CN112552174B - Device and method for rectifying acetic ester - Google Patents
Device and method for rectifying acetic ester Download PDFInfo
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- CN112552174B CN112552174B CN202011534926.0A CN202011534926A CN112552174B CN 112552174 B CN112552174 B CN 112552174B CN 202011534926 A CN202011534926 A CN 202011534926A CN 112552174 B CN112552174 B CN 112552174B
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- C07—ORGANIC CHEMISTRY
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- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
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- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/52—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
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Abstract
The invention provides a device and a method for rectifying acetic ester. The step of rectifying the acetic ester of the invention comprises: firstly, passing industrial-grade acetate through a pretreatment tower; then the pretreated acetate exchanges heat with a heat exchanger to raise the temperature, and then enters a rectifying tower for rectification; and (3) feeding the rectified acetate into a rectifying tower auxiliary tower through an in-tower distributor, cooling, and then feeding into a microfiltration device for filtering to obtain the electronic grade acetate. The method for rectifying the acetate has the advantages of simple process, low energy consumption and capability of reducing the production cost.
Description
Technical Field
The invention relates to a device and a method for rectifying acetic ester, belonging to the technical field of acetic ester.
Background
The ultra-clean high-purity reagent is internationally called as a process chemical, is also called as a wet chemical in Taiwan areas of America, europe and China, is one of key basic chemical materials in the manufacturing process of Integrated Circuits (ICs), very large scale integrated circuits (VLSI) and discrete devices, is mainly used for cleaning and corroding chips and cleaning wafers, has the purity and cleanliness directly influencing whether geometric figures of the chips can be realized, and has very important influence on the yield, the electrical property and the reliability of the integrated circuits. At present, ultra-clean reagents are mainly concentrated internationally in companies across countries such as Merck, ashland, olin, etc., and in recent years, some manufacturers and devices for producing electronic grade solvents are also sequentially appeared in China due to national policy guidance. The electronic grade solvent is mainly used for preparing chips, and is used for wet cleaning before gluing; the second is used for etching and removing photoresist in the chip photoetching process, and the third is used for cleaning in the manufacturing process of the silicon wafer.
At present, the common purification technologies for preparing the ultra-pure reagent at home and abroad mainly comprise technologies such as rectification, distillation, sub-boiling distillation, isothermal distillation, reduced pressure distillation, low-temperature distillation, sublimation, gas absorption, chemical treatment, resin exchange, membrane treatment and the like, and different purification technologies are suitable for purification processes of different products. The distillation method is a method for separating a distilland by partially vaporizing the distilland and condensing steam by utilizing the difference of the volatility of each component in a liquid mixture, and is the most widely applied liquid mixture separation means at present. Electronic grade acetates are commonly used in the preparation of cleaning formulations. Electronic-grade purification of organic matter (acetate) is generally a multi-column purification process. Taking industrial grade butyl acetate as an example, two-tower process is generally needed for light-weight removal and heavy-weight removal rectification separation, 1 ton of qualified finished product of electronic grade butyl acetate is produced, and the rectification energy consumption (rectification heat load) is about 290-350kw. The traditional rectification separation process is adopted, so that the process is more and high in energy consumption, the operation complexity is increased due to the more process, and the investment of a fixing device is increased.
Disclosure of Invention
The invention aims to provide a device and a method for rectifying acetic ester, and develops a method for rectifying acetic ester, which improves the interest rate of process system energy, reduces fixed investment, has high product purity, is simple and convenient to operate and has less three wastes by designing a rectifying tower.
In order to achieve the purpose, the invention adopts the technical scheme that: a device for rectifying acetate comprises a pretreatment tower, a heat exchanger, a rectifying tower, a reboiler and a microfiltration device;
a raw material feeding hole is formed in the bottom of the pretreatment tower; the top of the pretreatment tower is connected with a heat exchanger, the heat exchanger is connected with a rectifying tower, and the rectifying tower is respectively connected with the reboiler and the microfiltration device;
the rectifying tower comprises a main tower, an auxiliary tower, a tower bottom and a tower top; the main tower is provided with a feed inlet, the auxiliary tower is provided with a discharge outlet, the tower bottom is provided with a feed inlet and an industrial grade acetate byproduct outlet, and the tower top is provided with a gas phase water outlet; the main column and the auxiliary column are separated by a divider;
the heat exchanger is provided with two feed inlets and two discharge outlets, the first feed inlet is communicated with the discharge outlet of the pretreatment tower, the second feed inlet is communicated with the gas phase water outlet at the top of the tower, the first outlet is communicated with the feed inlet of the main tower, the second outlet is branched into two paths, one path is communicated with the top of the tower, and the other path is communicated with the industrial grade acetate byproduct outlet;
the feed inlet of the microfiltration device is communicated with the discharge outlet at the bottom of the auxiliary tower and is provided with an acetate discharge outlet.
