CN117732097A - Separation method - Google Patents
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- CN117732097A CN117732097A CN202311489980.1A CN202311489980A CN117732097A CN 117732097 A CN117732097 A CN 117732097A CN 202311489980 A CN202311489980 A CN 202311489980A CN 117732097 A CN117732097 A CN 117732097A
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- RBACIKXCRWGCBB-UHFFFAOYSA-N 1,2-Epoxybutane Chemical compound CCC1CO1 RBACIKXCRWGCBB-UHFFFAOYSA-N 0.000 description 31
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Landscapes
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The invention provides a separation method, which adopts a coupling refining unit with an extraction section, a low-boiling product condensation section, a low-boiling impurity rectification section, a low-boiling impurity stripping section, a product stripping section and a product rectification section as a separator, and comprises the following steps: allowing the to-be-separated matter and the extractant to enter an extraction section for extraction treatment; the extract liquid goes down to a low-boiling impurity stripping section for the first stripping treatment; the first stripping liquid goes downwards to enter a product stripping section for second stripping treatment, and part of second stripping gas goes upwards to enter a low-boiling impurity stripping section to participate in the first stripping treatment; the first distilled gas goes upward to enter a low-boiling product condensing section for condensation treatment, and the remaining second distilled gas goes upward to enter a product rectifying section for second rectification treatment; and introducing the second rectifying gas into a product condensation and separation unit outside the separator to perform product condensation and separation treatment to obtain a liquid-phase product. The method can uniformly carry out extraction, rectification and stripping, effectively reduces energy consumption and cost, and is easy for industrialization.
Description
Technical Field
The invention belongs to the technical field of production separation and purification, and particularly relates to a separation method.
Background
The epoxybutane, also called epoxybutene, is a substance with a three-membered ring structure, has active chemical properties, is an important organic synthesis raw material and an organic synthesis intermediate, is mainly used as an intermediate of a polyase polyol monomer and other synthetic materials, can be used as a stabilizer of chloride, foamed plastic, synthetic rubber, a nonionic surfactant and the like, and can also be used as a diluent of nitrolacquer instead of acetone, and can be used in the fields of high-end general chips and the like.
The traditional epoxybutane production process is a chlorohydrin method, but the process consumes a large amount of chlorine in the production process, and simultaneously generates a large amount of wastewater containing organic chloride, heavy organic impurities and waste residues, which pollute the environment, so the process is basically eliminated at present. The butene oxidation method adopts butene as raw material and cumene hydroperoxide as oxidant, and directly epoxidizes to generate epoxybutane under the action of a silicon-titanium molecular sieve catalyst. Compared with the chlorohydrin method, the butene oxidation method has advanced process, and particularly does not need to use chlorine, thereby greatly reducing environmental pollution. However, the reaction products of butene oxidation or other synthesis processes usually contain impurities such as water, methanol, propionaldehyde, methyl formate, butyraldehyde, butanone, glycol, etc., most of which have a boiling point close to that of butylene oxide and are easily azeotroped with butylene oxide, so that it is difficult to separate high-purity butylene oxide by ordinary rectification, but when butylene oxide is used as a monomer for polymerization, not only is the purity required to be high, but also the content of impurities such as water, aldehyde, etc. should be limited to a low range.
However, in the prior art, the multi-tower rectification process is adopted, so that the material returning operation difficulty between a plurality of reactors is increased, and the energy consumption for separation and purification is increased.
Disclosure of Invention
The invention provides a separation method, which aims to solve the problems of high energy consumption and high equipment investment in the existing multi-tower rectification process.
