CN209778702U - Device for separating n-butyl alcohol and n-butyl ether by extraction and rectification processes - Google Patents
Device for separating n-butyl alcohol and n-butyl ether by extraction and rectification processes Download PDFInfo
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- CN209778702U CN209778702U CN201821809673.1U CN201821809673U CN209778702U CN 209778702 U CN209778702 U CN 209778702U CN 201821809673 U CN201821809673 U CN 201821809673U CN 209778702 U CN209778702 U CN 209778702U
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Abstract
The utility model relates to a device for separating n-butyl alcohol and n-butyl ether by utilizing extraction and rectification processes, which comprises an extraction tower, a butyl ether recovery tower, an extractant regeneration tower, a butyl ether recovery tower top condenser, a butyl ether recovery tower bottom reboiler, an extractant regeneration tower top condenser and an extractant regeneration tower bottom reboiler; the method is characterized in that an extracting agent and butanol and butyl ether raw material liquid are subjected to continuous countercurrent extraction in an extraction tower; the liquid phase at the top of the extraction tower enters a butyl ether recovery tower, the separated qualified butyl ether product is extracted from the top of the extraction tower, and the regenerated extractant at the bottom of the extraction tower flows back to enter the extraction tower; and the liquid phase at the bottom of the extraction tower enters an extractant recovery tower, the separated qualified butanol product is extracted from the top of the extraction tower, and the regenerated extractant at the bottom of the extraction tower flows back to enter the extraction tower, so that the recycling of the extractant is realized. Method solved the difficult problem of separating of butanol and butyl ether in the current DBP production technology, the utility model discloses simple process is controllable, whole technology energy consumption is low, no waste material discharges.
Description
Technical Field
the utility model belongs to the technical field of the chemical industry, concretely relates to utilize extraction and rectification technology to separate device of n-butanol and n-butyl ether.
Background
the plasticizer dibutyl phthalate (DBP) is produced by esterification reaction of phthalic anhydride and butanol under the catalysis of concentrated sulfuric acid. Since this reaction is reversible, a butanol excess method is generally used in the production. Therefore, the butyl ether as a byproduct is continuously accumulated in the circulating alcohol, and the speed of the esterification reaction and the quality of the DBP product are influenced after a certain concentration is reached. The butyl ether is an important factor influencing the quality of the DBP product, and can be evaporated out together with alcohol and water at the esterification reaction temperature, and then reflows to the reactor together with the alcohol after being condensed and cooled; in the dealcoholization step, butanol and butyl ether can be removed together with alcohol, condensed and cooled, and then returned to the recovered alcohol receiving tank, so that separation of butanol and butyl ether is important. In the subsequent dealcoholization process, the butanol has certain solubility in water, so the part of the alcohol in the wastewater is recovered by a stripping method in the production. Butanol and butyl ether, however, can form ternary azeotropes with water and cannot be separated by conventional distillation methods. Therefore, the thrown-off recycled alcohol is generally disposed of as waste. However, butanol and butyl ether are important chemical raw materials, and the recycling of butanol and butyl ether not only saves resources, but also reduces sewage discharge and environmental pollution and increases benefits, so that it is very important to develop an environment-friendly method for separating butanol and butyl ether.
SUMMERY OF THE UTILITY MODEL
The utility model discloses to the difficult problem of separating of butanol and butyl ether in the DBP production technology, developed a technology energy consumption low, no waste discharge utilize the device and the method of extraction and rectification to separate butanol and butyl ether.
The utility model provides a technical scheme that above-mentioned technical problem adopted, its characterized in that includes following step:
A device for separating n-butyl alcohol and n-butyl ether by using extraction and rectification processes; comprises an extraction tower C1, a butyl ether recovery tower C2, an extractant regeneration tower C3, a C2 overhead condenser E1, a C2 tower bottom reboiler E2, a C3 overhead condenser E3 and a C3 tower bottom reboiler E4;
Wherein, in the extraction tower C1, a liquid phase extraction outlet is arranged at the top of the tower, and an extractant feed inlet, a normal butanol and n-butyl ether feed inlet and a tower bottom extraction outlet are respectively arranged from top to bottom; a liquid phase outlet at the top of the C1 tower is connected with a raw material inlet at the middle part of the C2 tower, and a liquid phase outlet at the bottom of the C1 tower is connected with a raw material inlet at the middle part of the C3 tower;
Wherein, in the butyl ether recovery tower C2, a gas phase outlet is arranged at the top of the tower, and a reflux port, a raw material inlet, a reboiler return tower port and a tower bottom discharge port are respectively arranged from top to bottom; the gas phase outlet at the top of the C2 tower is connected with a condenser E1 at the top of the C2 tower, the outlet of the condenser is divided into two pipelines, one pipeline is connected with the reflux inlet of the C2 tower, and the other pipeline is a n-butyl ether product; a discharge hole at the bottom of the C2 tower is divided into two pipelines, one pipeline is connected with an inlet of a reboiler E2 of the C2 tower, an outlet of a reboiler E2 of the C2 tower is connected with a reboiler return tower hole, and a pipeline at a discharge hole at the bottom of the C2 tower is connected with an extractant feed hole of the C1 extraction tower;
Wherein, in the extractant regeneration tower C3, a gas phase outlet is arranged at the top of the tower, and a reflux port, a feed inlet, a reboiler tower return port and a tower bottom extraction port are respectively arranged from top to bottom; the gas phase outlet at the top of the C3 tower is connected with a condenser E3 at the top of the C3 tower, the outlet of the condenser is divided into two pipelines, one pipeline is connected with the reflux port of the C3 tower, and the other pipeline is a normal butanol product; the outlet of the C3 tower bottom is divided into two pipelines, one pipeline is connected with the inlet of a C3 tower reboiler E4, the outlet of a C3 tower reboiler E4 is connected with the tower return port of a reboiler, and the pipeline of a C3 tower bottom outlet is connected with the feed port of an extracting agent of a C1 extraction tower.
