CN219023294U - Methacrylic acid purifying device - Google Patents

Methacrylic acid purifying device Download PDF

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CN219023294U
CN219023294U CN202223215030.3U CN202223215030U CN219023294U CN 219023294 U CN219023294 U CN 219023294U CN 202223215030 U CN202223215030 U CN 202223215030U CN 219023294 U CN219023294 U CN 219023294U
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extraction
tower
methacrylic acid
extractant
pipeline
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孙玉玉
蔡鑫磊
黄益平
黄晶晶
季雨凡
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China Construction Industrial and Energy Engineering Group Co Ltd
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China Construction Industrial and Energy Engineering Group Co Ltd
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Abstract

The utility model discloses a methacrylic acid purifying device, which comprises a pre-extraction tank, an extraction tower and a rectifying tower; the pre-extraction tank is provided with a methacrylic acid aqueous solution inlet, an oil phase feed inlet, a water phase material outlet and an oil phase material outlet; the extracted water phase material outlet is connected with the water phase material inlet of the extraction tower, and the extracted oil phase material outlet is connected with the oil phase material inlet of the rectifying tower; the top of the rectifying tower is provided with a light component extraction outlet; the side of the rectifying tower is provided with a circulating extractant collecting port, and the circulating extractant collecting port is connected with an extractant reflux port of the extracting tower through a rectifying tower side line circulating extractant pipeline; a methacrylic acid product extraction port is arranged at the tower side of the rectifying tower; the bottom of the rectifying tower is provided with a heavy component extraction outlet. The device of the utility model purifies methacrylic acid, has controllable temperature, effectively reduces the polymerization degree of methacrylic acid, has the product purity of more than 99.4 percent, and has small solid waste production amount and obvious economic benefit.

Description

Methacrylic acid purifying device
Technical Field
The utility model relates to a recovery and purification device of methacrylic acid.
Background
Methacrylic acid is used as an important organic chemical raw material and an intermediate of a polymer, and important derivative products thereof can be used for producing organic glass, polymer modification, paint, adhesive, composite material, ultraviolet curing agent, leather, chemical fiber papermaking, printing and dyeing and the like.
The second-stage catalytic oxidation of isobutene is one of the effective methods for synthesizing methacrylic acid, and the methacrylic acid is subjected to the second-stage catalytic oxidation to generate methacrylic acid-containing gas, so that a water absorption method is commonly adopted in industry, and a small amount of acid-containing byproducts generated by the methacrylic acid and the reaction are dissolved in water to realize the separation of methacrylic acid and other gases. However, in the separation of methacrylic acid from water, the separation of methacrylic acid is one of the problems in the art due to the azeotropy of methacrylic acid and water.
EP345083B discloses a method for extracting methacrylic acid with saturated hydrocarbons of 6 to 9 carbon atoms, CN111217687B discloses a method for separating aqueous methacrylic acid by means of mixed extraction with an ionic liquid and an organic solvent selected from one or more of n-hexane, n-octane, benzene, toluene, xylene and n-heptane. The ionic liquid and the organic solvent are mixed to be used as the extractant, so that the ionic liquid and methacrylic acid generate hydrogen bonds, and the energy consumption of the subsequent separation is greatly improved; when the extracting agents are selected for methacrylic acid extraction, one strand of material of methacrylic acid aqueous solution directly enters the extracting tower, the extracting agents directly enter the extracting tower from the tower kettle, the extracting agents and the methacrylic acid aqueous solution do not have the pre-extraction procedure, the selectivity of the extracting agents to the methacrylic acid is poor, the consumption of the extracting agents is large, and the energy consumption for separating and purifying the subsequent methacrylic acid is obviously improved.
Aiming at the extracted methacrylic acid organic phase, the patent CN103819331B discloses a method for decoloring and purifying methacrylic acid, wherein an extraction solvent recovery tower, a light component removal tower and a heavy component removal decoloring tower are adopted to finish the purification of methacrylic acid, which is also a common method for separating and purifying the methacrylic acid organic phase at present, the methacrylic acid has long residence time in the whole production process and is always present in the tower bottom of a rectifying tower, so that the polymerization is easy to occur, and the yield of the methacrylic acid is low.