The invention provides a separation method, which adopts a coupling refining unit with an extraction section, a low-boiling product condensation section, a low-boiling impurity rectification section, a low-boiling impurity stripping section, a product stripping section and a product rectification section as a separator, and comprises the following steps:
allowing the to-be-separated matter and the extractant to enter an extraction section for extraction treatment to generate an extract liquid and raffinate gas; the extract liquid downwards enters a low-boiling impurity stripping section to carry out first stripping treatment to generate first stripping gas and first stripping liquid; the first stripping liquid goes down to enter the product stripping section for second stripping treatment to generate second stripping gas and recover extractant, and part of the second stripping gas goes up to enter the low-boiling impurity stripping section to participate in the first stripping treatment;
the raffinate gas goes upward to enter the low-boiling impurity rectifying section to carry out first rectifying treatment to generate first rectifying liquid and first rectifying gas; the first rectifying liquid returns to the extraction section to participate in the extraction treatment; the first rectifying gas goes upward to enter a condensing section of the low-boiling product for condensation treatment to generate condensate and non-condensable gas, and at least part of the condensate returns to the low-boiling impurity rectifying section to participate in the first rectifying treatment;
the rest of the second stripping gas goes upward to enter the product rectifying section for second rectifying treatment to generate second rectifying gas and second rectifying liquid; and introducing the second rectifying gas into a product condensation and separation unit outside the separator to perform product condensation and separation treatment to obtain a liquid-phase product.
Further, introducing a gas phase obtained by the product condensation gas-liquid separation treatment into the low-boiling impurity rectification section to participate in the first rectification treatment; and/or the number of the groups of groups,
part of the liquid phase product is introduced into the product rectification section to participate in the second rectification treatment.
Further, the second rectification liquid is introduced into a high-boiling-point substance condensation phase separation unit outside the separator, and condensation phase separation treatment is carried out to obtain an organic phase and an inorganic phase; the organic phase is introduced into the product rectification section to participate in the second rectification treatment.
Further, the inorganic phase enters a separation unit outside the separator for separation treatment to obtain a crude product, high-boiling impurities and inorganic purified matters; the crude product is introduced into the low-boiling impurity stripping section to participate in the first stripping treatment.
Further, a first reboiling gas phase is obtained after the inorganic purified material is subjected to the first reboiling treatment, and the first reboiling gas phase is circulated to participate in the first reboiling treatment.
Further, the recovered extractant is introduced to the outside of the separator for second reboiling treatment to obtain a second reboiling gas phase and a second reboiling liquid phase; the second reboiling gas phase is introduced into the product stripping section to participate in the second stripping treatment, and the second reboiling liquid phase is introduced into the extraction section to participate in the extraction treatment.
Further, the method also comprises the steps of carrying out first temperature monitoring treatment on the gas phase and adjusting the working temperature of the condensation separation treatment of the product according to the temperature signal of the first temperature monitoring treatment.
Further, the method further comprises the steps of performing second temperature monitoring treatment on the second rectification liquid led out of the separator, adjusting the working temperature of condensation separation treatment of the product according to the temperature signals of the second temperature monitoring treatment and the first temperature monitoring treatment, and adjusting the flow of the second rectification liquid led out of the separator according to the temperature signals of the first temperature monitoring treatment.
Further, the substance to be separated is a crude product of epoxybutane; wherein, the weight ratio of the crude butylene oxide to the extractant is 1:0.25 to 3.50; and/or the number of the groups of groups,
the operating pressure of the extraction section is 0.05-0.8Mpa, and the operating temperature is 55-70 ℃; and/or the number of the groups of groups,
the operation pressure of the condensing section of the low-boiling product is 0.05-0.8Mpa, and the operation temperature is-50-40 ℃; and/or the number of the groups of groups,
the operating pressure of the low-boiling impurity rectifying section is 0.05-0.8Mpa, and the operating temperature is-20-55 ℃; and/or the number of the groups of groups,
the operating pressure of the low-boiling impurity stripping section is 0.05-0.8Mpa, and the operating temperature is 70-90 ℃; and/or the number of the groups of groups,
the operating pressure of the stripping section of the product is 0.05-0.8Mpa, and the operating temperature is 90-150 ℃; and/or the number of the groups of groups,
the operating pressure of the rectifying section of the product is 0.05-0.8Mpa, and the operating temperature is 0-90 ℃; and/or the number of the groups of groups,
the operation temperature of the condensed gas-liquid separation treatment is 0-40 ℃; and/or the number of the groups of groups,
the reflux ratio of the first rectification treatment is 2-12.