simultaneously the utility model also discloses a method for utilizing extraction and rectification technology to separate n-butyl alcohol and n-butyl ether, including the following steps:
moreover, the specific process control conditions of the extraction column C1 are: and (3) operating at normal temperature and normal pressure.
moreover, the operation pressure of the butyl ether recovery tower C2 is normal pressure, the reflux ratio is 1-3, the bottom temperature is 197.1-198.5 ℃, and the top temperature is 141.8-142.6 ℃.
Moreover, the extractant regeneration tower C3 has the operation pressure of normal pressure, the reflux ratio of 0.2-0.32, the tower bottom temperature of 179.5-179.9 ℃ and the tower top temperature of 117.3-117.5 ℃.
And the extractant is one or a mixture of more than two of octanol, glycerol and glycol.
When different kinds of extractants are mixed, the mixing mass ratio of the two extractants is 1-4, and the addition amount of the extractants is 1.3-5 times (mass ratio) of the feeding amount.
The utility model has the advantages of as follows with positive effect:
Method solved the difficult problem of separating of butanol and butyl ether in the current DBP production technology, the utility model discloses simple process is controllable, whole technology energy consumption is low, no waste material discharges.
the utility model discloses utilize the extractant to realize the complete separation of butanol and butyl ether, realize the separation of butanol and extractant, butyl ether and extractant through rectifier unit again to realize extractant cyclic utilization, and obtain the higher butanol and butyl ether product of purity. The process does not generate waste water, and belongs to an environment-friendly process.
drawings
FIG. 1 shows the process flow of the present invention for separating n-butanol and n-butyl ether by extraction and rectification.
A C1 extraction tower, a C2 butyl ether recovery tower, a C3 extractant regeneration tower, an E1C1 overhead condenser, an E2C1 tower bottom reboiler, an E3C3 overhead condenser and an E4C3 tower bottom reboiler;
1-extractant, 2-n-butanol and n-butyl ether raw material, 3-n-butanol and extractant, 4-n-butyl ether and extractant, 5-regenerative extractant, 6-regenerative extractant, 7-n-butanol and 8-n-butyl ether.
Detailed Description
The technical solution of the present invention is explained in detail below, and the specific embodiments described herein are only used for explaining the present invention, but the scope of protection of the present invention is not limited to the embodiments.
A device for separating n-butyl alcohol and n-butyl ether by using extraction and rectification processes; comprises an extraction tower C1, a butyl ether recovery tower C2, an extractant regeneration tower C3, a C2 overhead condenser E1, a C2 tower bottom reboiler E2, a C3 overhead condenser E3 and a C3 tower bottom reboiler E4;
wherein, in the extraction tower C1, a liquid phase extraction outlet is arranged at the top of the tower, and an extractant feed inlet, a normal butanol and n-butyl ether feed inlet and a tower bottom extraction outlet are respectively arranged from top to bottom; a liquid phase outlet at the top of the C1 tower is connected with a raw material inlet at the middle part of the C2 tower, and a liquid phase outlet at the bottom of the C1 tower is connected with a raw material inlet at the middle part of the C3 tower;
Wherein, in the butyl ether recovery tower C2, a gas phase outlet is arranged at the top of the tower, and a reflux port, a raw material inlet, a reboiler return tower port and a tower bottom discharge port are respectively arranged from top to bottom; the gas phase outlet at the top of the C2 tower is connected with a condenser E1 at the top of the C2 tower, the outlet of the condenser is divided into two pipelines, one pipeline is connected with the reflux inlet of the C2 tower, and the other pipeline is a n-butyl ether product; a discharge hole at the bottom of the C2 tower is divided into two pipelines, one pipeline is connected with an inlet of a reboiler E2 of the C2 tower, an outlet of a reboiler E2 of the C2 tower is connected with a reboiler return tower hole, and a pipeline at a discharge hole at the bottom of the C2 tower is connected with an extractant feed hole of the C1 extraction tower;
Wherein, in the extractant regeneration tower C3, a gas phase outlet is arranged at the top of the tower, and a reflux port, a feed inlet, a reboiler tower return port and a tower bottom extraction port are respectively arranged from top to bottom; the gas phase outlet at the top of the C3 tower is connected with a condenser E3 at the top of the C3 tower, the outlet of the condenser is divided into two pipelines, one pipeline is connected with the reflux port of the C3 tower, and the other pipeline is a normal butanol product; the outlet of the C3 tower bottom is divided into two pipelines, one pipeline is connected with the inlet of a C3 tower reboiler E4, the outlet of a C3 tower reboiler E4 is connected with the tower return port of a reboiler, and the pipeline of a C3 tower bottom outlet is connected with the feed port of an extracting agent of a C1 extraction tower.