Disclosure of Invention
The utility model aims to: the utility model aims to overcome the defects of the prior art and provide a methacrylic acid purification device with low energy consumption and high recovery rate.
The technical scheme is as follows: the utility model relates to a methacrylic acid purifying device which comprises a pre-extraction tank, an extraction tower and a rectifying tower.
The pre-extraction tank is provided with a methacrylic acid aqueous solution inlet, an oil phase feed inlet, a water phase material outlet and an oil phase material outlet; the extracted water phase material outlet is connected with the water phase material inlet of the extraction tower, and the extracted oil phase material outlet is connected with the oil phase material inlet of the rectifying tower;
the top of the rectifying tower is provided with a light component extraction outlet which is connected with a top condenser, and the outlet of the top condenser is connected with the inlet of a condenser reflux tank; the reflux material extraction port of the condenser reflux tank is connected with the methacrylic acid aqueous solution reflux port of the rectifying tower, the circulating material extraction port of the condenser reflux tank is connected with the methacrylic acid aqueous solution reflux port of the extracting tower, the non-condensable gas extraction port of the condenser reflux tank is connected with a vacuum system, and non-condensable gas is discharged; the side of the rectifying tower is provided with a circulating extractant collecting port, and the circulating extractant collecting port is connected with an extractant reflux port of the extracting tower through a rectifying tower side line circulating extractant pipeline; a methacrylic acid product extraction port is arranged at the tower side of the rectifying tower; the bottom of the rectifying tower is provided with a heavy component extraction outlet.
The top of the extraction tower is provided with an extraction phase extraction outlet, and the bottom of the extraction tower is provided with a raffinate phase extraction outlet; the extraction phase extraction outlet is connected with an oil phase feeding port on the pre-extraction tank; and the aqueous phase material collected at the aqueous phase material inlet in the extraction tower, methacrylic acid solution reflowed at the methacrylic acid aqueous solution reflow opening and the extractant reflowed at the extractant reflow opening are in countercurrent contact.
Preferably, in order to improve the material utilization efficiency, the heavy component extraction outlet is divided into two paths, one path is a return pipeline and is connected with the extractant return port of the rectifying tower through a tower kettle reboiler; the other path is a recovery pipeline, and is divided into two pipelines again, wherein one pipeline is a circulating extractant pipeline recovered from the tower kettle, and after being integrated into a side circulating extractant pipeline of the rectifying tower, the other pipeline is a heavy component pipeline discharge system and is connected with an extractant reflux port of the extracting tower through a circulating extractant condenser.
Preferably, in order to conveniently control the temperature of the tower kettle, a temperature detector is arranged on the extraction pipeline, and a supplementary extractant pipeline is arranged on the circulating extractant condenser; a first regulating valve is arranged on the side line circulating extractant pipeline of the rectifying tower; a second regulating valve is arranged on a circulating extractant pipeline extracted from the tower kettle; a third regulating valve is arranged on the heavy component pipeline; a fourth regulating valve is arranged on the supplemental extractant pipeline; when the temperature of the temperature detector is higher than a set value, opening the first regulating valve, the third regulating valve and the fourth regulating valve, and closing the second regulating valve; when the temperature of the temperature detector is lower than the set value, the first regulating valve, the third regulating valve and the fourth regulating valve are closed, and the second regulating valve is opened.
Preferably, the extraction tower is provided with 5 to 15 sieve plates, more preferably 5 to 10 sieve plates.
Preferably, the rectifying tower is provided with 30-50 trays, the oil phase material inlet is positioned at the 20 th-30 th tray, the methacrylic acid product extraction outlet is positioned at the 17 th-25 th tray, and the circulating extractant extraction outlet is positioned at the 25 th-45 th tray.