In the above apparatus for rectifying acetic ester, preferably, the number of theoretical plates of the main column of the rectifying column is not less than 6, and the number of theoretical plates of the auxiliary column is not less than 3.
In a rectification column, it is assumed that the gas phase and the liquid phase are in sufficient contact time for the two phases to reach equilibrium and that the relationship between the components on the trays corresponds to the number of trays required for the relationship specified by the equilibrium curve. In the case of a fixed feed condition and reflux ratio, the higher the product purity, the larger the number of required plates, but the larger the number of plates, the larger the plate resistance, and the higher the operating pressure of the column, resulting in a decrease in the separation effect. The number of the tower plates is determined according to raw materials in the process of producing the acetate.
In the above apparatus for rectifying acetic ester, preferably, the rectifying tower distributor is made of plastic, and the inside of the tower is lined with plastic.
Plastics are chemically stable, lightweight, strong, and easily formed into various shapes.
Further, the present invention provides a method for rectifying acetic ester by using the apparatus for rectifying acetic ester according to any one of claims 1 to 3, comprising the steps of: firstly, passing industrial-grade acetate through a pretreatment tower; then the pretreated acetate exchanges heat with a heat exchanger to raise the temperature, and then enters a rectifying tower for rectification; the rectified acetate enters a rectifying tower auxiliary tower through an in-tower distributor, and enters a microfiltration device after being cooled to be filtered to obtain electronic grade acetate; the acetate is one of ethyl acetate, propyl acetate or butyl acetate.
As a preferred embodiment of the method for rectifying acetic ester according to the present invention, the volume ratio of the main column and the subsidiary column of the rectifying column is 1:0.3-1:1. more preferably, the volume ratio of the main column and the auxiliary column of the rectifying column is 1:0.5-1:1. more preferably, the volume ratio of the main column and the auxiliary column of the rectifying column is 1:0.8-1:1.
the volume ratio of the main column and the subsidiary column of the rectification column affects the heat load of the apparatus in the method for rectifying acetic ester and the quality of acetic ester. Research shows that when the volume ratio of the main tower to the auxiliary tower of the rectifying tower is 1:0.5-1:1, reducing the thermal load of the rectifying tower, and reducing the content of acetic acid and water in a finished product; particularly, when the volume ratio of the main tower to the auxiliary tower of the rectifying tower is 1:0.8-1:1, the method for rectifying the acetic ester has the advantages that the heat load of the rectifying tower is lowest, and the quality of the acetic ester is optimal.
As a preferred embodiment of the method for rectifying acetic ester of the present invention, the reflux ratio at the top of the main column is 0.1 to 10, the reflux ratio at the bottom of the main column is 100 to 10000, and the reflux ratio at the bottom of the subsidiary column is 0 to 1. More preferably, the reflux ratio at the top of the main tower is 0.5-0.7, and the reflux ratio at the bottom of the main tower is 500-4000.
The reflux ratio is also a main factor influencing the load of the rectifying tower, the quality of the acetic ester and the yield of the acetic ester in the method for rectifying the acetic ester, and researches show that the reflux ratio of the top of the main tower is 0.5-0.7, and the reflux ratio of the bottom of the main tower is 500-4000.
As a preferred embodiment of the method for rectifying acetic ester of the present invention, the butyl acetate rectification conditions are: the temperature of the bottom of the main tower is 124.5-128 ℃, the temperature of the top of the main tower is 123.5-125.4 ℃, the temperature of the bottom of the auxiliary tower is 125.5-128 ℃, and the temperature of the top of the auxiliary tower is 124-125.5 ℃; the propyl acetate rectification conditions are as follows: the temperature of the bottom of the main tower is 101-102.9 ℃, the temperature of the top of the main tower is 99.5-101.5 ℃, the temperature of the bottom of the auxiliary tower is 101-102.9 ℃, and the temperature of the top of the auxiliary tower is 100.5-101.5 ℃; the ethyl acetate rectification conditions are as follows: the temperature of the bottom of the main tower is 76-78.5 ℃, the temperature of the top of the main tower is 75-77.5 ℃, the temperature of the bottom of the auxiliary tower is 76-78.5 ℃, and the temperature of the top of the auxiliary tower is 75-78 ℃.
Compared with the prior art, the invention has the following beneficial effects: according to the invention, by designing the rectifying tower, the reboiler and the heat exchanger in the traditional multi-tower process are replaced by utilizing energy coupling in the tower, the cost is reduced by about 10-30%, meanwhile, the discharge amount of unorganized VOC is reduced, and the acetate prepared by pretreatment, the rectifying tower and microfiltration reaches the SEMI-C7 standard.
Drawings
FIG. 1 is a schematic view showing the structure of an apparatus for rectifying acetic ester in the example of the present invention;
description of the symbols of the drawings:
1 a pretreatment tower, 2 heat exchangers, 3 a rectifying tower, 4 a reboiler and 5 a microfiltration device.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to the accompanying drawings and specific embodiments.
