CN216629706U - Separation refining system device suitable for low-concentration organic solution - Google Patents
Separation refining system device suitable for low-concentration organic solution Download PDFInfo
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Abstract
The application discloses separation refining system device suitable for low concentration organic solution, including heat transfer unit device, preconcentration system and rectifying column system, preconcentration system includes membrane module and vacuum system, vacuum system is to membrane module extraction vacuum, raw materials liquid sends into the membrane module after heat transfer unit device preheats and divides the water preconcentration, the preliminary concentrate of high temperature of formation is as heat source of one of them of heat transfer unit device, the preliminary concentrate of high temperature is after heat transfer unit device retrieves the heat, send into rectifying column system, heat transfer unit device is used for heat source and raw materials liquid cold source to carry out the heat transfer, heat in the heat source is retrieved, and heat raw materials liquid to the required temperature of preconcentration. The device of this application sets up heat exchanger unit device, but the low-grade heat source that the system produced reduces the energy consumption index in the conventional rectification to partial azeotropic distillation, the loss that can effectual reduction target product, very big improvement economic benefits.
Description
Technical Field
The application relates to a separation refining system device suitable for low-concentration organic solution.
Background
In the chemical production process, a large amount of aqueous solution containing low-concentration organic solvent is often generated, and the organic solvent in the aqueous solution is recovered and mostly treated by adopting a rectification process at present. However, because the concentration of the organic solvent in the aqueous solution is low, the number of theoretical plates of the rectifying tower required for obtaining a purer organic solvent product by rectifying and separating is high, the reflux ratio is high, and the energy consumption is high. Especially for some organic solution systems with low concentration or azeotrope, the energy consumption of the conventional rectification is further greatly improved, the loss of the target product is large, and the rectification yield is low.
Disclosure of Invention
The application aims to provide a separation and refining system device suitable for low-concentration organic solution aiming at the existing refining and separation of conventional low-concentration organic solution, and provides a high-efficiency and energy-saving treatment scheme and system aiming at the problems of high energy consumption and large target product loss in conventional rectification of the conventional low-concentration organic solution.
The technical scheme adopted by the application is as follows:
the separation refining system device suitable for the low-concentration organic solution is characterized by comprising a heat exchange unit device, a pre-concentration system and a rectifying tower system, wherein the heat exchange unit device consists of a multi-channel heat exchanger and comprises a cold source channel and a plurality of heat source channels; the pre-concentration system comprises a membrane component and a matched vacuum system, wherein the membrane component adopts a membrane tube separator and comprises a shell and a hollow fiber membrane component arranged in the shell, and membrane micropores for water vapor to pass through are formed in the hollow fiber membrane; an inlet of the vacuum system is connected with a shell of the membrane module through a pipeline, and an outlet of the vacuum system is connected with a condensing system through a pipeline;
the cold source channel inlet of the heat exchange unit device is used for introducing raw material liquid, and the cold source channel outlet of the heat exchange unit device is connected with the membrane tube side inlet of the membrane component through a pipeline; the membrane tube pass outlet of the membrane component is connected with the rectifying tower system through a pipeline through one of the heat source channels of the heat exchange unit device, so that the high-temperature primary concentrated solution which is discharged from the membrane tube pass outlet of the membrane component and subjected to water diversion is used as one of the heat sources of the heat exchange unit device, and the high-temperature primary concentrated solution enters the rectifying tower system after heat is recovered by the heat exchange unit device.