The extractant in the utility model is selected from organic acid esters with boiling point higher than 161 ℃, such as at least one of dimethyl phthalate, diethyl phthalate, dipropyl phthalate, dibutyl phthalate, diisobutyl hexahydrophthalate or dibutyl sebacate.
The mass ratio of methacrylic acid to organic acid esters in the methacrylic acid aqueous solution is 1: (1-2), more preferably 1: (1.2-1.5).
The circulating extractant is extracted from the tower side of the rectifying tower, condensed to 25-40 ℃ and then refluxed to the extracting tower, more preferably condensed to 30-35 ℃, and can be realized by setting the temperature of a circulating extractant condenser.
The rectifying tower is operated under reduced pressure, and the working pressure is preferably 0.001-0.01 MPa.
The beneficial effects are that: (1) According to the utility model, the pre-extraction tank is arranged in front of the extraction tower, so that the consumption of the extractant is reduced; (2) According to the utility model, the temperature detector is arranged on the extraction pipeline of the rectifying tower, so that the extraction of the rectifying tower is controlled, the rectifying tower is flexibly regulated and controlled, the energy consumption in the production process is reduced, and the product yield is increased; (3) According to the utility model, the methacrylic acid aqueous solution reflux port is arranged in the extraction tower, methacrylic acid solution is refluxed according to the extraction effect, so that methacrylic acid is promoted to be better dissolved in the extractant, the extraction effect is ensured, and the energy consumption in the subsequent separation process is reduced; (4) The device for purifying the methacrylic acid has the advantages of short residence time and controllable temperature in the whole process, effectively reduces the polymerization degree of the methacrylic acid, ensures that the product purity reaches more than 99.4 percent, has small solid waste production amount and obvious economic benefit.
Drawings
FIG. 1 is a process flow diagram of the present utility model.
In the figure: the device comprises a D1-pre-extraction tank, a T1-extraction tower, a T2-rectifying tower, an E1-tower top condenser, an E2-tower kettle reboiler, a D2-condenser reflux tank, a P1-vacuum system and an E3-circulating extractant condenser.
1-methacrylic acid aqueous solution to be extracted, 2-extracting water phase materials in a pre-extracting tank, 3-circulating extractant, 4-extracting phase materials, 5-raffinate phase materials, 6-methacrylic acid-containing condensate, 7-extracting oil phase materials in a pre-extracting tank, 8-non-condensable light components, 9-purified methacrylic acid products, 10-circulating extractant, 11-tower kettle-extracted circulating extractant, 12-heavy components, 13-tower kettle reboiler materials, 14-non-condensable gas and 15-supplementary extractant.
Detailed Description
The technical scheme of the utility model is described in detail below through the drawings, but the protection scope of the utility model is not limited to the embodiments.
Example 1: the aqueous methacrylic solution 1 to be extracted having a methacrylic acid content (mass fraction, hereinafter the same) of 29.21%, a water content of 61.51%, an acetic acid content of 6.1%, other light component impurities (impurities having a boiling point lower than that of methacrylic acid, hereinafter the same) of 1.98%, a heavy component impurities (impurities having a boiling point higher than that of methacrylic acid, hereinafter the same) of 1.2% were fed from the aqueous methacrylic solution inlet of the pre-extraction tank D1 at a flow rate of 5000kg/h, the circulating extractant 3 having a methacrylic acid content (mass fraction, hereinafter the same) of 8.03%, a dibutyl phthalate content of 89.83%, and a heavy component impurities content of 2.14% was fed into the extraction column T1 at a flow rate of 1902 kg/h. The number of the tower plates of the extraction tower T1 is 9, and the temperature in the pre-extraction tank D1 is 30 ℃. Methacrylic acid is dissolved in dibutyl phthalate through pre-extraction and extraction, an extraction phase extracted material 4 is extracted from the top of an extraction tower, a raffinate phase extracted material 5 is extracted from the bottom of the extraction tower, an oil phase extracted material 7 is extracted from an oil phase extracted material outlet in a pre-extraction tank, an aqueous phase extracted material 2 is extracted from an aqueous phase extracted material outlet in the pre-extraction tank, and the contents of the materials 2, 4, 5 and 7 are shown in table 1.