In the following examples, the information on the raw materials used is shown in tables 1, 2 and 3.
TABLE 1 Industrial n-butyl acetate information
TABLE 2 Industrial propyl acetate information
TABLE 3 technical grade ethyl acetate
| Item | Quality index |
| Chroma (Pt-Co color number)/number | 10 |
| Density (P20, g/cm 3) | 0.902 |
| Ethyl acetate content/m% | 99.8 |
| Water content/m% | 0.04 |
| Free acid (calculated as acetic acid)/m% | 0.003 |
| The evaporation residue is m% | 0.001 |
| Ethanol/m% | 0.05 |
| Ethyl butyl ether/ppm | 6 |
| N-butyl acetate/m% | 0.003 |
| Sulfuric acid test/no | 30 |
| Benzene/ppm | 0.5 |
| Toluene/ppm | 1 |
| Ethylbenzene/ppm | 2 |
| Xylene per ppm | 10 |
Example 1
This example provides an apparatus for rectifying butyl acetate, as shown in fig. 1, the apparatus for rectifying butyl acetate includes: the system comprises a pretreatment tower 1, a heat exchanger 2, a rectifying tower 3, a reboiler 4 and a microfiltration device 5;
the bottom of the pretreatment tower 1 is provided with a raw material inlet; the top of the pretreatment tower 1 is connected with a heat exchanger 2, the heat exchanger 2 is connected with a rectifying tower 3, and the rectifying tower 3 is respectively connected with a reboiler 4 and the microfiltration device 5;
the rectifying tower 1 comprises a main tower A, an auxiliary tower B, a tower top C and a tower bottom D; the main tower is provided with a feed inlet, the auxiliary tower is provided with a discharge outlet, the tower bottom is provided with a feed inlet and an industrial grade acetate byproduct outlet, and the tower top is provided with a gas phase water outlet; the main column and the auxiliary column are separated by a divider;
the heat exchanger 2 is provided with two feed inlets and two discharge outlets, the first feed inlet is communicated with the discharge outlet of the pretreatment tower 1, the second feed inlet is communicated with the gas phase water outlet at the top of the tower C, the first outlet is communicated with the feed inlet of the main tower A, the second outlet is branched into two paths, one path is communicated with the top of the tower C, and the other path is communicated with the industrial grade acetic ester byproduct outlet;
the feed inlet of the microfiltration device 5 is communicated with the discharge outlet at the bottom of the auxiliary tower B and is provided with an acetate discharge outlet.
The number of the theoretical plates of the main tower of the rectifying tower 3 is 11, and the number of the theoretical plates of the auxiliary tower is 5; the distributor of the rectifying tower 3 is made of plastic, the inside of the tower is lined with the plastic, and the plastic is made of F46.
In addition, the embodiment also provides a method for rectifying butyl acetate, which comprises the following steps: firstly, dehydrating industrial grade butyl acetate for 2 hours through a pretreatment tower 1, and performing ceramic coarse filtration; then the pretreated butyl acetate exchanges heat with the heat exchanger 2 to increase the temperature, and then enters the rectifying tower 3 for rectification; and (3) the rectified butyl acetate enters a rectifying tower auxiliary tower B through an in-tower distributor, is cooled to 40 ℃, and then enters a microfiltration device 5 with the specification of 0.05 mu m for filtration to obtain the rectified butyl acetate.
Wherein, the volume ratio of the main tower to the auxiliary tower is 1:0.8; the reflux ratio of the top of the main tower is 0.5, the reboiling ratio of the bottom of the main tower is 4000, and the reflux ratio of the bottom of the auxiliary tower is 0.03; the temperature of the bottom of the main tower is 126.8-127.3 ℃, and the temperature of the top of the main tower is 124.8-125.0 ℃; the temperature of the bottom of the side column is 125.8-126.2 ℃, and the temperature of the top of the side column is 125.0-125.5 ℃.
Example 2
This embodiment provides an apparatus for rectifying propyl acetate, as shown in fig. 1, the apparatus for rectifying propyl acetate includes: the system comprises a pretreatment tower 1, a heat exchanger 2, a rectifying tower 3, a reboiler 4 and a microfiltration device 5;
the bottom of the pretreatment tower 1 is provided with a raw material inlet; the top of the pretreatment tower 1 is connected with a heat exchanger 2, the heat exchanger 2 is connected with a rectifying tower 3, and the rectifying tower 3 is respectively connected with a reboiler 4 and the microfiltration device 5;
the rectifying tower 1 comprises a main tower A, an auxiliary tower B, a tower top C and a tower bottom D; the main tower is provided with a feed inlet, the auxiliary tower is provided with a discharge outlet, the tower bottom is provided with a feed inlet and an industrial grade acetate byproduct outlet, and the tower top is provided with a gas phase water outlet; the main column and the auxiliary column are separated by a divider;
the heat exchanger 2 is provided with two feed inlets and two discharge outlets, the first feed inlet is communicated with the discharge outlet of the pretreatment tower 1, the second feed inlet is communicated with the gas phase water outlet at the top of the tower C, the first outlet is communicated with the feed inlet of the main tower A, the second outlet is branched into two paths, one path is communicated with the top of the tower C, and the other path is communicated with the industrial grade acetic ester byproduct outlet;
the feed inlet of the microfiltration device 5 is communicated with the discharge outlet at the bottom of the auxiliary tower B and is provided with an acetate discharge outlet.