The separation and refining system device suitable for the low-concentration organic solution is characterized in that the rectifying tower system comprises a rectifying tower, a tower bottom reboiler and a tower top condenser, wherein an outlet at the top of the rectifying tower is connected with a tower top liquid separation tank through the tower top condenser by a pipeline, so that tower top gas discharged from the outlet at the top of the rectifying tower is condensed by the tower top condenser to form tower top liquid and is collected in the tower top liquid separation tank; heating the kettle liquid of the rectifying tower by a tower bottom reboiler, wherein the tower bottom reboiler adopts a tubular heat exchanger structure, a high-temperature heat source is introduced into a heat source channel of the tower bottom reboiler for heating, and a secondary heat source is discharged from a heat source channel outlet of the tower bottom reboiler; the outlet at the bottom of the rectifying tower is connected with a delivery pump through a pipeline, so that high-temperature tower bottom separation liquid in the tower bottom of the rectifying tower is pumped out by the delivery pump;
the heat exchange unit device comprises a cold source channel and three heat source channels, wherein raw material liquid is introduced into the cold source channel of the heat exchange unit device and is used for heating the raw material liquid to a temperature required by preconcentration;
the membrane tube pass outlet of the membrane component is connected with the rectifying tower system through a pipeline through one of the heat source channels of the heat exchange unit device, the outlet of the delivery pump is connected with the downstream device through a pipeline through the second heat source channel of the heat exchange unit device, and the heat source channel outlet of the tower bottom reboiler is connected with the downstream device through the last heat source channel of the heat exchange unit device through a pipeline, so that the three heat source channels of the heat exchange unit device are respectively introduced with high-temperature primary concentrated liquid, high-temperature tower bottom separation liquid and a secondary heat source, heat exchange is conveniently carried out on the three heat source channels and raw material liquid, and heat of the three heat sources is recovered.
The separation and refining system device suitable for the low-concentration organic solution is characterized by further comprising a supplementary heat source inlet pipeline, wherein the supplementary heat source inlet pipeline is connected to a pipeline between a heat source channel outlet of the tower bottom reboiler and one of heat source channels of the heat exchange unit device, so that a supplementary heat source input by the supplementary heat source inlet pipeline is added into a secondary heat source, and the heating effect of heat exchange of the raw material liquid is ensured.
The separation and refining system device suitable for the low-concentration organic solution is characterized in that a liquid discharge port of the tower top liquid separation tank is divided into two paths, the first path is connected with a reflux port at the top of the rectifying tower through a pipeline, the second path is discharged through the pipeline and sent to a downstream working section, or the second path is connected with a cold source channel inlet of the heat exchange unit device through the pipeline.
Compared with the prior art, the beneficial effects obtained by the application are that:
1. the system adopts the membrane module to pretreat the organic solvent, removes most of water, can effectively reduce the energy consumption of the device and greatly reduce the loss of the corresponding target product of an azeotropic system.
2. The rectifying tower system that this application set up simultaneously can only refine the raw materials that can tentatively concentrate after handling the membrane, reaches a higher purity.
3. In addition, the heat exchanger unit device is arranged in the system device, so that low-grade heat sources generated by the device system can be effectively recovered, the system energy consumption of the device is further reduced, and the device has high economic value.
Drawings
FIG. 1 is a system diagram of a separation and purification system apparatus suitable for low concentration organic solution;
in the figure: e01-heat exchange system unit device, E02-tower bottom reboiler, E03-tower top condenser, X01-membrane module, X02-vacuum system, P01-transfer pump, T01-rectifying tower, V01-tower top liquid separation tank, 1-raw material liquid, 2-high temperature raw material liquid, 3-high temperature primary concentrated liquid, 4-low temperature primary concentrated liquid, 5-high temperature tower bottom separated liquid, 6-low temperature tower bottom separated liquid, 7-tower top gas, 8-tower top returned liquid, 9-tower top separated liquid, 10-high temperature heat source, 11-secondary heat source, 12-supplementary heat source, 13-low temperature heat source, 14-condensed water and 15-tower top returned liquid.
Detailed Description
The present invention is further illustrated by the following examples, which should not be construed as limiting the scope of the invention.
Example (b): compare FIG. 1
A separation refining system device suitable for low-concentration organic solution comprises a heat exchange unit device E01, a pre-concentration system and a rectifying tower system, wherein the heat exchange unit device E01 is used for exchanging heat between a heat source and a raw material liquid cold source, recovering heat in the heat source and heating the raw material liquid to a temperature required by pre-concentration; the pre-concentration system comprises a membrane component X01 and a matched vacuum system X02, raw material liquid is preheated by a heat exchange unit device E01 and then is sent into a membrane tube pass of a membrane component X01, the vacuum system X02 is used for extracting vacuum from the shell pass of the membrane component X01 through a pipeline, a pumping outlet of the vacuum system X02 is connected with a condensing system through a pipeline, moisture in raw material liquid passes through the membrane component X01 and is pumped out by the vacuum system X02, pumped water vapor is cooled by the condensing system to produce condensed water 14, a membrane tube pass outlet of the membrane component X01 discharges high-temperature primary concentrated liquid 3 after water diversion, the high-temperature primary concentrated liquid 3 serves as one of heat sources of the heat exchange unit device E01, the high-temperature primary concentrated liquid 3 is cooled by recovering heat through the heat exchange unit device E01 to form low-temperature primary concentrated liquid 4, and the low-temperature primary concentrated liquid enters a rectifying tower system for further rectification and purification, and the rectifying mode comprises pressurization rectification and vacuum rectification according to different rectification pressures.
