CN214105872U - Process unit for separating ethylene glycol and 1, 2-butanediol by azeotropic distillation - Google Patents
Process unit for separating ethylene glycol and 1, 2-butanediol by azeotropic distillation Download PDFInfo
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- CN214105872U CN214105872U CN202022913310.6U CN202022913310U CN214105872U CN 214105872 U CN214105872 U CN 214105872U CN 202022913310 U CN202022913310 U CN 202022913310U CN 214105872 U CN214105872 U CN 214105872U
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Abstract
The utility model relates to a process unit for separating glycol and 1, 2-butanediol by azeotropic distillation, which comprises a glycol refining tower, an entrainer recovery tower and a butanediol removing tower, wherein a tower kettle discharge port of the glycol refining tower is connected with a glycol product tank; the device comprises an ethylene glycol refining tower, an entrainer recovery tower, an entrainer reflux pump, a butanediol removal tower condenser, a butanediol removal tower reflux tank and a butanediol removal tower reflux pump, wherein a tower top discharge port of the ethylene glycol refining tower is connected to a feed inlet of the entrainer recovery tower, a tower top outlet of the entrainer recovery tower is connected to a shell pass inlet of the entrainer recovery tower condenser through a pipeline, a shell pass outlet of the entrainer recovery tower condenser is connected to the entrainer recovery tower reflux pump, the entrainer recovery tower reflux pump is connected to a feed inlet of the butanediol removal tower, a tower bottom discharge port of the butanediol removal tower is connected to the butanediol removal tower condenser, the butanediol removal tower reflux tank and the butanediol removal tower reflux pump, the butanediol removal tower reflux pump is connected to a feed inlet of the entrainer recovery tower, and a tower bottom discharge port of the butanediol removal tower is connected to a 1, 2-butanediol product tank. The utility model has the characteristics of low energy consumption, high purity of the obtained glycol and 1, 2-butanediol and high yield.
Description
Technical Field
The utility model relates to a chemical industry separation technical field, concretely relates to device of azeotropic distillation separation ethylene glycol and 1, 2-butanediol, especially the device of the crude ethylene glycol separation refined ethylene glycol and 1, 2-butanediol in the coal system ethylene glycol route.
Background
Ethylene glycol is used as an important chemical raw material, is mainly used for producing polyester terylene, polyester resin, a plasticizer, a surfactant, synthetic fibers and the like, can also be used as a solvent, a cooling liquid and the like of dye and printing ink, and has become the largest ethylene glycol consuming country in the world in China. In order to reduce the dependence on petroleum resources, the coal-to-ethylene glycol route is more and more emphasized, and has important practical significance for China.
In the dimethyl oxalate process route for preparing ethylene glycol from coal, the boiling points of ethylene glycol and a byproduct 1, 2-butanediol are relatively close and have a difference of 4.5 ℃, and the ethylene glycol and the byproduct 1, 2-butanediol can form a low-point azeotrope, and the two are difficult to separate completely by adopting a common rectification technology.
The conventional methods comprise pressure swing distillation, extractive distillation, reactive distillation, selective adsorption, azeotropic distillation and the like. In the pressure swing distillation separation method, Huizenga and Sanders realize the separation of ethylene glycol and 1, 2-butanediol, 99.6 percent of ethylene glycol is obtained from a high-pressure tower kettle, 1, 2-butanediol cannot be effectively separated from a low-pressure tower kettle, and the composition of an azeotrope of the ethylene glycol and the 1, 2-butanediol is small along with the pressure change, so that the circulation volume is large, the operation load of the tower is increased, and the practical application is not facilitated. For the extractive distillation separation method, the poplars have high boiling points as the ethylene glycol and the 1, 2-butanediol are indicated, the selection of a third polar solvent with a higher boiling point is difficult, and in addition, the recovery energy consumption of the subsequent third component solvent is high, so that the process technology loses advantages. For the reactive distillation separation method, Gaoxin et al propose a reactive distillation process for separating ethylene glycol and 1, 2-butanediol by using acetone, Choptade and Sharma propose that dihydric alcohols such as ethylene glycol are converted into acetal compounds with high boiling point difference by using an aldol condensation reaction so as to reduce the separation difficulty, but the two main problems of reactive distillation are too long process flow and too much water consumption of hydrolysis reaction. For selective adsorption, ethylene glycol and 1, 2-butanediol solution are purified by MF1 zeolite adsorption bed, the purity of ethylene glycol can reach 99.8%, but the problems of short service life of adsorbent, large regeneration difficulty, small production capacity and the like restrict industrialization.