Further, the operating pressure of the separation unit is 0.06-0.9 Mpa, and the temperature is-10-160 ℃.
The invention provides a separation method, which adopts a coupling refining unit with an extraction section, a low-boiling product condensation section, a low-boiling impurity rectification section, a low-boiling impurity stripping section, a product stripping section and a product rectification section as a separator, and can uniformly perform extraction, rectification and stripping.
Drawings
FIG. 1 is a schematic view of a separation device according to the present invention;
fig. 2 is a schematic view of another separation device according to the present invention.
Reference numerals illustrate:
01: a coupling refining unit; 02: a product condensation gas-liquid separation unit; 04: a high-boiling-point substance condensed phase separation unit; 06: a second reboiling unit; 07: a separation unit; 08: a first reboiling unit; 021: a first temperature monitoring unit; 022: a first temperature control unit; 023: a second temperature monitoring unit; 024: and a second temperature control unit.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the present invention more apparent, the technical solutions in the embodiments of the present invention will be clearly and completely described in the following in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The invention provides a separation method, which adopts a separation device shown in figure 1, and comprises a coupling refining unit, wherein the coupling refining unit is provided with an extraction section, a low-boiling product condensation section, a low-boiling impurity rectification section, a low-boiling impurity stripping section, a product stripping section and a product rectification section, as a separator, and the method comprises the following steps:
allowing the to-be-separated matter and the extractant to enter an extraction section for extraction treatment to generate an extract liquid and raffinate gas; the extract liquid goes down to a low-boiling impurity stripping section for first stripping treatment to generate first stripping gas and first stripping liquid; the first stripping liquid goes down to enter a product stripping section for second stripping treatment to generate second stripping gas and recover extractant, and part of the second stripping gas goes up to enter a low-boiling impurity stripping section to participate in the first stripping treatment;
allowing the raffinate gas to go into a low-boiling impurity rectifying section for first rectifying treatment to generate a first rectifying liquid and a first rectifying gas; the first rectifying liquid returns to the extraction section to participate in the extraction treatment; the first rectifying gas goes upward to enter a condensing section of the low-boiling product for condensation treatment to generate condensate and non-condensable gas, and at least part of condensate returns to the low-boiling impurity rectifying section to participate in the first rectifying treatment;
the remaining second stripping gas goes into a product rectifying section to carry out second rectifying treatment to generate second rectifying gas and second rectifying liquid; and introducing the second rectifying gas into a product condensation gas-liquid separation unit outside the separator to perform product condensation gas-liquid separation treatment, so as to obtain a liquid phase product.
It will be appreciated that products produced in industrial processes typically contain impurities and that some low boiling impurities tend to form azeotropes with the product making it difficult to obtain high purity products by conventional rectification separation. The invention provides a separation method adopting a coupling refining unit with an extraction section, a low-boiling product condensation section, a low-boiling impurity rectification section, a low-boiling impurity stripping section, a product stripping section and a product rectification section as a separator, which is particularly suitable for the separation of the type of products. In the application process, the invention is not limited in the type of the substance to be separated, and is suitable for separating and purifying azeotrope formed by all products and impurities.
Taking crude epoxybutane as an example, the material to be separated not only contains impurities formed by high-boiling impurities such as butyraldehyde and butanone, but also contains low-boiling impurities such as carbon dioxide, epoxypropane, acetone, propionaldehyde, methanol and the like, and azeotrope formed by the impurities and epoxybutane. By adopting the separation method provided by the invention, the azeotropic relationship between the epoxybutane and the low-boiling impurities can be destroyed, and the separation of epoxybutane, the low-boiling impurities and the high-boiling impurities from each other can be finally realized, so that the purification and separation of epoxybutane products can be realized.
