CN111643918A - Rectification purification device and purification method for multi-component material - Google Patents
Rectification purification device and purification method for multi-component material Download PDFInfo
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- CN111643918A CN111643918A CN202010548874.6A CN202010548874A CN111643918A CN 111643918 A CN111643918 A CN 111643918A CN 202010548874 A CN202010548874 A CN 202010548874A CN 111643918 A CN111643918 A CN 111643918A
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- B01D3/14—Fractional distillation or use of a fractionation or rectification column
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Abstract
The invention relates to a rectification purification device and a purification method for a multi-component material. A rectification purification device for multi-component materials is characterized by comprising a heating tower kettle and at least two rectification towers, wherein a gas phase outlet of the heating tower kettle is simultaneously connected with a tower bottom reflux port of each rectification tower; the tower bottom liquid outlet of the rectifying tower is connected with the heating tower kettle through a pipeline; the top gas phase extraction outlet of the rectifying tower is connected with the inlet of the condenser, the top reflux port of the rectifying tower is provided with a reflux pipe, and the outlet of the condenser is communicated with the reflux pipe at the top of the rectifying tower through a pipeline. And provides a corresponding purification method. The invention provides a method and a device suitable for rectifying and purifying high-purity medical bodies, which not only can obtain products with higher purity, but also can effectively solve the problem of low single product yield in the traditional intermittent rectification operation process in the medical industry, and improve the single product yield.
Description
Technical Field
The invention relates to a rectification purification device and a purification method for a multi-component material, and belongs to the technical field of rectification tower purification.
Background
The product separation and purification type rectification project in the pharmaceutical industry at present usually adopts a single-tower intermittent rectification mode, namely, various components in the material to be processed are separated by a rectification tower, and finally front fraction, qualified products, transition fraction and the like are sequentially extracted from the top of the tower, and a large amount of replacement is needed in the process of extracting high-purity products, so that the operation and treatment time is long, the transition fraction yield is high, and the single yield of the qualified products is low.
Disclosure of Invention
The invention provides a rectification purification device and a purification method for multi-component materials, aiming at the problems in the existing treatment process.
The technical scheme for solving the technical problems is as follows: a rectification purification device for multi-component materials is characterized by comprising a heating tower kettle and at least two rectification towers, wherein a gas phase outlet of the heating tower kettle is simultaneously connected with a tower bottom reflux port of each rectification tower; the tower bottom liquid outlet of the rectifying tower is connected with the heating tower kettle through a pipeline; the top gas phase extraction outlet of the rectifying tower is connected with the inlet of the condenser, the top reflux port of the rectifying tower is provided with a reflux pipe, and the outlet of the condenser is communicated with the reflux pipe at the top of the rectifying tower through a pipeline. A loop is formed between each rectifying tower and the heating tower kettle, each rectifying tower shares one heating tower kettle, and the rectifying towers connected with the gas phase outlets of the heating tower kettles can be switched as required, so that the substances separated by the rectifying towers are different.
On the basis of the technical scheme, in order to achieve the convenience of use and the stability of equipment, the invention can also make the following improvements on the technical scheme:
furthermore, a switching valve is arranged between the rectifying towers of the heating tower kettle. The switching valve is used for realizing which rectifying tower the gas phase outlet of the heating tower kettle is connected with.
Furthermore, a main pipeline is arranged at a gas phase outlet of the heating tower kettle, a reflux port at the bottom of each rectifying tower is communicated with the main pipeline through auxiliary management, and a switch valve is arranged on the auxiliary pipeline. The gas phase outlet of the heating tower kettle is controlled to be connected with which rectifying tower by controlling the on-off of the switch valve on the auxiliary pipeline.
Furthermore, the number of the rectifying towers is two.
Furthermore, the heating tower kettle is of a sinking structure.
Furthermore, the condenser can adopt a one-stage condensation mode or a multi-stage condensation mode.