As for the azeotropic distillation separation method, the great wealth and the Zhengmingyuan and the like indicate that the relative volatility between the diols can be obviously improved by adopting the azeotropic distillation, so that the number of theoretical plates is reduced, the fixed cost of a distillation tower is reduced, most of the entrainers discovered at present form an azeotrope with a main product, namely the glycol, and therefore, the using amount of the entrainers and the energy consumption are high. The document CN108017517B avoids the problem that an azeotropic agent and a main product ethylene glycol form an azeotrope, and the adoption of a DMO azeotropic agent and 1, 2-butanediol forms an azeotrope, so that the ethylene glycol with the purity of 99.9 percent and the 1, 2-butanediol with the purity of 99.5 percent can be obtained. But the process is pure and has the following defects: the freezing point of the adopted entrainer DMO is 54 ℃, a process pipeline is easy to block in the production process, and the overhaul and the maintenance are inconvenient; the ethylene glycol separation tower and the ethylene glycol refining tower are operated under the pressure of 8-10 bar, the boiling point of ethylene glycol is 265-280 ℃ under the pressure, and the ethylene glycol is a heat-sensitive substance and is easy to polymerize at high temperature; the operation pressures of the ethylene glycol separation tower, the ethylene glycol refining tower, the low-pressure tower and the high-pressure tower are respectively 8-10 bar, 5-10 bar and 10-30 bar, pressure container equipment is required, and the equipment investment cost is high; the process is operated under high pressure, the higher the distillation pressure is, the smaller the relative volatility is, the more difficult the separation becomes, and simultaneously, the tower bottom and the tower top have high temperature, a high-grade heat source needs to be adopted, and the circulating consumption of cooling water is large, which means that the operation cost is high.
SUMMERY OF THE UTILITY MODEL
The utility model aims to solve the technical problem that the prior art has high separation energy consumption and high equipment investment cost, and provides a device for separating ethylene glycol and 1, 2-butanediol by azeotropic distillation. The utility model discloses the people finds in research and development process that diethyl oxalate only forms azeotrope with 1, 2-butanediol, does not form azeotrope with ethylene glycol, and the separator that provides based on this discovery has the energy consumption low, and gained ethylene glycol, 1, 2-butanediol purity are high, characteristics that the yield is high.
In order to solve the technical problem, the utility model discloses the technical scheme who takes as follows:
a process unit for separating glycol and 1, 2-butanediol by azeotropic distillation comprises a glycol refining tower, an entrainer recovery tower and a butanediol removing tower, wherein a discharge port of a tower kettle of the glycol refining tower is connected with a glycol product tank through a pipeline; the device comprises an ethylene glycol refining tower, an azeotropic agent recovery tower reflux tank, an azeotropic agent recovery tower reflux pump, an azeotropic agent recovery tower, a butanediol removal tower reflux tank, a butanediol removal tower reflux pump, an azeotropic agent recovery tower reflux pump, a butanediol removal tower, an azeotropic agent recovery tower reflux tower, a butanediol removal tower and an azeotropic agent recovery tower reflux tower, wherein a tower top discharge port of the ethylene glycol refining tower is connected with an ethylene glycol refining tower condenser, the ethylene glycol refining tower reflux tank and the ethylene glycol refining tower reflux pump through pipelines, the ethylene glycol refining tower reflux pump is connected with a feed inlet of the azeotropic agent recovery tower, a tower top outlet of the azeotropic agent recovery tower is connected with a shell pass inlet of the azeotropic agent recovery tower condenser through a pipeline, the butanediol removal tower reflux tank and the butanediol removal tower reflux pump are connected with the tower top discharge port of the butanediol removal tower through pipelines, the discharge port of the tower kettle of the debutanizing alcohol tower is connected with a 1, 2-butanediol product tank through a pipeline.
And the tower kettle of the butanediol removing tower is connected with a butanediol removing tower supplement reboiler.
And the condenser of the entrainer recovery tower is simultaneously used as a reboiler of the butanediol removing tower, and the inlet and the outlet of the condenser tube pass of the entrainer recovery tower are respectively connected with the tower kettle of the butanediol removing tower.
And the ethylene glycol refining tower, the entrainer recovery tower and the butanediol removal tower are one or a combination of a plate tower, a bulk packed tower or a regular packed tower.
And the outlet of the reflux pump of the ethylene glycol refining tower is divided into two paths, one path is connected to the top reflux port of the ethylene glycol refining tower, and the other path is connected to the feed inlet of the entrainer recovery tower.
And the outlet of the reflux pump of the entrainer recovery tower is divided into two paths, one path is connected to the top reflux port of the entrainer recovery tower, and the other path is connected to the feed inlet of the butanediol removal tower.