Further, the membrane module X01 may be a membrane tube separator, which includes a housing and a hollow fiber membrane module disposed in the housing, wherein the hollow fiber membrane module is provided with membrane micropores for water vapor to pass through. The raw material liquid 1 is heated to a certain temperature (generally 70-90 ℃) to form a high-temperature raw material liquid 2, and the high-temperature raw material liquid enters a membrane component X01 and a matched vacuum system X02. In the membrane module X01, a large number of micropores on the surface of the hollow fiber membrane and high-temperature raw material liquid are utilized to generate steam pressure difference on two sides of the membrane, the evaporated steam permeates through the membrane holes and enters the other side of the membrane module, meanwhile, the steam is extracted by a vacuum system X02, and the extracted steam is cooled to generate condensed water 14.
Referring to fig. 1, the rectification column system includes a rectification column T01, a bottoms reboiler E02, and an overhead condenser E03. The raw material liquid is separated by a membrane component X01, dewatered and discharged high-temperature primary concentrated liquid 3, heat of which is recycled by a heat exchange unit device E01 to realize temperature reduction, and then enters a rectifying tower T01 for rectification. The overhead gas 7 discharged from the top outlet of the rectifying tower T01 is condensed by an overhead condenser E03 to form overhead liquid, and the overhead liquid is collected in an overhead liquid separation tank V01, and the overhead liquid can be sent to a downstream working section according to requirements, can be mixed with a raw material liquid for repeated refining, and can also flow back to the top of the rectifying tower T01. In comparison with fig. 1, the liquid outlet of the tower top liquid separation tank V01 is divided into two paths, the first path is taken as the tower top reflux liquid 15 and flows back to the top of the rectification tower T01, the second path is taken as the tower top separation liquid 9 and is sent to the downstream section, or the second path is taken as the tower top return liquid 8 and is mixed with the raw material liquid and then sent to the heat exchange unit device E01 as the cold source to be heated to the temperature required for preconcentration. The bottom liquid of the rectifying tower T01 is heated by a tower bottom reboiler E02, the tower bottom reboiler E02 adopts a tubular heat exchanger structure, a high-temperature heat source 10 is introduced into a heat source channel of the tower bottom reboiler E02 for heating, and a secondary heat source 11 is discharged from a heat source channel outlet of the tower bottom reboiler E02. The high-temperature bottom separated liquid 5 in the bottom of the rectifying tower T01 is pumped out by a transfer pump P01.
The heat exchange unit device E01 comprises a multi-channel heat exchanger, and comprises a cold source channel and three heat source channels, wherein the cold source channel of the heat exchange unit device E01 is filled with raw material liquid for heating the raw material liquid to a temperature required by pre-concentration; and three heat source channels of the heat exchange unit device E01 are respectively introduced with the high-temperature primary concentrated solution 3, the high-temperature tower bottom separation solution 5 and the secondary heat source 11 so as to respectively exchange heat with the raw material solution and recover the heat of the three heat sources. And the separation liquid 5 at the bottom of the high-temperature tower is subjected to heat exchange by a heat exchange unit device E01 to form separation liquid 6 at the bottom of the low-temperature tower, and the separation liquid is sent to a downstream device. The rectifying column is heated by a tower bottom reboiler E02, the high temperature heat source 10 used for the rectifying column is usually hot water, low pressure steam, or the like, and the heat is recovered by a heat exchange unit device E01 through a secondary heat source 11 after heat exchange by the tower bottom reboiler to form a low temperature heat source 13 delivery device (in this application, the low temperature heat source 13 is condensed water). Meanwhile, according to different separation media, the possibility that a heat source in the system is insufficient to heat the raw material liquid to a specified temperature exists, and at the moment, a supplementary heat source 12 can be added into the secondary heat source 11 to ensure the heating effect. Referring to fig. 1, the apparatus of the present application further includes a supplementary heat source inlet pipe, and a supplementary heat source 12 input by the supplementary heat source inlet pipe is added to the secondary heat source 11 to ensure a heating effect of heat exchange on the raw material liquid.