Meanwhile, the rectification purification device for the multi-component material is combined, and a purification method is provided:
a rectification purification method for multicomponent materials is characterized in that one of at least two rectification towers is a main tower, a condenser matched with the main tower is a main tower condenser, the other rectification towers are auxiliary towers, and the condenser matched with the auxiliary towers is an auxiliary tower condenser;
adding the multi-component material to be separated into the heating tower kettle at one time, heating the material in the heating tower kettle by heating medium such as low-pressure steam or heat-conducting oil, etc. to realize vaporization of the material, selecting the material to enter the main tower or the auxiliary tower according to different boiling points of the components in the material,
when the boiling point of the impurity fraction in the material to be treated is lower than that of the main product, the gas phase obtained after the vaporization of the material in the heating tower kettle firstly enters an auxiliary tower, and the gas phase extracted from the top of the auxiliary tower is cooled by an auxiliary tower condenser, and then part of the gas phase flows back and part of the gas phase is extracted as front fraction impurities;
when the impurity content of the front fraction in the heating tower kettle reaches a set value, switching the rectifying tower to communicate the main tower heating tower kettle, cooling the gas phase extracted from the top of the main tower by a main tower condenser, partially refluxing to the main tower, and partially extracting the gas phase as a qualified product;
and (3) with the gradual reduction of the concentration of the product in the heating tower kettle, switching to the auxiliary tower again to extract the transition fraction when the qualified product cannot be extracted from the top of the main tower, stopping heating when the product does not exist in the heating tower kettle, and discharging the residual kettle liquid in the heating tower kettle to finish single-batch operation.
The method is used for rectifying, separating and purifying the high-purity medical intermediate.
The invention has the advantages that: the invention provides a method and a device suitable for rectifying and purifying high-purity medical bodies, which can not only obtain products with higher purity, but also effectively solve the problem of low single product yield in the traditional intermittent rectification operation process in the medical industry and improve the single product yield; the process of a large amount of replacement in the rectifying tower in the process of extracting different components by rectifying separation and the liquid holdup of the tower kettle at the later stage of rectification are reduced, the single-batch rectification efficiency is improved, and the product yield in the single-batch rectification separation process is improved.
Drawings
FIG. 1 is a schematic diagram of a distillation purification apparatus for multi-component materials according to the present application.
The reference numbers are recorded as follows: 1-1, a main column; 1-2, a main column condenser; 2-1, auxiliary tower; 2-2, auxiliary tower condenser; 3-1, heating the tower kettle.
Detailed Description
The principles and features of this invention are described below in conjunction with the following drawings, which are set forth by way of illustration only and are not intended to limit the scope of the invention.
A rectification purification device (see figure 1) for multi-component materials comprises a heating tower kettle 3-1 and at least two rectification towers, wherein two rectification towers are taken as examples in the application, a gas phase outlet of the heating tower kettle 3-1 is simultaneously connected with a tower bottom reflux port of each rectification tower, and the heating tower kettle 3-1 is of a sinking structure; the tower bottom liquid outlet of the rectifying tower is connected with a heating tower kettle 3-1 through a pipeline; the top gas phase extraction outlet of the rectifying tower is connected with the inlet of the condenser, the top reflux port of the rectifying tower is provided with a reflux pipe, and the outlet of the condenser is communicated with the reflux pipe at the top of the rectifying tower through a pipeline;
a switching valve is arranged between the rectifying towers of the heating tower kettle 3-1; the gas phase outlet of the heating tower kettle is provided with a main pipeline, the tower bottom return ports of the rectifying towers are communicated with the main pipeline through auxiliary management, and the auxiliary pipeline is provided with a switch valve;
the condenser can be one-stage condensation, two-stage condensation or multi-stage condensation.