In the separation process, crude epoxybutane and an extracting agent respectively enter an extraction section in a coupling refining unit 01, extraction treatment is carried out in the extraction section, at the moment, the azeotropic relationship between the epoxybutane and low-boiling impurities is destroyed, the epoxybutane is extracted into the extracting agent to form an extracting solution, and the low-boiling impurities form raffinate gas, so that the separation of the epoxybutane and the low-boiling impurities is realized; when the to-be-separated matter is crude epoxybutane, the extractant can be water, various solvent oils, sulfolane, N-methyl pyrrolidone, N-dimethylformamide and other high-boiling point organic solvents and mixtures thereof;
the raffinate gas goes into a low-boiling impurity rectifying section to be subjected to first rectifying treatment to form first rectifying gas and first rectifying liquid, so that the low-boiling impurities are further separated from the epoxybutane and the extractant; the first rectifying liquid rich in epoxybutane and extractant flows down to enter the extraction section again to participate in extraction treatment, the product is further recovered, the first rectifying gas rich in low-boiling impurities flows up to enter the low-boiling product condensation section to be condensed, wherein the low-boiling impurities are condensed into condensate, the gas phase which cannot be condensed is the most non-condensable gas and continuously flows up, and at least part of condensate returns to the low-boiling impurity rectification section again to be subjected to the first rectification treatment after the condensate flows down, so that epoxybutane in the low-boiling impurity is further recovered;
the extraction liquid enters a low-boiling impurity stripping section under the action of gravity to carry out first stripping treatment to form first stripping gas and first stripping liquid, so as to realize concentration of butylene oxide and low-boiling impurities, wherein the low-boiling impurities which are easy to gasify form the first stripping gas and then go upward to enter the extraction section again to further participate in the extraction treatment, the butylene oxide, the extractant, the high-boiling impurities and the like form the first stripping liquid and go downward to enter a product stripping section to carry out second stripping treatment to form second stripping liquid and second stripping gas, so as to realize concentration and separation of the extractant, wherein butylene oxide, water, the high-boiling impurities and the like are gasified into the second stripping gas, and materials mainly used as the extractant form a recovery extractant; and part of the second stripping gas goes upward to reenter the low-boiling impurity stripping section to participate in the first stripping treatment, so that the concentration of the epoxybutane and the low-boiling impurities is further realized, the other part of the second stripping gas goes upward to enter the product rectifying section to carry out the second rectifying treatment to form second rectifying gas and second rectifying liquid, the separation and refining of the epoxybutane, water and high-boiling substances are realized, the second rectifying liquid mainly containing water, high-boiling impurities and a small amount of epoxybutane goes downward, the second rectifying gas mainly rich in epoxybutane goes upward to be discharged through a product outlet of the product rectifying section, and goes into a product condensation gas-liquid separation unit 02 outside the separator to carry out the product condensation gas-liquid separation treatment to obtain a liquid phase product, the gas phase material can be separated into a gas phase and a liquid phase in the cooling process at the same time, or the gas-liquid mixture after cooling is subjected to gas-liquid separation to obtain the gas phase and the liquid phase respectively, and finally the effect of separating the product is achieved.
The invention provides a separation method, which adopts a coupling refining unit with an extraction section, a low-boiling product condensation section, a low-boiling impurity rectification section, a low-boiling impurity stripping section, a product stripping section and a product rectification section as a separator.