The method for separating and refining the low-concentration organic solution by the device comprises the following steps:
1) taking a low-concentration organic solution as a raw material solution, taking the raw material solution as a cold source, feeding the raw material solution into a cold channel of a heat exchange unit device E01, heating to a temperature required by preconcentration, feeding the raw material solution into a membrane tube pass of a membrane component X01 for preconcentration, simultaneously extracting vacuum from a shell pass of the membrane component X01 through a vacuum system X02, and cooling water vapor extracted by a vacuum system X02 through a condensing system to produce condensed water 14; a membrane tube pass outlet of the membrane component X01 discharges the high-temperature primary concentrated solution 3 after water separation;
the high-temperature primary concentrated solution 3 is used as one path of heat source of a heat exchange unit device E01, the high-temperature primary concentrated solution 3 is cooled after heat is recovered by the heat exchange unit device E01, and then enters a rectifying tower T01 for rectification, the kettle of the rectifying tower T01 is heated by a tower bottom reboiler E02, a high-temperature heat source 10 is introduced into a heat channel of the tower bottom reboiler E02 for heating, a secondary heat source 11 is discharged from an outlet of the heat channel of the tower bottom reboiler E02, and the secondary heat source 11 and the high-temperature tower bottom separated liquid 5 discharged from the tower bottom of the rectifying tower T01 are respectively used as the other two paths of heat sources of the heat exchange unit device E01;
2) the overhead gas 7 discharged from the top outlet of the rectifying tower T01 is condensed by an overhead condenser E03 to form overhead liquid and is collected in an overhead liquid separation tank V01, the liquid in the overhead liquid separation tank V01 is sent to a downstream section as overhead separation liquid 9 except a part of the liquid used for overhead reflux 15, or the liquid in the overhead liquid separation tank V01 is mixed with raw material liquid as overhead return liquid 8 to be subjected to the operation steps of pre-concentration, heat exchange cooling and refining repeatedly.
The low concentration organic solution of this application is the azeotrope of organic matter and water, and the mass concentration of organic matter is below 15%, and the temperature of the preliminary concentrate of high temperature 3, high temperature tower bottom parting liquid 5 all is less than secondary heat source 11's temperature.
Further, the low-concentration organic solution is an acrylic acid aqueous solution with the concentration of less than 15wt%, the acrylic acid aqueous solution is heated to 60-90 ℃, then the acrylic acid aqueous solution is sent to a membrane assembly X01 for pre-concentration until the concentration is increased to 25-40 wt%, and the temperature of the high-temperature primary concentrated solution 3 is 60-90 ℃. And recovering heat of the high-temperature primary concentrated solution 3 through a heat exchange unit device E01, cooling to 20-40 ℃, and then, rectifying in a rectifying tower T01, wherein the rectification vacuum degree is below 10 kPa. The temperature of the separation liquid 5 at the bottom of the high-temperature tower is 70-85 ℃, and the temperature of the secondary heat source 11 is 95-110 ℃.
Example 1: raw material liquid (10% by weight aqueous acrylic acid solution) was fed in an amount of 7000kg/h
The raw material liquid 1 enters a heat exchange unit device E01, and is heated and heated (to 60-90 ℃) through a secondary heat source 11, a supplementary heat source 12, a high-temperature primary concentrated liquid 3 and a high-temperature tower bottom separation liquid 5. The preheated high-temperature raw material liquid 2 enters a pre-concentration system, in a membrane component, X01, steam pressure difference is generated on two sides of the membrane by utilizing a large number of micropores on the surface of the hollow fiber membrane and the raw material liquid under high temperature, and evaporated steam penetrates through membrane holes to enter the other side of the membrane component and is extracted by utilizing a vacuum system X02. The extracted water vapor is cooled to produce condensed water 14. The content of acrylic acid in the high-temperature primary concentrated solution 3 which is left after membrane separation and concentration is increased to 25-40% by weight, and then the acrylic acid is cooled to (20-40 ℃) after heat is recovered by a heat exchange unit device E01, and enters a rectifying tower system.