The method for separating the n-butyl alcohol and the n-butyl ether by using the device is characterized in that an extracting agent enters from an extracting agent feed inlet of an extracting tower C1, the n-butyl alcohol and the n-butyl ether enter from a feed inlet at the bottom of the extracting tower C1, a filler is filled in the extracting tower C1, the extracting agent is continuously in countercurrent contact with a mixture of the n-butyl alcohol and the n-butyl ether in the tower, the butyl ether and the extracting agent are enriched at the top of the tower under the action of the extracting agent, and the butanol and the extracting agent are enriched at the bottom; the liquid phase of the butyl ether and the extractant at the top of the tower enter a raw material inlet at the middle part of a butyl ether recovery tower C2, the steam at the top of the tower is condensed by a condenser E1 at the top of the tower, then part of the steam flows back to a tower C2 and is extracted as a qualified product n-butyl ether, and the regenerated extractant at the bottom of the tower flows back to an extractant inlet of an extraction tower C1; butanol and an extractant liquid phase at the bottom of the extraction tower C1 enter a raw material inlet at the middle part of an extractant regeneration tower C3, steam at the top of the extraction tower partially flows back to the C3 tower after being condensed by a condenser E3, part of the steam is taken as a qualified product n-butanol to be extracted, a regenerated extractant at the bottom of the extraction tower flows back to an extractant inlet of the extraction tower C1, and the extractant is recycled.
It is further characterized in that the specific process control conditions of the extraction column C1 are as follows: and (3) operating at normal temperature and normal pressure.
The method is further characterized in that the operation pressure of the butyl ether recovery tower C2 is normal pressure, the reflux ratio is 1-3, the bottom temperature is 197.1-198.5 ℃, and the top temperature is 141.8-142.6 ℃.
It is further characterized in that the extractant regeneration tower C3 has the operation pressure of normal pressure, the reflux ratio of 0.2-0.32, the tower bottom temperature of 179.5-179.9 ℃ and the tower top temperature of 117.3-117.5 ℃.
The method is further characterized in that the extracting agent is one or a mixture of more than two of octanol, glycerol and glycol.
the method is further characterized in that when different kinds of extracting agents are mixed, the mixing mass ratio of the two extracting agents is 1-4, and the adding amount of the extracting agent is 1.3-5 times (mass ratio) of the feeding amount.
Detailed description of the preferred embodiment 1
a method for separating n-butyl alcohol and n-butyl ether by using extraction and rectification processes comprises the following steps:
The raw material comes from a DBP process and is characterized in that butyl ether accounts for 93 percent by weight and butanol accounts for 7 percent by weight, the extraction tower is operated at normal temperature and normal pressure, and the feeding amounts of the extracting agent and the raw material are respectively 500 kg/h; butyl ether recovery tower, normal pressure operation, reflux ratio 1, extractant recovery tower, normal pressure operation, reflux ratio 0.26. The temperature of the top of the butyl ether recovery tower is 142.1 ℃, the temperature of the bottom of the butyl ether recovery tower is 197.6 ℃, the temperature of the top of the extractant recovery tower is 117.5 ℃, and the temperature of the bottom of the extractant recovery tower is 178.2 ℃. The equipment is continuously operated for 12 hours, the purity of the butyl ether product is 98.6 percent, and the purity of the butanol product is 99.7 percent.