The present invention is not limited to a specific arrangement of the separator, and for example, the coupling refining unit as a reactor includes a column body having a cavity therein, a first partition plate, and a second partition plate; the plate surface of the first partition plate extends along the vertical direction, the first end and the second end of the first partition plate which are oppositely arranged in the horizontal direction are respectively connected to the side wall of the cavity, so that the first partition plate is suspended in the cavity, the third end and the fourth end of the first partition plate which are oppositely arranged in the vertical direction are spaced from the top wall and the bottom wall of the cavity, and the plate surface and the side wall of the first partition plate are spaced; the second partition board is connected between the side wall of the cavity and a third end, and the third end is close to the top wall; a first area is formed between the plane where the end face of the fourth end is positioned and the bottom wall of the cavity, and the product stripping section is positioned in the first area; a second area is formed between the plane where the plate surface of the second partition plate is positioned and the top wall of the cavity, and the low-boiling impurity rectifying section and the low-boiling product condensing section are positioned in the second area, wherein the low-boiling product condensing section is close to the top wall and is communicated with the low-boiling impurity rectifying section; an intermediate area is arranged between the first area and the second area, the first partition plate divides the intermediate area into a first intermediate area and a second intermediate area close to the second partition plate, wherein the low-boiling impurity stripping section and the extraction section close to the second area are positioned in the first intermediate area, and the product rectifying section is positioned in the second intermediate area.
With the separation device shown in fig. 2, in a specific embodiment, the gas phase obtained by the product condensation gas-liquid separation treatment is introduced into a low-boiling impurity rectifying section to participate in the first rectifying treatment;
in another embodiment, a portion of the liquid phase product is introduced into the product rectification section to participate in the second rectification process.
It can be understood that in the product condensation gas-liquid separation process, volatile matter containing low boiling impurities and the like forms a gas phase which is discharged from the gas phase outlet of the product condensation gas-liquid separation unit 02 and introduced into the low boiling impurity rectifying section to be re-participated in the first rectifying process, and after being concentrated therein, the volatile matter enters the low boiling product condensing section to be condensed, wherein preferably, the temperature of the condensing process is lower than the condensing temperature of the product condensation gas-liquid separation process to further recover a small amount of the product contained therein;
the materials with the main components of the product are condensed into liquid-phase products and separated from gas phase, the liquid-phase products are extracted through a liquid-phase outlet of a product condensation gas-liquid separation unit 02, at least part of the liquid-phase products are introduced into a product rectifying section and are re-participated in second rectifying treatment, and further recovery of butylene oxide products is realized; and outputting the rest liquid phase products as products.
Further, the second rectification liquid is introduced into a high-boiling-point substance condensation phase separation unit 04 outside the separator to be subjected to condensation phase separation treatment, so as to obtain an organic phase and an inorganic phase; the organic phase is introduced into the product rectification section to participate in the second rectification treatment.
The second rectification liquid mainly containing water, high-boiling impurities and a small amount of products is converged at the bottom of the product rectification section, is discharged through a high-boiling substance outlet, is introduced into a high-boiling substance condensation phase separation unit 04 outside the separator, and is subjected to condensation phase separation treatment. Because the solubility of the product in water is lower at low temperature, the product can be separated from the water phase containing water and high-boiling impurities after condensation by condensation phase separation treatment to obtain an organic phase, or the product can be obtained by condensing liquid phase materials first and then carrying out phase separation to obtain the organic phase rich in the product and the water phase rich in water and high-boiling impurities. And then reintroducing the organic phase into the product rectification unit to participate in the second rectification treatment, and further separating and refining the product. It can be appreciated that the main component in the inorganic phase is water, but it is also difficult to avoid inclusion of organic impurities, with high boiling impurities being the main.
Further, the water phase enters a separation unit outside the separator for separation treatment to obtain a crude product, high-boiling impurities and inorganic purified matters; the crude product is introduced into a low-boiling impurity stripping section to participate in the first stripping treatment.
Introducing the low-temperature water phase subjected to the condensation phase separation treatment into a separation unit 07 outside the separator for separation treatment, separating a gas phase containing a small amount of products from high-boiling impurities and water, wherein the gas phase containing the small amount of products is reintroduced into the low-boiling impurity stripping section as a crude product to participate in the first stripping treatment, and further separating and recovering the products in the gas phase; wherein the high-boiling impurity liquid phase is extracted from the side line of the separation unit and is output out of the limit as a high-boiling product; a liquid phase whose main component is water is extracted from the bottom of the separation unit 07 as an inorganic purified matter; realizes the function of purifying water, external coupling of purifying water and separating and refining, and recovery treatment of high-boiling-point substances.