The rectification column system comprises a rectification column T01, a bottom reboiler E02 and an overhead condenser E03. And (3) carrying out vacuum rectification on the high-temperature primary concentrated solution (the concentration of acrylic acid is 25-40 wt%) from the upstream in a rectifying tower T01, wherein the vacuum degree is 8 kPa.
The rectified overhead gas 7 is a mixed gas of water and acrylic acid (the concentration of the acrylic acid is 7-10 wt%), the temperature is 40-50 ℃, the mixed gas is condensed by an overhead condenser E03 to form overhead liquid, the overhead liquid is collected in an overhead liquid separation tank V01, the overhead liquid can be used as overhead separation liquid 9 to be sent to a downstream working section according to needs, and the overhead return liquid 8 can be used as the overhead liquid to be mixed with raw material liquid and then repeatedly subjected to operations of pre-concentration, heat exchange cooling and refining. In example 1, the entire overhead liquid in the overhead liquid separation tank V01 was mixed with the raw material liquid as the overhead return liquid 8, and then subjected to the operations of preconcentration, heat exchange for cooling, and purification repeatedly.
And (3) after rectification, the purity of acrylic acid in the tower bottom separated liquid 5 is more than or equal to 99%, the temperature is 70-85 ℃, the flow rate is 450-650 kg/h, part of the tower bottom separated liquid 5 is pressurized and pumped out through a conveying pump P01, and is sent to a downstream device after being subjected to heat exchange through a heat exchange unit device E01 and cooled to 30-50 ℃, and the overall recovery rate of the acrylic acid in the embodiment 1 is 70-90%.
The rectifying tower is heated by a reboiler E02 at the bottom of the tower, and the high-level heat source 10 adopted in the embodiment 1 is low-pressure steam (0.12 Mpa, 105 ℃) with the dosage of 3000 kg/h-4500 kg/h. The high-level heat source 10 forms a secondary heat source 11 (0.12 Mpa, 100 ℃) after heat exchange and condensation in a tower bottom reboiler E02, and the heat is recovered through a heat exchange unit device E01 and then cooled to (30-50 ℃) to be sent out of the device.
In example 1, the raw material liquid 1 is heated by the supplementary heat source 12 to secure the heating effect. The supplementary heat source in the embodiment 1 is high-temperature hot water (0.2 MPa, 100 ℃), and the using amount is 5000-7500 kg/h.
According to the embodiment, the product purity of acrylic acid can be more than or equal to 99% by refining the acrylic acid aqueous solution with 10wt% of raw materials, the consumption of low-pressure water vapor (0.12 Mpa, 105 ℃) is 3000-4500 kg/h, and the consumption of high-temperature hot water (0.2 Mpa, 100 ℃) is 5000-7500 kg/h.
And the conventional single-tower vacuum rectification is adopted to rectify and purify a raw material liquid (10 wt% of acrylic acid aqueous solution), the treatment capacity of the raw material liquid is 7000kg/h, low-pressure steam (0.12 Mpa, 105 ℃) is adopted as a heat source of a reboiler at the tower bottom, and the dosage of the low-pressure steam (0.12 Mpa, 105 ℃) is 18000-21000 kg/h under the same condition that the purity of rectification target acrylic acid is more than or equal to 99%, meanwhile, acrylic acid lost along with the gas phase at the tower top reaches 350-400 kg/h due to the azeotropy of the acrylic acid and water, and the recovery rate of the acrylic acid is only 40-50%.
Therefore, when the low-concentration acrylic acid aqueous solution is separated and purified, compared with the conventional single-tower vacuum rectification, the embodiment can save steam by about 70 percent, effectively reduce energy consumption and improve the recovery rate.
The statements in this specification merely set forth a list of implementations of the inventive concept and the scope of the present invention should not be construed as limited to the particular forms set forth in the examples.