The number of theoretical plates of a main tower of the rectifying tower 3 is 10, and the number of theoretical plates of an auxiliary tower is 5; the distributor of the rectifying tower 3 is made of plastic, the inside of the tower is lined with the plastic, and the plastic is made of F46.
In addition, the embodiment also provides a method for rectifying propyl acetate, which comprises the following steps: firstly, dehydrating industrial-grade propyl acetate for 1.5 hours through a pretreatment tower 1, and performing ceramic coarse filtration; then the pretreated propyl acetate exchanges heat with the heat exchanger 2 to raise the temperature, and then enters a rectifying tower 3 for rectification; and (3) feeding the rectified propyl acetate into a rectifying tower auxiliary tower B through an in-tower distributor, cooling to 40 ℃, and then feeding into a microfiltration device 5 with the specification of 0.05 mu m for filtering to obtain the rectified propyl acetate.
Wherein, the volume ratio of the main tower to the auxiliary tower is 1:1; the reflux ratio of the top of the main tower is 0.7, the reboiling ratio of the bottom of the main tower is 2000, and the reflux ratio of the bottom of the auxiliary tower is 0.05; the temperature of the bottom of the main tower is 101.6-101.9 ℃, and the temperature of the top of the main tower is 100.5-100.8 ℃; the temperature of the bottom of the auxiliary tower is 101.5-101.6 ℃, and the temperature of the top of the auxiliary tower is 100.8-101.2 ℃.
Example 3
This embodiment provides an apparatus for rectifying ethyl acetate, as shown in fig. 1, the apparatus for rectifying ethyl acetate includes: the system comprises a pretreatment tower 1, a heat exchanger 2, a rectifying tower 3, a reboiler 4 and a microfiltration device 5;
the bottom of the pretreatment tower 1 is provided with a raw material inlet; the top of the pretreatment tower 1 is connected with a heat exchanger 2, the heat exchanger 2 is connected with a rectifying tower 3, and the rectifying tower 3 is respectively connected with a reboiler 4 and the microfiltration device 5;
the rectifying tower 1 comprises a main tower A, an auxiliary tower B, a tower top C and a tower bottom D; the main tower is provided with a feed inlet, the auxiliary tower is provided with a discharge outlet, the tower bottom is provided with a feed inlet and an industrial grade acetate byproduct outlet, and the tower top is provided with a gas phase water outlet; the main column and the auxiliary column are separated by a divider;
the heat exchanger 2 is provided with two feed inlets and two discharge outlets, the first feed inlet is communicated with the discharge outlet of the pretreatment tower 1, the second feed inlet is communicated with the gas phase water outlet at the top of the tower C, the first outlet is communicated with the feed inlet of the main tower A, the second outlet is branched into two paths, one path is communicated with the top of the tower C, and the other path is communicated with the industrial grade acetic ester byproduct outlet;
the feed inlet of the microfiltration device 5 is communicated with the discharge outlet at the bottom of the auxiliary tower B and is provided with an acetate discharge outlet.
The number of the theoretical plates of the main tower of the rectifying tower 3 is 6, and the number of the theoretical plates of the auxiliary tower is 3; the distributor of the rectifying tower 3 is made of plastic, the inside of the tower is lined with the plastic, and the plastic is made of F46.
In addition, the embodiment also provides a method for rectifying ethyl acetate, which comprises the following steps: firstly, dehydrating industrial ethyl acetate for 1 hour through a pretreatment tower 1, and performing ceramic coarse filtration; then the pretreated ethyl acetate exchanges heat with the heat exchanger 2 to raise the temperature, and then enters a rectifying tower 3 for rectification; and (3) feeding the rectified ethyl acetate into a rectifying tower auxiliary tower B through an in-tower distributor, cooling to 35 ℃, and then feeding into a microfiltration device 5 with the specification of 0.05 mu m for filtration to obtain the rectified ethyl acetate.