TABLE 1 Pre-extraction tank and extraction tank outlet Material content
Figure SMS_1
The oil phase material 7 extracted from the extraction pre-extraction tank enters a rectifying tower T2 with the operating pressure of 0.003MPa and the number of the tower plates of 40 from the 28 th tower plate, light component materials are extracted from the top of the rectifying tower T2 and condensed to 30 ℃ through a condenser E1, part of the light component materials are refluxed, the liquid phase which is not refluxed is the condensate 6 containing methacrylic acid and enters the 3 rd tower plate of the extraction tower, and the noncondensable gas 14 is discharged from a vacuum system; purified methacrylic acid product 9 is extracted from a 24 th tray of the rectifying tower T2, and a side-extracted circulating extractant 10 is extracted from a 26 th tray of the rectifying tower T2; the circulating extractant 11 and heavy components 12 extracted from the tower bottom are extracted from the tower bottom of the rectifying tower T2.
And a temperature detector on a tower kettle extraction pipeline shows that the temperature of the tower kettle material is 109.5 ℃, then a first regulating valve and a third regulating valve on a rectifying tower side line circulating extractant 10 pipeline and a heavy component 12 pipeline are closed, a second regulating valve on a circulating extractant 11 pipeline extracted from the tower kettle is opened, and a fourth regulating valve on a supplementary extractant 15 pipeline is closed. The circulating extractant 11 extracted from the tower kettle is cooled to 30 ℃ through a circulating extractant condenser E3 and flows back to the extraction tower T1 for recycling. Wherein the contents of each of materials 6, 9, 11 and 14 are shown in Table 2.
TABLE 2 rectifying column and condenser reflux drum outlet Material content
Figure SMS_2
Example 2: the aqueous methacrylic solution 1 to be extracted having a methacrylic acid content (mass fraction, hereinafter the same) of 29.21%, a water content of 61.51%, an acetic acid content of 6.1%, other light component impurities (impurities having a boiling point lower than that of methacrylic acid, hereinafter the same) of 1.98%, a heavy component impurities (impurities having a boiling point higher than that of methacrylic acid, hereinafter the same) of 1.2% were fed from the aqueous methacrylic solution inlet of the pre-extraction tank D1 at a flow rate of 5000kg/h, the circulating extractant 3 having a methacrylic acid content (mass fraction, hereinafter the same) of 8.03%, a dibutyl phthalate content of 89.83%, and a heavy component impurities content of 2.14% was fed into the extraction column T1 at a flow rate of 1902.7 kg/h. The number of the plates of the extraction column is 9, and the temperature in the pre-extraction tank D1 is 30 ℃. Methacrylic acid is dissolved in dibutyl phthalate through pre-extraction and extraction, an extraction phase extracted material 4 is extracted from the top of an extraction tower, a raffinate phase extracted material 5 is extracted from the bottom of the extraction tower, an oil phase extracted material 7 is extracted from an oil phase extracted material outlet in a pre-extraction tank, an aqueous phase extracted material 2 is extracted from an aqueous phase extracted material outlet in the pre-extraction tank, and the contents of the materials 2, 4, 5 and 7 are shown in table 3.
TABLE 3 Pre-extraction tank and extraction tank outlet Material content
Figure SMS_3
Figure SMS_4
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The oil phase material 7 extracted from the extraction pre-extraction tank enters a rectifying tower T2 with the operating pressure of 0.003MPa and the number of the tower plates of 40 from the 28 th tower plate, light component materials are extracted from the top of the rectifying tower T2 and condensed to 30 ℃ through a condenser E1, part of the light component materials are refluxed, the liquid phase which is not refluxed is the condensate 6 containing methacrylic acid and enters the 3 rd tower plate of the extraction tower, and the noncondensable gas 14 is discharged from a vacuum system; purified methacrylic acid product 9 is extracted from a 24 th tray of the rectifying tower T2, and a side-extracted circulating extractant 10 is extracted from a 26 th tray of the rectifying tower T2; the circulating extractant 11 and heavy components 12 extracted from the tower bottom are extracted from the tower bottom of the rectifying tower T2.