Claims (4)
1. A separation refining system device suitable for low-concentration organic solution is characterized by comprising a heat exchange unit device (E01), a pre-concentration system and a rectifying tower system, wherein the heat exchange unit device (E01) consists of a multi-channel heat exchanger and comprises a cold source channel and a plurality of heat source channels; the pre-concentration system comprises a membrane module (X01) and a matched vacuum system (X02), the membrane module (X01) adopts a membrane tube separator, and comprises a shell and a hollow fiber membrane module arranged in the shell, and membrane micropores which are convenient for water vapor to pass through are arranged on the hollow fiber membrane; the inlet of the vacuum system (X02) is connected with the shell of the membrane module (X01) through a pipeline, and the outlet of the vacuum system (X02) is connected with the condensation system through a pipeline;
a cold source channel inlet of the heat exchange unit device (E01) is used for introducing raw material liquid, and a cold source channel outlet of the heat exchange unit device (E01) is connected with a membrane tube side inlet of the membrane component (X01) through a pipeline;
the membrane tube pass outlet of the membrane component (X01) is connected with the rectifying tower system through one of the heat source channels of the heat exchange unit device (E01) by a pipeline, so that the high-temperature primary concentrated solution (3) which is discharged from the membrane tube pass outlet of the membrane component (X01) and subjected to water diversion is used as one of the heat sources of the heat exchange unit device (E01), and the high-temperature primary concentrated solution (3) enters the rectifying tower system after heat is recovered by the heat exchange unit device (E01).
2. The apparatus of claim 1, wherein the rectification column system comprises a rectification column (T01), a reboiler (E02) at the bottom of the rectification column, and a condenser (E03) at the top of the rectification column (T01), and the outlet at the top of the rectification column (T01) is connected to the overhead liquid separation tank (V01) through an overhead condenser (E03), so that the overhead gas (7) discharged from the outlet at the top of the rectification column (T01) is condensed by the overhead condenser (E03) to form an overhead liquid and is collected in the overhead liquid separation tank (V01); the bottom liquid of the rectifying tower (T01) is heated by a tower bottom reboiler (E02), the tower bottom reboiler (E02) adopts a tubular heat exchanger structure, a high-temperature heat source (10) is introduced into a heat source channel of the tower bottom reboiler (E02) for heating, and a secondary heat source (11) is discharged from a heat source channel outlet of the tower bottom reboiler (E02); the bottom outlet of the rectifying tower (T01) is connected with a delivery pump (P01) through a pipeline, so that the high-temperature tower bottom separated liquid (5) in the tower bottom of the rectifying tower (T01) is pumped outwards by the delivery pump (P01);
the heat exchange unit device (E01) comprises a cold source channel and three heat source channels, and raw material liquid is introduced into the cold source channel of the heat exchange unit device (E01) and is used for heating the raw material liquid to a temperature required by pre-concentration;
the membrane tube side outlet of the membrane component (X01) is connected with the rectifying tower system through a pipeline through one of heat source channels of the heat exchange unit device (E01), the outlet of the delivery pump (P01) is connected with the downstream device through a second heat source channel of the heat exchange unit device (E01) through a pipeline, the heat source channel outlet of the tower bottom reboiler (E02) is connected with the downstream device through a pipeline through the last heat source channel of the heat exchange unit device (E01), so that the three heat source channels of the heat exchange unit device (E01) are respectively introduced with the high-temperature primary concentrated liquid (3), the high-temperature tower bottom separated liquid (5) and the secondary heat source (11) to respectively exchange heat with the raw material liquid and recover the heat of the three heat sources.
3. The apparatus of claim 2, further comprising a supplementary heat source inlet pipe connected to a line between an outlet of the heat source channel of the bottom reboiler (E02) and one of the heat source channels of the heat exchange unit apparatus (E01), so that the supplementary heat source (12) inputted from the supplementary heat source inlet pipe is added to the secondary heat source (11) to ensure a heating effect of heat exchange of the raw material liquid.
4. The apparatus of claim 2, wherein the liquid outlet of the liquid tank (V01) is divided into two paths, the first path is connected to the top reflux port of the rectification column (T01) via a pipeline, the second path is discharged via a pipeline to a downstream process, or the second path is connected to the inlet of the cold source channel of the heat exchange unit apparatus (E01) via a pipeline.
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