Wherein, the volume ratio of the main tower to the auxiliary tower is 1:0.3. the reflux ratio of the top of the main tower is 0.6, the reboiling ratio of the bottom of the main tower is 500, and the reflux ratio of the bottom of the auxiliary tower is 0.03; the temperature of the bottom of the main tower is 77.8-78.1 ℃, and the temperature of the top of the main tower is 76.5-76.7 ℃; the temperature of the bottom of the auxiliary tower is 77.6-77.9 ℃, and the temperature of the top of the auxiliary tower is 76.7-77.0 ℃.
Example 4
This embodiment provides an apparatus for rectifying ethyl acetate, as shown in fig. 1, the apparatus for rectifying ethyl acetate includes: the system comprises a pretreatment tower 1, a heat exchanger 2, a rectifying tower 3, a reboiler 4 and a microfiltration device 5;
the bottom of the pretreatment tower 1 is provided with a raw material inlet; the top of the pretreatment tower 1 is connected with a heat exchanger 2, the heat exchanger 2 is connected with a rectifying tower 3, and the rectifying tower 3 is respectively connected with a reboiler 4 and the microfiltration device 5;
the rectifying tower 1 comprises a main tower A, an auxiliary tower B, a tower top C and a tower bottom D; the main tower is provided with a feed inlet, the auxiliary tower is provided with a discharge outlet, the tower bottom is provided with a feed inlet and an industrial grade acetate byproduct outlet, and the tower top is provided with a gas phase water outlet; the main column and the auxiliary column are separated by a divider;
the heat exchanger 2 is provided with two feed inlets and two discharge outlets, the first feed inlet is communicated with the discharge outlet of the pretreatment tower 1, the second feed inlet is communicated with the gas phase water outlet at the top of the tower C, the first outlet is communicated with the feed inlet of the main tower A, the second outlet is branched into two paths, one path is communicated with the top of the tower C, and the other path is communicated with the industrial grade acetic ester byproduct outlet;
the feed inlet of the microfiltration device 5 is communicated with the discharge outlet at the bottom of the auxiliary tower B and is provided with an acetate discharge outlet.
The number of the theoretical plates of the main tower of the rectifying tower 3 is 6, and the number of the theoretical plates of the auxiliary tower is 3; the distributor of the rectifying tower 3 is made of plastic, the inside of the tower is lined with the plastic, and the plastic is made of F46.
In addition, the embodiment also provides a method for rectifying ethyl acetate, which comprises the following steps: firstly, dehydrating industrial ethyl acetate for 2 hours through a pretreatment tower 1, and performing ceramic coarse filtration; then the pretreated ethyl acetate exchanges heat with the heat exchanger 2 to raise the temperature, and then enters a rectifying tower 3 for rectification; and (3) feeding the rectified ethyl acetate into a rectifying tower auxiliary tower B through an in-tower distributor, cooling to 35 ℃, and then feeding into a microfiltration device 5 with the specification of 0.05 mu m for filtering to obtain the rectified ethyl acetate.
Wherein, the volume ratio of the main tower to the auxiliary tower is 1:0.5. the reflux ratio of the top of the main tower is 0.6, the reboiling ratio of the bottom of the main tower is 100, and the reflux ratio of the bottom of the auxiliary tower is 0.03; the temperature of the bottom of the main tower is 77.8-78.1 ℃, and the temperature of the top of the main tower is 76.5-76.7 ℃; the temperature of the bottom of the auxiliary tower is 77.6-77.9 ℃, and the temperature of the top of the auxiliary tower is 76.7-77.0 ℃.
Example 5
This embodiment provides an apparatus for rectifying ethyl acetate, as shown in fig. 1, the apparatus for rectifying ethyl acetate includes: the system comprises a pretreatment tower 1, a heat exchanger 2, a rectifying tower 3, a reboiler 4 and a microfiltration device 5;
the bottom of the pretreatment tower 1 is provided with a raw material inlet; the top of the pretreatment tower 1 is connected with a heat exchanger 2, the heat exchanger 2 is connected with a rectifying tower 3, and the rectifying tower 3 is respectively connected with a reboiler 4 and the microfiltration device 5;
the rectifying tower 1 comprises a main tower A, an auxiliary tower B, a tower top C and a tower bottom D; the main tower is provided with a feed inlet, the auxiliary tower is provided with a discharge outlet, the tower bottom is provided with a feed inlet and an industrial grade acetate byproduct outlet, and the tower top is provided with a gas phase water outlet; the main column and the auxiliary column are separated by a divider;
the heat exchanger 2 is provided with two feed inlets and two discharge outlets, the first feed inlet is communicated with the discharge outlet of the pretreatment tower 1, the second feed inlet is communicated with the gas phase water outlet at the tower top C, the first outlet is communicated with the feed inlet of the main tower A, the second outlet is branched into two paths, one path is communicated with the tower top C, and the other path is communicated with the industrial grade acetate byproduct outlet;
the feed inlet of the microfiltration device 5 is communicated with the discharge outlet at the bottom of the auxiliary tower B and is provided with an acetate discharge outlet.