And the outlet of the reflux pump of the butanediol removing tower is divided into two paths, one path is connected to the top reflux port of the butanediol removing tower, and the other path is connected to the feed inlet of the entrainer recovery tower.
And a tower kettle discharge port of the ethylene glycol refining tower is sequentially connected with an ethylene glycol refining tower kettle pump, an ethylene glycol product cooler and an ethylene glycol product tank through pipelines.
And a tower kettle discharge port of the debutanizing tower is sequentially connected with a debutanizing tower kettle pump, a 1, 2-butanediol product cooler and a 1, 2-butanediol product tank through pipelines.
The utility model discloses following beneficial effect has:
1. the utility model provides an use diethyl oxalate as azeotropic agent to separate out ethylene glycol and 1, 2-butanediol from the mixture of ethylene glycol and 1, 2-butanediol in the dimethyl oxalate process route of coal system ethylene glycol, the diethyl oxalate freezing point-40.6 ℃, can not block up the process line in the production process.
2. The ethylene glycol refining tower is operated under vacuum, and the ethylene glycol is not easy to polymerize.
3. The whole process is operated under low pressure, no pressure vessel is involved, the equipment investment cost is low, and the temperature of the tower kettle under low pressure is low, so that a high-grade heat source is not needed.
4. The top gas of the entrainer recovery tower is used as a heat source of a reboiler of a butanediol removal tower kettle, so that the steam consumption of the butanediol removal tower is reduced, the circulating water consumption of a condenser of the entrainer recovery tower is saved, the operation cost of the process is reduced, and the economic benefit is obvious.
Drawings
Fig. 1 is a structural diagram of the present invention.
In fig. 1, T101 is an ethylene glycol refining tower, T102 is an entrainer recovery tower, T103 is a butanediol removing tower, E101 is an ethylene glycol refining tower reboiler, E102 is an ethylene glycol refining tower condenser, E103 is an ethylene glycol product cooler, E201 is an entrainer recovery tower reboiler, E202 is an entrainer recovery tower condenser and also a butanediol removing tower reboiler, E301 is a butanediol removing tower supplement reboiler, E302 is a butanediol removing tower condenser, E303 is a 1, 2-butanediol product cooler, P101 is an ethylene glycol refining tower reflux pump, P102 is an ethylene glycol refining tower kettle pump, P201 is an entrainer recovery tower reflux pump, P202 is an entrainer recovery tower kettle pump, P301 is a butanediol removing tower reflux pump, P302 is a butanediol removing tower kettle pump, V101 is an ethylene glycol refining tower reflux tank, V102 is an ethylene glycol product tank, V201 is an entrainer recovery tower reflux tank, V301 is a butanediol removing tower reflux tank, V302 is a 1, 2-butanediol product tank, 1 is a supplement entrainer diethyl oxalate, 2 is a mixture of ethylene glycol and 1, 2-butanediol, 3 is an ethylene glycol product, 4 is an azeotropic mixed liquid of 1, 2-butanediol and diethyl oxalate, 5 is the entrainer diethyl oxalate, 6 is an azeotropic mixed gas of 1, 2-butanediol and diethyl oxalate at the top of an entrainer recovery tower, 7 is an azeotropic mixed liquid of 1, 2-butanediol and diethyl oxalate, 8 is a 1, 2-butanediol product, and 9 is an azeotropic circulating liquid of 1, 2-butanediol and diethyl oxalate.
Detailed Description
The method for separating ethylene glycol and 1, 2-butanediol by azeotropic distillation according to the present invention will be described in detail with reference to the following examples.