The temperature detector on the extraction pipeline of the tower kettle shows that the temperature of the material at the tower kettle is 230.6 ℃, then the second regulating valve on the 11 pipelines of the circulating extractant extracted from the tower kettle is closed, the 10 pipelines of the side circulating extractant of the rectifying tower and the first regulating valve and the third regulating valve on the 12 pipelines of the heavy component are opened, meanwhile, the fourth regulating valve on the 15 pipelines of the supplementary extractant is opened, the 15 pipelines of the supplementary extractant are supplemented into the system at the flow rate of 390kg/h, the flow rate of the 10 pipelines of the side circulating extractant of the rectifying tower is controlled, and the temperature of the material extracted from the 10 pipelines of the circulating extractant is ensured to be 110 ℃. The materials of the side-line extracted circulating extractant 10 pipeline and the supplementary extractant 15 pipeline are cooled to 30 ℃ by a circulating extractant condenser and returned to the extraction tower T1 for recycling. Wherein the contents of each of materials 6, 9, 10, 12 and 14 are shown in Table 4.
TABLE 4 rectifying column and condenser reflux drum outlet Material content
Figure SMS_5
Figure SMS_6
Example 3: the aqueous methacrylic solution 1 to be extracted having a methacrylic acid content (mass fraction, hereinafter the same) of 30.60%, a water content of 61.10%, an acetic acid content of 5.1%, other light component impurities (impurities having a boiling point lower than that of methacrylic acid, hereinafter the same) of 2.19% and a heavy component impurities (impurities having a boiling point higher than that of methacrylic acid, hereinafter the same) of 1.01% was fed from the aqueous methacrylic solution inlet of the pre-extraction tank D1 at a flow rate of 3000kg/h, the methacrylic acid content (mass fraction, hereinafter the same) of 9.64%, the dipropyl phthalate content of 88.26%, and the heavy component impurities content of 2.1% was fed into the extraction column T1 at a flow rate of 1106.55 k/h. The number of plates of the extraction column is 8, and the temperature in the pre-extractor is 34 ℃. Methacrylic acid is dissolved in dipropyl phthalate through pre-extraction and extraction, an extraction phase extracted material 4 is extracted from the top of an extraction tower, a raffinate phase extracted material 5 is extracted from the bottom of the extraction tower, an oil phase extracted material 7 is extracted from an oil phase extracted material outlet in a pre-extraction tank, an aqueous phase extracted material 2 is extracted from an aqueous phase extracted material outlet in the pre-extraction tank, and the contents of the materials 2, 4, 5 and 7 are shown in table 5.
TABLE 5 Pre-extraction tank and extraction tank outlet Material content
Figure SMS_7
The oil phase material 7 extracted from the pre-extraction tank after extraction enters a rectifying tower T2 with the operating pressure of 0.004MPa and the number of the tower plates of 30 from the 28 th tower plate, light component materials are extracted from the top of the rectifying tower T2 and condensed to 34 ℃ through a condenser E1, partial reflux is carried out, the non-refluxed liquid phase is the condensate 6 containing methacrylic acid, enters the 3 rd tower plate of the extraction tower, and the non-condensable gas 14 is discharged from a vacuum system; purified methacrylic acid product 9 is extracted from a 20 th tray of the rectifying tower T2, and a side-extracted circulating extractant 10 is extracted from a 26 th tray of the rectifying tower T2; the circulating extractant 11 and heavy components 12 extracted from the tower bottom are extracted from the tower bottom of the rectifying tower.