The number of the theoretical plates of the main tower of the rectifying tower 3 is 6, and the number of the theoretical plates of the auxiliary tower is 3; the distributor of the rectifying tower 3 is made of plastic, the inside of the tower is lined with the plastic, and the plastic is made of F46.
In addition, the embodiment also provides a method for rectifying ethyl acetate, which comprises the following steps: firstly, dehydrating industrial ethyl acetate for 2 hours through a pretreatment tower 1, and performing ceramic coarse filtration; then the pretreated ethyl acetate exchanges heat with the heat exchanger 2 to raise the temperature, and then enters a rectifying tower 3 for rectification; and (3) the rectified ethyl acetate enters a rectifying tower secondary tower B through an in-tower distributor, is cooled to 40 ℃, and then enters a microfiltration device 5 with the specification of 0.05 mu m for filtration to obtain the rectified ethyl acetate.
Wherein, the volume ratio of the main tower to the auxiliary tower is 1:0.5. the reflux ratio of the top of the main tower is 0.6, the reboiling ratio of the bottom of the main tower is 500, and the reflux ratio of the bottom of the auxiliary tower is 0.03; the temperature of the bottom of the main tower is 77.8-78.1 ℃, and the temperature of the top of the main tower is 76.5-76.7 ℃; the temperature of the bottom of the auxiliary tower is 77.6-77.9 ℃, and the temperature of the top of the auxiliary tower is 76.7-77.0 ℃.
Example 6
This embodiment provides an apparatus for rectifying butyl acetate, as shown in fig. 1, the apparatus for rectifying butyl acetate includes: the system comprises a pretreatment tower 1, a heat exchanger 2, a rectifying tower 3, a reboiler 4 and a microfiltration device 5;
the bottom of the pretreatment tower 1 is provided with a raw material inlet; the top of the pretreatment tower 1 is connected with a heat exchanger 2, the heat exchanger 2 is connected with a rectifying tower 3, and the rectifying tower 3 is respectively connected with a reboiler 4 and the microfiltration device 5;
the rectifying tower 1 comprises a main tower A, an auxiliary tower B, a tower top C and a tower bottom D; the main tower is provided with a feed inlet, the auxiliary tower is provided with a discharge outlet, the tower bottom is provided with a feed inlet and an industrial grade acetate byproduct outlet, and the tower top is provided with a gas phase water outlet; the main column and the auxiliary column are separated by a divider;
the heat exchanger 2 is provided with two feed inlets and two discharge outlets, the first feed inlet is communicated with the discharge outlet of the pretreatment tower 1, the second feed inlet is communicated with the gas phase water outlet at the top of the tower C, the first outlet is communicated with the feed inlet of the main tower A, the second outlet is branched into two paths, one path is communicated with the top of the tower C, and the other path is communicated with the industrial grade acetic ester byproduct outlet;
the feed inlet of the microfiltration device 5 is communicated with the discharge outlet at the bottom of the auxiliary tower B and is provided with an acetate discharge outlet.
The number of the theoretical plates of the main tower of the rectifying tower 3 is 11, and the number of the theoretical plates of the auxiliary tower is 5; the distributor of the rectifying tower 3 is made of plastic, the inside of the tower is lined with the plastic, and the plastic is made of F46.
In addition, the embodiment also provides a method for rectifying butyl acetate, which comprises the following steps: firstly, dehydrating industrial grade butyl acetate for 2 hours through a pretreatment tower 1, and performing ceramic coarse filtration; then the pretreated butyl acetate exchanges heat with the heat exchanger 2 to raise the temperature, and then enters the rectifying tower 3 for rectification; and (3) the rectified butyl acetate enters a rectifying tower auxiliary tower B through an in-tower distributor, is cooled to 40 ℃, and then enters a microfiltration device 5 with the specification of 0.05 mu m for filtration to obtain the rectified butyl acetate.
Wherein, the volume ratio of the main tower to the auxiliary tower is 1:0.5; the reflux ratio of the top of the main tower is 0.5, the reboiling ratio of the bottom of the main tower is 10000, and the reflux ratio of the bottom of the auxiliary tower is 0.03; the temperature of the bottom of the main tower is 126.8-127.3 ℃, and the temperature of the top of the main tower is 124.8-125.0 ℃; the temperature of the bottom of the side column is 125.8-126.2 ℃, and the temperature of the top of the side column is 125.0-125.5 ℃.