Specific example 2
A method for separating n-butyl alcohol and n-butyl ether by using extraction and rectification processes comprises the following steps:
The overall scheme is the same as example 1, but with the following differences: the raw material comes from a DBP process and is characterized in that butyl ether accounts for 93 percent by weight and butanol accounts for 7 percent by weight, the extraction tower is operated at normal temperature and normal pressure, and the feeding amounts of the extracting agent and the raw material are respectively 1000kg/h and 500 kg/h; the butyl ether recovery tower is operated under normal pressure, the reflux ratio is 2, the extractant recovery tower is operated under normal pressure, and the reflux ratio is 0.3. The temperature of the top of the butyl ether recovery tower is 142.3 ℃, the temperature of the bottom of the butyl ether recovery tower is 198.4 ℃, the temperature of the top of the extractant recovery tower is 117.4 ℃, and the temperature of the bottom of the extractant recovery tower is 179.9 ℃. The equipment is continuously operated for 12 hours, the purity of the butyl ether product is 98.8 percent, and the purity of the butanol product is 99.8 percent.
Claims (3)
1. A device for separating n-butyl alcohol and n-butyl ether by using extraction and rectification processes; the method is characterized in that: the method comprises an extraction tower (C1), a butyl ether recovery tower (C2), an extractant regeneration tower (C3), a butyl ether recovery tower (C2) overhead condenser (E1), a butyl ether recovery tower (C2) bottom reboiler (E2), an extractant regeneration tower (C3) overhead condenser (E3) and an extractant regeneration tower (C3) bottom reboiler (E4);
in the extraction tower (C1), a liquid phase extraction outlet is arranged at the top of the tower, and an extractant feeding port, a normal butanol and n-butyl ether feeding port and a tower bottom extraction outlet are respectively arranged from top to bottom; the liquid phase outlet at the top of the extraction tower (C1) is connected with the raw material inlet at the middle part of the butyl ether recovery tower (C2), and the bottom extraction outlet of the extraction tower (C1) is connected with the raw material inlet at the middle part of the extractant regeneration tower (C3);
In the butyl ether recovery tower (C2), a gas phase outlet is arranged at the top of the tower, and a reflux port, a raw material inlet, a reboiler tower return port and a tower bottom discharge port are respectively arranged from top to bottom; a gas phase outlet at the top of the butyl ether recovery tower (C2) is connected with a condenser (E1) at the top of the butyl ether recovery tower (C2), the outlet of the condenser is divided into two pipelines, one pipeline is connected with a reflux port of the butyl ether recovery tower (C2), and the other pipeline is a n-butyl ether product; a discharge hole at the bottom of the butyl ether recovery tower (C2) is divided into two pipelines, one pipeline is connected with an inlet of a reboiler (E2) of the butyl ether recovery tower (C2), an outlet of the reboiler (E2) of the butyl ether recovery tower (C2) is connected with a tower return port of the reboiler, and a pipeline at the discharge hole at the bottom of the butyl ether recovery tower (C2) is connected with an extracting agent feed port of an extraction tower (C1);
In the extractant regeneration tower (C3), a gas phase outlet is arranged at the top of the tower, and a reflux port, a feed inlet, a reboiler tower return port and a tower bottom extraction port are respectively arranged from top to bottom; the gas phase outlet at the top of the extractant regeneration tower (C3) is connected with a condenser (E3) at the top of the extractant regeneration tower (C3), the outlet of the condenser is divided into two pipelines, one pipeline is connected with the reflux port of the extractant regeneration tower (C3), and the other pipeline is a normal butanol product; the bottom discharge port of the extractant regeneration tower (C3) is divided into two pipelines, one pipeline is connected with the inlet of a reboiler (E4) of the extractant regeneration tower (C3), the outlet of the reboiler (E4) of the extractant regeneration tower (C3) is connected with the tower return port of the reboiler, and the bottom discharge port of the extractant regeneration tower (C3) is connected with the inlet of an extractant of the extractant extraction tower (C1).
2. the apparatus for separating n-butanol and n-butyl ether by extraction and rectification as claimed in claim 1, wherein: the operation pressure of the butyl ether recovery tower (C2) is normal pressure, the reflux ratio is 1-2, the temperature of the bottom of the tower is 197.1-198.5 ℃, and the temperature of the top of the tower is 141.8-142.6 ℃.
3. The apparatus for separating n-butanol and n-butyl ether by extraction and rectification as claimed in claim 1, wherein: the operation pressure of the extractant regeneration tower (C3) is normal pressure, the reflux ratio is 0.2-0.32, the bottom temperature is 179.5-179.9 ℃, and the top temperature is 117.3-117.5 ℃.
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| CN201821809673.1U CN209778702U (en) | 2018-11-05 | 2018-11-05 | Device for separating n-butyl alcohol and n-butyl ether by extraction and rectification processes |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109438178A (en) * | 2018-11-05 | 2019-03-08 | 石家庄白龙化工股份有限公司 | The device and method of n-butanol and n-butyl ether is separated with rectification process using extraction |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109438178A (en) * | 2018-11-05 | 2019-03-08 | 石家庄白龙化工股份有限公司 | The device and method of n-butanol and n-butyl ether is separated with rectification process using extraction |
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