On the basis of the rectification purification device for the multi-component material, a specific use method of the device is provided:
a method for rectifying and purifying multicomponent materials is characterized in that one of at least two rectifying towers is a main tower 1-1, a condenser matched with the main tower 1-1 is a main tower condenser 1-2, the other rectifying towers are auxiliary towers 2-1, and a condenser matched with the auxiliary towers 2-1 is an auxiliary tower condenser 2-2;
adding the multi-component material to be separated into the heating tower kettle 3-1 at one time, heating the material in the heating tower kettle 3-1 by heating medium such as low-pressure steam or heat-conducting oil, etc. to realize vaporization of the material, selecting the material to enter the main tower 1-1 or the auxiliary tower 2-1 according to different boiling points of the components in the material,
when the boiling point of the impurity fraction in the material to be processed is lower than that of the main product, the gas phase obtained after the vaporization of the material in the heating tower kettle 3-1 firstly enters the auxiliary tower 2-1, and the gas phase extracted from the top of the auxiliary tower 2-1 is cooled by the auxiliary tower condenser 2-2, part of the gas phase flows back, and part of the gas phase is extracted as front fraction impurities;
when the impurity content of the front fraction in the heating tower kettle 3-1 reaches a set value, switching the rectifying tower to connect the heating tower kettle 3-1 of the main tower 1-1, cooling the gas phase extracted from the top of the main tower 1-1 through a main tower condenser 1-2, returning part of the gas phase to the main tower 1-1, and extracting part of the gas phase as a qualified product;
with the gradual reduction of the product concentration in the heating tower kettle 3-1, when the top of the main tower 1-1 can not extract qualified products, switching to the auxiliary tower 2-1 again to extract transition fractions, when the heating tower kettle 3-1 does not contain the products, stopping heating, and discharging the residual kettle liquid in the heating tower kettle 3-1 to finish the single batch operation.
Is used for rectifying, separating and purifying high-purity medical intermediates.
When the boiling point of the impurity fraction in the material to be treated is higher than that of the main product, the opening modes of the method can be reversed, namely, the main tower is firstly used, and then the auxiliary tower is used.
The device can adopt the design of single cauldron multicolumn according to material component kind, adopts one set of tower cauldron to heat promptly, and wherein the heating tower cauldron adopts formula structural design that sinks, can effectively reduce tower cauldron holdup, and different fraction products are respectively extracted to the different rectifying column of two tower structures make full use of, reduce the replacement of each tower switching in-process tower holdup, improve the single yield of rectification separation efficiency and qualified product.
In this embodiment, two specific implementation cases are also provided to prove the effectiveness of the scheme of the present application:
case one
A certain medical intermediate is separated and purified, the treatment capacity is 7 t/batch, the medical intermediate is treated in 8 hours, the front fraction content is 13%, the main product content is 75%, the rear fraction content is 12%, the boiling point difference between the front fraction and the main product is 14 ℃, the theoretical plate number of a rectifying tower required in the separation process is high, the reflux ratio in the operation process is high, if single-tower rectifying separation is adopted, the required rectifying tower is phi 1.0m multiplied by 25m, the single-kettle double-tower technology of the scheme is adopted, the required main tower is phi 700mm multiplied by 25m, and the auxiliary tower is phi 600mm multiplied by 15m, compared with the single-tower rectifying technology, although the equipment investment is slightly improved, the operation energy consumption of the ton product after the operation process of the scheme can be saved by 20-25%, the yield of a single-batch product can be improved to about 85% from about 60%, and the submerged single-kettle double-tower structure of the scheme can effectively improve the rectifying efficiency by comprehensively considering, the method is particularly suitable for the working conditions of low single batch treatment capacity, high product separation requirement and high product yield requirement in the pharmaceutical industry.
Case two
The purification project of the pharmaceutical intermediate sevoflurane has the treatment capacity of 5 t/batch, the purification project is finished after 8 hours of treatment, the impurity content of the front fraction is 26%, the main product content is 58%, the impurity content of the back fraction is 16%, if single-tower rectification separation is adopted, the required rectification tower is phi 1.2m multiplied by 23m, and the single-kettle double-tower technology of the scheme is adopted, the required main tower is phi 800mm multiplied by 23m, and the auxiliary tower is phi 700mm multiplied by 12 m.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (7)
1. A rectification purification device for multi-component materials is characterized by comprising a heating tower kettle (3-1) and at least two rectification towers, wherein a gas phase outlet of the heating tower kettle (3-1) is simultaneously connected with a tower bottom reflux port of each rectification tower; the tower bottom liquid outlet of the rectifying tower is connected with the heating tower kettle (3-1) through a pipeline; the top gas phase extraction outlet of the rectifying tower is connected with the inlet of the condenser, the top reflux port of the rectifying tower is provided with a reflux pipe, and the outlet of the condenser is communicated with the reflux pipe at the top of the rectifying tower through a pipeline.
2. The apparatus for the extractive distillation purification of a multicomponent material according to claim 1, wherein a switching valve is provided between the rectifying towers of the heating tower (3-1).