Example 7
This embodiment provides an apparatus for rectifying butyl acetate, as shown in fig. 1, the apparatus for rectifying butyl acetate includes: the system comprises a pretreatment tower 1, a heat exchanger 2, a rectifying tower 3, a reboiler 4 and a microfiltration device 5;
the bottom of the pretreatment tower 1 is provided with a raw material inlet; the top of the pretreatment tower 1 is connected with a heat exchanger 2, the heat exchanger 2 is connected with a rectifying tower 3, and the rectifying tower 3 is respectively connected with a reboiler 4 and the microfiltration device 5;
the rectifying tower 1 comprises a main tower A, an auxiliary tower B, a tower top C and a tower bottom D; the main tower is provided with a feed inlet, the auxiliary tower is provided with a discharge outlet, the tower bottom is provided with a feed inlet and an industrial grade acetate byproduct outlet, and the tower top is provided with a gas phase water outlet; the main column and the auxiliary column are separated by a divider;
the heat exchanger 2 is provided with two feed inlets and two discharge outlets, the first feed inlet is communicated with the discharge outlet of the pretreatment tower 1, the second feed inlet is communicated with the gas phase water outlet at the top of the tower C, the first outlet is communicated with the feed inlet of the main tower A, the second outlet is branched into two paths, one path is communicated with the top of the tower C, and the other path is communicated with the industrial grade acetic ester byproduct outlet;
the feed inlet of the microfiltration device 5 is communicated with the discharge outlet at the bottom of the auxiliary tower B and is provided with an acetate discharge outlet.
The number of the theoretical plates of the main tower of the rectifying tower 3 is 11, and the number of the theoretical plates of the auxiliary tower is 5; the distributor of the rectifying tower 3 is made of plastic, the inside of the tower is lined with the plastic, and the plastic is made of F46.
In addition, the embodiment also provides a method for rectifying butyl acetate, which comprises the following steps: firstly, dehydrating industrial grade butyl acetate for 2 hours through a pretreatment tower 1, and performing ceramic coarse filtration; then the pretreated butyl acetate exchanges heat with the heat exchanger 2 to raise the temperature, and then enters the rectifying tower 3 for rectification; and (3) the rectified butyl acetate enters a rectifying tower auxiliary tower B through an in-tower distributor, is cooled to 40 ℃, and then enters a microfiltration device 5 with the specification of 0.05 mu m for filtration to obtain the rectified butyl acetate.
Wherein, the volume ratio of the main tower to the auxiliary tower is 1:0.3; the reflux ratio of the top of the main tower is 0.1, the reboiling ratio of the bottom of the main tower is 4000, and the reflux ratio of the bottom of the auxiliary tower is 0.03; the temperature of the bottom of the main tower is 126.8-127.3 ℃, and the temperature of the top of the main tower is 124.8-125.0 ℃; the temperature of the bottom of the side column is 125.8-126.2 ℃, and the temperature of the top of the side column is 125.0-125.5 ℃.
Example 8
This example provides an apparatus for rectifying propyl acetate, as shown in fig. 1, the apparatus for rectifying acetic ester includes: the system comprises a pretreatment tower 1, a heat exchanger 2, a rectifying tower 3, a reboiler 4 and a microfiltration device 5;
the bottom of the pretreatment tower 1 is provided with a raw material inlet; the top of the pretreatment tower 1 is connected with a heat exchanger 2, the heat exchanger 2 is connected with a rectifying tower 3, and the rectifying tower 3 is respectively connected with a reboiler 4 and the microfiltration device 5;
the rectifying tower 1 comprises a main tower A, an auxiliary tower B, a tower top C and a tower bottom D; the main tower is provided with a feed inlet, the auxiliary tower is provided with a discharge outlet, the tower bottom is provided with a feed inlet and an industrial-grade acetate byproduct outlet, and the tower top is provided with a gas-phase water outlet; the main column and the auxiliary column are separated by a divider;
the heat exchanger 2 is provided with two feed inlets and two discharge outlets, the first feed inlet is communicated with the discharge outlet of the pretreatment tower 1, the second feed inlet is communicated with the gas phase water outlet at the top of the tower C, the first outlet is communicated with the feed inlet of the main tower A, the second outlet is branched into two paths, one path is communicated with the top of the tower C, and the other path is communicated with the industrial grade acetic ester byproduct outlet;
the feed inlet of the microfiltration device 5 is communicated with the discharge outlet at the bottom of the auxiliary tower B and is provided with an acetate discharge outlet.
The number of the main tower theoretical plates of the rectifying tower 3 is 10, and the number of the auxiliary tower theoretical plates is 5; the distributor of the rectifying tower 3 is made of plastic, the inside of the tower is lined with the plastic, and the plastic is made of F46.
In addition, the embodiment also provides a method for rectifying propyl acetate, which comprises the following steps: firstly, dehydrating industrial-grade propyl acetate for 1.5 hours through a pretreatment tower 1, and performing ceramic coarse filtration; then the pretreated propyl acetate exchanges heat with the heat exchanger 2 to raise the temperature, and then enters the rectifying tower 3 for rectification; and (3) the rectified propyl acetate enters a rectifying tower auxiliary tower B through an in-tower distributor, and is cooled to 35 ℃ and then enters a microfiltration device 5 with the specification of 0.05 mu m for filtration to obtain the rectified propyl acetate.
