboiler RB1 is 140-165 ℃, the tube side temperature of the reboiler RB2 is 170-190 ℃, and the tube side temperature of the reboiler RB3 is 90-135 ℃; the shell side temperature of the thermal coupling reboiler E1 is 170-190 ℃, and the tube side temperature is 140-165 ℃; the shell side temperature of the thermal coupling reboiler E2 is 164-187 ℃, and the tube side temperature is 90-135 ℃.
2. The differential pressure thermal coupling rectification process for the coal-to-ethylene glycol byproduct as claimed in claim 1, wherein the raw material liquid comprises, by mass, 65% -85% of ethylene glycol, 10% -30% of 1-2 butanediol, 0.1% -3% of other butanediol (2, 3-butanediol), 0.1% -1.5% of 1, 2-propanediol, and 0.01% -0.1% of esters (gamma-butyrolactone and ethylene carbonate).
3. The differential pressure thermal coupling rectification process of coal-to-ethylene glycol byproduct as claimed in claim 1, wherein the flow ratio of the pipeline 9, the pipeline 10 and the pipeline 11 is 0.001:0.899:0.1-0.01:0.79: 0.2.
4. The differential pressure thermal coupling rectification process of the coal-made ethylene glycol byproduct as claimed in claim 1, wherein the differential pressure thermal coupling rectification system of the coal-made ethylene glycol byproduct comprises a lightness-removing column LPT1, a high pressure column HPT and a low pressure column LPT 2; the feed pump P1 is connected with the feed inlet of the lightness-removing column LPT1 through a pipeline 1; the top steam outlet of the light component removal tower LPT1 is connected with a top reflux tank V1 of the light component removal tower through a condenser CX1, the outlet of the reflux tank V1 is connected with a reflux pump P2, and the outlet of the reflux pump P2 is respectively connected with the top of the light component removal tower LPT1 and the extraction pipeline 3; the kettle of the light component removal tower LPT1 is respectively connected with a reboiler RB1, a heat coupling reboiler E1 of the light component removal tower and a feed pump P3; the reboiler RB1 and the lightness-removing column thermal coupling reboiler E1 are respectively connected with the column bottom of a lightness-removing column LPT1, and the feed pump P3 is connected with the feed inlet of a high pressure column HPT;
the top of the high-pressure tower HPT is respectively connected with a condenser CX2 at the top of the high-pressure tower and a thermal coupling reboiler E2 at the low-pressure tower; the top condenser CX2 is connected with the high-pressure column reflux tank V2, and the condensate outlet of the low-pressure column thermal coupling reboiler E2 is connected with the high-pressure column reflux tank V2; a discharge port of the high-pressure tower reflux tank V2 is respectively connected with a top of a high-pressure tower HPT and a feed port of a low-pressure tower LPT2 through a high-pressure tower reflux pump P4; the outlet of the high-pressure tower HPT tower is divided into two parts, one part is connected with the bottom of the high-pressure tower HPT tower through a high-pressure tower reboiler RB2, and the other part is connected with an ethylene glycol product tank V3 through a high-pressure tower discharge pump P5, a thin film evaporator TFE1, a light component removal tower thermal coupling reboiler E1, an ethylene glycol product start condenser CX3 in sequence;
the top of the low-pressure tower LPT2 is sequentially connected with a low-pressure tower top condenser CX4, a low-pressure tower reflux tank V4 and a low-pressure tower reflux pump P6, an outlet of the low-pressure tower reflux pump P6 is connected with three pipelines, one pipeline is connected with the top of the low-pressure tower LPT2 through a pipeline 8, the second pipeline is connected with a light component extraction outlet through a pipeline 9, and the third pipeline is respectively connected with a high-pressure tower HPT feed inlet and a light component removal tower LPT1 feed inlet through a pipeline 10 and a pipeline 11; the tower kettle of the low-pressure tower LPT2 is connected with three pipelines, one pipeline is connected with the bottom of a low-pressure tower LPT2 through a low-pressure tower start reboiler RB3, the second pipeline is connected with the bottom of a low-pressure tower LPT2 through a low-pressure tower thermal coupling reboiler E2, and the third pipeline is connected with a1, 2-butanediol extraction outlet through a low-pressure tower discharge pump P7, a low-pressure tower film evaporator TFE2, a1, 2-butanediol product condenser CX5, a1, 2-butanediol product tank V5 and a pipeline 12 in sequence.
5. The differential pressure thermal coupling rectification process of a coal-to-ethylene glycol byproduct as claimed in claim 4, wherein the light component removal column LPT1, the high pressure column HPT and the low pressure column LPT2 are all packed columns; the number of theoretical plates of the light component removal tower LPT1 is 40-60, and the feeding position is 30-40; the theoretical plate number of the high pressure column HPT is 70-90, and the feeding position is 53-68; the theoretical plate number of the low-pressure column LPT2 is 50 to 75, and the feed position is 35 to 41.
6. The differential pressure thermal coupling rectification process of the coal-to-ethylene glycol byproduct as claimed in claim 4, wherein the reboiler RB1, the reboiler RB2 and the reboiler RB3 are thermosiphon reboilers, forced circulation reboilers, falling film reboilers or plate evaporators;
the thermally coupled reboiler E1 is the same as the thermally coupled reboiler E2 and is a thermosiphon reboiler, a forced circulation reboiler, a falling film reboiler or a plate evaporator.
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