A process unit for separating glycol and 1, 2-butanediol by azeotropic distillation comprises a glycol refining tower T101, an entrainer recovery tower T102 and a butanediol removing tower T103, wherein the glycol refining tower T101 is provided with two feed inlets, the tower kettle of the glycol refining tower T101 is connected with a glycol refining tower reboiler E101, and the tower kettle discharge outlet of the glycol refining tower T101 is sequentially connected with a glycol refining tower kettle pump P102, a glycol product cooler E103 and a glycol product tank V102 through pipelines. The outlet of the reflux pump P101 of the ethylene glycol refining tower is divided into two paths, one path is connected to the top reflux port of the ethylene glycol refining tower, and the other path is connected to the feed inlet of the entrainer recovery tower T102. The entrainer recovery column T102 has two feed ports. The outlet of the entrainer recovery tower T102 is connected to the entrainer inlet pipeline of the ethylene glycol refining tower T101 through an entrainer recovery tower kettle pump P202. The top outlet of the entrainer recovery tower T102 is connected to the shell side inlet of an entrainer recovery tower condenser E202 through a pipeline, and the entrainer recovery tower condenser E202 is simultaneously used as a reboiler of a butanediol removal tower T103. The shell pass outlet of the entrainer recovery tower condenser E202 is sequentially connected with an entrainer recovery tower reflux tank V201 and an entrainer recovery tower reflux pump P201, the outlet of the entrainer recovery tower reflux pump P201 is divided into two paths, one path is connected to the top reflux opening of the entrainer recovery tower T102, the other path is connected to the feed inlet of the debutanizer T103, the top discharge opening of the debutanizer T103 is sequentially connected with a debutanizer condenser E302, a debutanizer reflux tank V301 and a debutanizer reflux pump P301 through pipelines, the outlet of the debutanizer reflux pump P301 is divided into two paths, one path is connected to the top reflux opening of the debutanizer T103, and the other path is connected to the other feed inlet of the debutanizer T102. A tower bottom discharge port of the butanediol removing tower T103 is sequentially connected with a butanediol removing tower bottom pump P302, a 1, 2-butanediol product cooler E303 and a 1, 2-butanediol product tank V302 through pipelines. The tower kettle of the butanediol removing tower T103 is connected with a butanediol removing tower supplement reboiler E301.
The device comprises the following technical method:
sending a mixture 2 of ethylene glycol and 1, 2-butanediol and an entrainer diethyl oxalate 5 to an ethylene glycol refining tower T101, supplying heat to the ethylene glycol refining tower by an ethylene glycol refining tower reboiler E101, separating and refining to obtain an ethylene glycol product 3, then pumping the ethylene glycol product 3 through an ethylene glycol product cooler E103 by an ethylene glycol refining tower kettle pump P102, then entering an ethylene glycol product tank V102, condensing azeotropic mixed gas of 1, 2-butanediol and diethyl oxalate at the tower top through an ethylene glycol refining tower condenser E102, then entering an ethylene glycol refining tower reflux tank V101, pressurizing the liquid in the reflux tank through an ethylene glycol refining tower reflux pump P101, then refluxing a part of the liquid, sending a part of azeotropic mixed liquid 4 of 1, 2-butanediol and diethyl oxalate to a double-tower flow formed by the entrainer recovery tower T102 and a butanediol removal tower T103, pressurizing the entrainer diethyl oxalate 5 recovered at the tower bottom of the entrainer recovery tower T102 by an entrainer recovery kettle pump P202, and then circulating to the ethylene glycol refining tower T101, and an entrainer 1 is supplemented at a proper time, an entrainer recovery tower reboiler E201 supplies heat to an entrainer recovery tower T102, azeotropic mixed gas 6 of 1, 2-butanediol and diethyl oxalate at the top of the entrainer recovery tower T102 enters an entrainer recovery tower reflux tank V201 after being condensed by an entrainer recovery tower condenser E202, and the entrainer recovery tower condenser E202 is also a reboiler of a butanediol removal tower and supplies heat to a butanediol removal tower T103. After the liquid in the reflux tank V201 of the entrainer recovery tower is pressurized by a reflux pump P201 of the entrainer recovery tower, part of the liquid reflows, part of azeotropic mixed liquid 7 of 1, 2-butanediol and diethyl oxalate is sent to a butanediol removal tower T103, a supplement reboiler E301 of the butanediol removal tower supplies heat for the butanediol removal tower T103, 1, 2-butanediol product 8 is separated and refined from the bottom of the butanediol removal tower T103, pumping the mixed gas by a butanediol removing tower kettle pump P302 through a 1, 2-butanediol product cooler E303, then feeding the mixed gas into a 1, 2-butanediol product tank V302, condensing the azeotropic mixed gas of 1, 2-butanediol and diethyl oxalate at the top of a butanediol removing tower T103 through a butanediol removing tower condenser E302, then feeding the condensed mixed gas into a butanediol removing tower reflux tank V301, pressurizing the reflux tank liquid by a butanediol removing tower reflux pump P301, then refluxing a part of the reflux tank liquid, and circulating a part of azeotropic circulating liquid 9 of 1, 2-butanediol and diethyl oxalate to an azeotropic agent recovery tower T102.
The operation pressure of the ethylene glycol refining tower T101 is 2-35 kPa, the theoretical plate number is 35-80, the reflux ratio is 5-14, and the temperature of a tower kettle is not more than 165 ℃.
The operation pressure of the entrainer recovery tower T102 is 80-115 kPa, the theoretical plate number is 20-60, the reflux ratio is 5-14, and the temperature of a tower kettle is not more than 191 ℃.