3. The apparatus according to claim 1, wherein a main pipeline is provided at the gas phase outlet of the heating tower, the main pipeline is connected to the bottom reflux port of each distillation tower through a secondary management, and a switch valve is provided on the secondary pipeline.
4. The apparatus of claim 1, wherein there are two distillation columns.
5. The apparatus for the extractive distillation purification of a multicomponent material according to claim 1, wherein the heating column bottom (3-1) has a sinking structure.
6. The apparatus of claim 1, wherein the condenser is one-stage or multi-stage.
7. A rectification purification method for multi-component materials is characterized in that the rectification purification device for multi-component materials in any claim 1 to 5 is used, one of the at least two rectification towers is a main tower (1-1), a condenser matched with the main tower (1-1) is a main tower condenser (1-2), the other rectification towers are auxiliary towers (2-1), and a condenser matched with the auxiliary towers (2-1) is an auxiliary tower condenser (2-2);
multi-component materials to be separated are added into a heating tower kettle (3-1) at one time, the materials in the heating tower kettle (3-1) are heated by heating media such as low-pressure steam or heat-conducting oil, so as to realize the vaporization of the materials, the materials are selected to enter a main tower (1-1) or an auxiliary tower (2-1) according to the different boiling points of the components in the materials,
when the boiling point of the impurity fraction in the material to be treated is lower than that of the main product, the gas phase obtained after the vaporization of the material in the heating tower kettle (3-1) firstly enters an auxiliary tower (2-1), and the gas phase extracted from the top of the auxiliary tower (2-1) is cooled by an auxiliary tower condenser (2-2), part of the gas phase flows back, and part of the gas phase is extracted as front fraction impurities;
when the impurity content of the front fraction in the heating tower kettle (3-1) reaches a set value, switching the rectifying tower to connect the heating tower kettle (3-1) of the main tower (1-1), cooling the gas phase extracted from the top of the main tower (1-1) by a main tower condenser (1-2), partially refluxing to the main tower (1-1), and partially extracting the gas phase as a qualified product;
with the gradual reduction of the product concentration in the heating tower kettle (3-1), when the top of the main tower (1-1) can not extract qualified products, switching to the auxiliary tower (2-1) again to extract transition fractions, when the heating tower kettle (3-1) does not contain the products, stopping heating, and discharging residual kettle liquid in the heating tower kettle (3-1) to finish single-batch operation.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113956137A (en) * | 2021-11-24 | 2022-01-21 | 衢州建华南杭药业有限公司 | Preparation method for alcohol head polymerization purification |
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| US6045661A (en) * | 1998-05-20 | 2000-04-04 | Phillips Petroleum Company | Process and apparatus for recovering diluent, monomer, and comonomer from a polymerization reactor effluent |
| CN102701960A (en) * | 2012-05-22 | 2012-10-03 | 天津大学 | Method and device for refining crude products of m-phthaloyl chloride |
| CN103087094A (en) * | 2013-01-30 | 2013-05-08 | 天津大学 | Method and device for rectifying and purifying triethyl phosphate in batches |
| CN108147942A (en) * | 2018-01-22 | 2018-06-12 | 广州赫尔普化工有限公司 | A kind of hexane oil combined production device and the production method using the combined production device |
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Patent Citations (5)
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| US6045661A (en) * | 1998-05-20 | 2000-04-04 | Phillips Petroleum Company | Process and apparatus for recovering diluent, monomer, and comonomer from a polymerization reactor effluent |
| JP2000044967A (en) * | 1998-08-03 | 2000-02-15 | Jgc Corp | Process for treating petroleum and apparatus therefor |
| CN102701960A (en) * | 2012-05-22 | 2012-10-03 | 天津大学 | Method and device for refining crude products of m-phthaloyl chloride |
| CN103087094A (en) * | 2013-01-30 | 2013-05-08 | 天津大学 | Method and device for rectifying and purifying triethyl phosphate in batches |
| CN108147942A (en) * | 2018-01-22 | 2018-06-12 | 广州赫尔普化工有限公司 | A kind of hexane oil combined production device and the production method using the combined production device |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113956137A (en) * | 2021-11-24 | 2022-01-21 | 衢州建华南杭药业有限公司 | Preparation method for alcohol head polymerization purification |
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Application publication date: 20200911 |