And a temperature detector on a tower kettle extraction pipeline shows that the temperature of the tower kettle material is 109.8 ℃, then a first regulating valve and a third regulating valve on a rectifying tower side line circulating extractant 10 pipeline and a heavy component 12 pipeline are closed, a second regulating valve on a circulating extractant 11 pipeline extracted from the tower kettle is opened, and a fourth regulating valve on a supplementary extractant 15 pipeline is closed. The circulating extractant 11 extracted from the tower kettle is cooled to 34 ℃ through a circulating extractant condenser E3 and flows back to the extraction tower T1 for recycling. Wherein the contents of each of materials 6, 9, 11 and 14 are shown in Table 6.
TABLE 6 rectifying column and condenser reflux drum outlet Material content
Figure SMS_8
Example 4: the aqueous methacrylic solution 1 to be extracted having a methacrylic acid content (mass fraction, hereinafter the same) of 30.60%, a water content of 61.10%, an acetic acid content of 5.1%, other light component impurities (impurities having a boiling point lower than that of methacrylic acid, hereinafter the same) of 2.19% and a heavy component impurities (impurities having a boiling point higher than that of methacrylic acid, hereinafter the same) of 1.01% was fed from the aqueous methacrylic solution inlet of the pre-extraction tank D1 at a flow rate of 3000kg/h, the methacrylic acid content (mass fraction, hereinafter the same) of 10.53%, the dipropyl phthalate content of 87.39% and the heavy component impurities content of 2.08% was fed into the extraction column T1 at a flow rate of 1117.65 kg/h. The number of plates of the extraction column is 8, and the temperature in the pre-extraction tank D1 is 34 ℃. Methacrylic acid is dissolved in dipropyl phthalate through pre-extraction and extraction, an extraction phase extracted material 4 is extracted from the top of an extraction tower, a raffinate phase extracted material 5 is extracted from the bottom of the extraction tower, an oil phase extracted material 7 is extracted from an oil phase extracted material outlet in a pre-extraction tank, an aqueous phase extracted material 2 is extracted from an aqueous phase extracted material outlet in the pre-extraction tank, and the contents of the materials 2, 4, 5 and 7 are shown in table 7.
TABLE 7 Pre-extraction tank and extraction tank outlet Material content
Figure SMS_9
Figure SMS_10
The oil phase materials extracted from the pre-extraction tank after extraction enter a rectifying tower T2 with the number of plates being 30 and the operating pressure being 0.005MPa from the 28 th plate, light component materials are extracted from the top of the rectifying tower T2 and condensed to 34 ℃ by a condenser E1 after rectification separation, partial reflux is carried out, the non-refluxed liquid phase is a condensate 6 containing methacrylic acid, enters the 3 rd plate of the extraction tower, and non-condensable gas 14 is discharged from a vacuum system; purified methacrylic acid product 9 is extracted from a 20 th tray of the rectifying tower, and a side-stream extracted circulating extractant 10 is extracted from a 26 th tray of the rectifying tower T2; the circulating extractant 11 and heavy components 12 extracted from the tower bottom are extracted from the tower bottom of the rectifying tower T2.
The temperature detector on the material pipeline 11 of the material extraction port of the tower kettle shows that the temperature of the material at the tower kettle is 211.3 ℃, then the second regulating valve on the circulating extractant 11 pipeline extracted from the tower kettle is closed, the first regulating valve and the third regulating valve on the circulating extractant 10 pipeline of the side line of the rectifying tower and the heavy component 12 pipeline are opened, meanwhile, the fourth regulating valve on the supplementing extractant 15 pipeline is opened, the supplementing extractant 15 pipeline is supplemented into the system at the flow rate of 163.7kg/h, the flow rate of the circulating extractant 10 pipeline of the rectifying tower is controlled, and the material extraction temperature of the circulating extractant 10 pipeline is ensured to be 109.5 ℃. The materials of the side-line extracted circulating extractant 10 pipeline and the supplementary extractant 15 pipeline are cooled to 34 ℃ by a circulating extractant condenser and returned to the extraction tower T1 for recycling. Wherein the contents of each of materials 6, 9, 10, 12 and 14 are shown in Table 8.