Wherein, the volume ratio of the main tower to the auxiliary tower is 1:1; the reflux ratio of the top of the main tower is 10, the reboiling ratio of the bottom of the main tower is 2000, and the reflux ratio of the bottom of the auxiliary tower is 0.05; the temperature of the bottom of the main tower is 101.6-101.9 ℃, and the temperature of the top of the main tower is 100.5-100.8 ℃; the temperature of the bottom of the auxiliary tower is 101.5-101.6 ℃, and the temperature of the top of the auxiliary tower is 100.8-101.2 ℃.
The acetic acid esters prepared in examples 1 to 8 were measured for purity, moisture, chromaticity and metal ions by GB/T27563-2011, ICP-MS, GB/T6283-2008, and Table 4 shows the results.
TABLE 4
Note that d.l. is the detection limit of ICP-MS used in the experiment, making all detection limits below 10ppb, where < d.l. is used when below the detection limit of the apparatus.
As can be seen from Table 1, the purity of the acetate produced by the method for rectifying the acetate reaches the SEMI-C7 standard, and the energy consumption of the process is reduced by over 30 percent.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (4)
1. A method for rectifying acetic ester is characterized in that a device for rectifying the acetic ester is adopted for rectification, and the method comprises the following steps: firstly, passing industrial-grade acetate through a pretreatment tower; then the pretreated acetate exchanges heat with a heat exchanger to raise the temperature, and then enters a rectifying tower for rectification; the rectified acetate enters a rectifying tower auxiliary tower through an in-tower distributor, and enters a microfiltration device after being cooled to be filtered to obtain electronic grade acetate; the acetate is one of ethyl acetate, propyl acetate or butyl acetate; the device for rectifying the acetate comprises a pretreatment tower, a heat exchanger, a rectifying tower, a reboiler and a microfiltration device;
a raw material feeding hole is formed in the bottom of the pretreatment tower; the top of the pretreatment tower is connected with a heat exchanger, the heat exchanger is connected with a rectifying tower, and the rectifying tower is respectively connected with the reboiler and the microfiltration device; the rectifying tower comprises a main tower, an auxiliary tower, a tower bottom and a tower top; the main tower is provided with a feed inlet, the auxiliary tower is provided with a discharge outlet, the tower bottom is provided with a feed inlet and an industrial grade acetate byproduct outlet, and the tower top is provided with a gas phase water outlet; the main column and the auxiliary column are separated by a divider; the heat exchanger is provided with two feed inlets and two discharge outlets, the first feed inlet is communicated with the discharge outlet of the pretreatment tower, the second feed inlet is communicated with the gas phase water outlet at the top of the tower, the first outlet is communicated with the feed inlet of the main tower, the second outlet is branched into two paths, one path is communicated with the top of the tower, and the other path is communicated with the industrial grade acetate byproduct outlet; the feed inlet of the microfiltration device is communicated with the discharge outlet at the bottom of the auxiliary tower and is provided with an acetate discharge outlet;
the volume ratio of the main tower to the auxiliary tower of the rectifying tower is 1:0.8-1:1; the reflux ratio of the top of the main tower is 0.1-10, the reflux ratio of the bottom of the main tower is 100-10000, and the reflux ratio of the bottom of the auxiliary tower is 0-1; the butyl acetate rectification conditions are as follows: the temperature of the bottom of the main tower is 124.5-128 ℃, the temperature of the top of the main tower is 123.5-125.4 ℃, the temperature of the bottom of the auxiliary tower is 125.5-128 ℃, and the temperature of the top of the auxiliary tower is 124-125.5 ℃; the propyl acetate rectification conditions are as follows: the temperature of the bottom of the main tower is 101-102.9 ℃, the temperature of the top of the main tower is 99.5-101.5 ℃, the temperature of the bottom of the auxiliary tower is 101-102.9 ℃, and the temperature of the top of the auxiliary tower is 100.5-101.5 ℃; the ethyl acetate rectification conditions are as follows: the temperature of the bottom of the main tower is 76-78.5 ℃, the temperature of the top of the main tower is 75-77.5 ℃, the temperature of the bottom of the auxiliary tower is 76-78.5 ℃, and the temperature of the top of the auxiliary tower is 75-78 ℃.
2. The method for rectifying acetic ester according to claim 1, wherein the number of theoretical plates of the main column of the rectifying column is 6 or more, and the number of theoretical plates of the subsidiary column is 3 or more.
3. The method for rectifying acetic ester according to claim 1, wherein the rectifying tower distributor is made of plastic, and the tower is lined with the plastic.
4. The process for the rectification of acetic ester according to claim 1 wherein the reflux ratio at the top of the main column is from 0.5 to 0.7 and the reflux ratio at the bottom of the main column is from 500 to 4000.
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