The operation pressure of the butanediol removing tower T103 is 2-25 kPa, the theoretical plate number is 20-60, the reflux ratio is 8-18, and the temperature of a tower kettle is not more than 150 ℃.
The azeotropic agent recovery column T102 has a concentration of 1, 2-butanediol (wt%) in the overhead azeotropic gas 6 of 19.8 to 30.8.
The azeotrope 9 at the top of the butanediol removing tower T103 contains 1, 2-butanediol with the concentration of 5.7-17.5 (wt%).
The ethylene glycol refining tower T101, the entrainer recovery tower T102 and the butanediol removal tower T103 are combined by one or more of a plate tower, a bulk packed tower or a regular packed tower.
The above embodiments are merely illustrative and not restrictive of the present invention, and various modifications can be made without departing from the scope of the present invention, which is intended to be covered by the appended claims.
Claims (9)
1. A process units for separating glycol and 1, 2-butanediol by azeotropic distillation, which is characterized in that: comprises an ethylene glycol refining tower, an entrainer recovery tower and a butanediol removal tower, wherein a tower kettle discharge port of the ethylene glycol refining tower is connected with an ethylene glycol product tank through a pipeline; the device comprises an ethylene glycol refining tower, an azeotropic agent recovery tower reflux tank, an azeotropic agent recovery tower reflux pump, an azeotropic agent recovery tower, a butanediol removal tower reflux tank, a butanediol removal tower reflux pump, an azeotropic agent recovery tower reflux pump, a butanediol removal tower, an azeotropic agent recovery tower reflux tower, a butanediol removal tower and an azeotropic agent recovery tower reflux tower, wherein a tower top discharge port of the ethylene glycol refining tower is connected with an ethylene glycol refining tower condenser, the ethylene glycol refining tower reflux tank and the ethylene glycol refining tower reflux pump through pipelines, the ethylene glycol refining tower reflux pump is connected with a feed inlet of the azeotropic agent recovery tower, a tower top outlet of the azeotropic agent recovery tower is connected with a shell pass inlet of the azeotropic agent recovery tower condenser through a pipeline, the butanediol removal tower reflux tank and the butanediol removal tower reflux pump are connected with the tower top discharge port of the butanediol removal tower through pipelines, the discharge port of the tower kettle of the debutanizing alcohol tower is connected with a 1, 2-butanediol product tank through a pipeline.
2. The apparatus of claim 1, wherein: and the tower kettle of the butanediol removing tower is connected with a butanediol removing tower supplement reboiler.
3. The apparatus of claim 1, wherein: the condenser of the entrainer recovery tower is simultaneously used as a reboiler of the butanediol removing tower, and the inlet and the outlet of the condenser tube pass of the entrainer recovery tower are respectively connected with the tower kettle of the butanediol removing tower.
4. The apparatus of claim 1, wherein: the ethylene glycol refining tower, the entrainer recovery tower and the butanediol removal tower are one or a combination of a plate tower, a bulk packed tower or a regular packed tower.
5. The apparatus of claim 1, wherein: the outlet of the reflux pump of the ethylene glycol refining tower is divided into two paths, one path is connected to the top reflux port of the ethylene glycol refining tower, and the other path is connected to the feed inlet of the entrainer recovery tower.
6. The apparatus of claim 1, wherein: the outlet of the reflux pump of the entrainer recovery tower is divided into two paths, one path is connected to the top reflux port of the entrainer recovery tower, and the other path is connected to the feed port of the butanediol removal tower.
7. The apparatus of claim 1, wherein: the outlet of the reflux pump of the butanediol removing tower is divided into two paths, one path is connected to the top reflux port of the butanediol removing tower, and the other path is connected to the feed inlet of the entrainer recovery tower.
8. The apparatus of claim 1, wherein: the discharge port of the tower kettle of the ethylene glycol refining tower is sequentially connected with an ethylene glycol refining tower kettle pump, an ethylene glycol product cooler and an ethylene glycol product tank through pipelines.
9. The apparatus of claim 1, wherein: the discharge port of the tower bottom of the debutanizing tower is sequentially connected with a debutanizing tower bottom pump, a 1, 2-butanediol product cooler and a 1, 2-butanediol product tank through pipelines.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202022913310.6U CN214105872U (en) | 2020-12-08 | 2020-12-08 | Process unit for separating ethylene glycol and 1, 2-butanediol by azeotropic distillation |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202022913310.6U CN214105872U (en) | 2020-12-08 | 2020-12-08 | Process unit for separating ethylene glycol and 1, 2-butanediol by azeotropic distillation |
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