TABLE 8 rectifying column and condenser reflux drum outlet Material content
Figure SMS_11
As described above, although the present utility model has been shown and described with reference to certain preferred embodiments, it is not to be construed as limiting the utility model itself. Various changes in form and details may be made therein without departing from the spirit and scope of the utility model as defined by the appended claims.

Claims (5)

1. A methacrylic acid purification device, characterized in that: comprises a pre-extraction tank (D1), an extraction tower (T1) and a rectifying tower (T2);
the pre-extraction tank (D1) is provided with a methacrylic acid aqueous solution inlet, an oil phase feeding port, a produced water phase material outlet and a produced oil phase material outlet; the extracted water phase material outlet is connected with a water phase material inlet of the extraction tower (T1), and the extracted oil phase material outlet is connected with an oil phase material inlet of the rectifying tower (T2);
the top of the rectifying tower (T2) is provided with a light component extraction outlet which is connected with a top condenser (E1), and the outlet of the top condenser (E1) is connected with the inlet of a condenser reflux tank (D2); the reflux material extraction port of the condenser reflux tank (D2) is connected with the methacrylic acid aqueous solution reflux port of the rectifying tower (T2), the circulating material extraction port of the condenser reflux tank (D2) is connected with the methacrylic acid aqueous solution reflux port of the extracting tower (T1), and the non-condensable gas extraction port of the condenser reflux tank (D2) is connected with the vacuum system (P1) and is discharged; the side of the rectifying tower (T2) is provided with a circulating extractant collecting port, and the circulating extractant collecting port is connected with an extractant reflux port of the extracting tower (T1) through a rectifying tower side line circulating extractant pipeline; a methacrylic acid product extraction port is arranged at the tower side of the rectifying tower (T2); a heavy component extraction outlet is arranged at the bottom of the rectifying tower (T2);
the top of the extraction tower (T1) is provided with an extraction phase extraction outlet, and the bottom of the extraction tower is provided with a raffinate phase extraction outlet; the extraction phase extraction outlet is connected with an oil phase feeding port on the pre-extraction tank (D1); the aqueous phase material collected by the aqueous phase material inlet of the extraction tower (T1), methacrylic acid solution which flows back from the methacrylic acid aqueous solution reflux port and the extractant which flows back from the extractant reflux port are in countercurrent contact.
2. The apparatus for purifying methacrylic acid according to claim 1, wherein: the heavy component extraction port is divided into two paths, one path is a return pipeline and is connected with an extractant return port of the rectifying tower (T2) through a tower kettle reboiler (E2); the other path is a extraction pipeline, and is divided into two pipelines again, wherein one pipeline is a circulating extractant pipeline extracted from the tower kettle, and after being integrated into a side circulating extractant pipeline of the rectifying tower, the other pipeline is a heavy component pipeline discharge system and is connected with an extractant reflux port of the extracting tower (T1) through a circulating extractant condenser (E3).
3. The apparatus for purifying methacrylic acid according to claim 2, wherein: a temperature detector is arranged on the extraction pipeline, and a supplementary extractant pipeline is arranged on the circulating extractant condenser (E3); a first regulating valve is arranged on the side line circulating extractant pipeline of the rectifying tower; a second regulating valve is arranged on a circulating extractant pipeline extracted from the tower kettle; a third regulating valve is arranged on the heavy component pipeline; the fourth regulating valve is arranged on the supplemental extractant pipeline.
4. The apparatus for purifying methacrylic acid according to claim 1, wherein: the extraction tower (T1) is provided with 5-15 sieve plates.
5. The apparatus for purifying methacrylic acid according to claim 1, wherein: the rectifying tower is provided with 30-50 trays, the oil phase material inlet is positioned at the 20 th-30 th tray, the methacrylic acid product extraction outlet is positioned at the 17 th-25 th tray, and the circulating extractant extraction outlet is positioned at the 25 th-45 th tray.
CN202223215030.3U 2022-12-01 2022-12-01 Methacrylic acid purifying device Active CN219023294U (en)

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