In one embodiment, the inorganic purified material is subjected to a first reboiling treatment to obtain a first reboiling gas phase, and the first reboiling gas phase is recycled to participate in the first reboiling treatment.
Introducing the inorganic purified material extracted from the bottom of the separation unit 07 into a first reboiling unit 08, and performing first reboiling treatment to obtain a first reboiling gas phase and a first reboiling liquid phase after reboiling, so that the first reboiling gas phase reenters the lower part of the separation unit 07, and the water, high-boiling impurities and products contained in the inorganic purified material are circulated to participate in the first reboiling treatment to be further separated; the first reboiling liquid phase is used as purified water to be output out of the limit, so that the high-efficiency recovery and the synchronous water purification treatment of the product are realized.
Further, the recovered extractant is introduced to the outside of the separator for second reboiling treatment to obtain a second reboiling gas phase and a second reboiling liquid phase; the second reboiling gas phase is introduced into the product stripping section to participate in the second stripping treatment, and the second reboiling liquid phase is introduced into the extraction section to participate in the extraction treatment.
The recovered extractant obtained in the second stripping treatment descends to the bottom of a product stripping section, is discharged through an extractant outlet, is introduced into a second reboiling unit 06 outside the separator, and is subjected to second reboiling treatment to obtain a second reboiling gas phase and a second reboiling liquid phase; wherein, the second reboiling gas phase containing the product is reintroduced into the product stripping section to participate in the second stripping treatment, and further the product is separated from the extractant; and the second reboiling liquid phase rich in the extractant is reintroduced into the extraction section to participate in the extraction treatment, thereby realizing the recycling of the extractant.
In one embodiment, the method further comprises the steps of performing a first temperature monitoring process on the gas phase and adjusting the working temperature of the condensation separation process of the product according to the temperature signal of the first temperature monitoring process.
Since the temperature control of the product condensation gas-liquid separation process is very important for the purity of the product, the first temperature monitoring process is performed by the first temperature monitoring unit 021, the gas phase temperature output from the outlet of the product condensation separation process is monitored, and the working temperature of the product condensation separation process is adjusted according to the monitored temperature signal. Specifically, the working temperature of the product condensation separation process may be controlled by the first temperature control unit 022, and the effect of adjusting the working temperature of the product condensation separation process may be achieved by specifically adjusting the amount of water fed to the circulating cooling process during the product condensation separation process.
Further, the method further comprises the steps of performing second temperature monitoring treatment on the second rectification liquid led out of the separator, adjusting the working temperature of condensation separation treatment of the product according to the temperature signals of the second temperature monitoring treatment and the first temperature monitoring treatment, and adjusting the flow of the second rectification liquid led out of the separator according to the temperature signals of the first temperature monitoring treatment.
In order to meet the high requirement on the purity of the product, the second temperature monitoring treatment can be performed through the second temperature monitoring unit 023, the temperature of the second rectification liquid outside the separator is monitored, the working temperature of the condensation separation treatment of the product is regulated simultaneously according to the monitored temperature signal, the flow of the second rectification liquid outside the separator is controlled through the second temperature control unit 024 according to the temperature signal of the first temperature monitoring treatment, the prediction adjustment of the temperature of the product is realized, and the accurate regulation of the outlet temperature of the product is ensured.
Preferably, the low-boiling product condensing section is a built-in condensing section and is internally provided with a heat exchange tube, the heat exchange tube is internally provided with a tube side, the outside of the heat exchange tube is provided with a shell side, and the low-boiling product condensing section is provided with a low-boiling impurity shell side outlet, a non-condensable gas shell side outlet and a gas phase shell side inlet; the raffinate gas enters a condensation section of the low-boiling product through a gas phase shell side inlet for condensation treatment, wherein noncondensable gas which is difficult to condense is discharged through a noncondensable gas shell side outlet, condensate containing low-boiling impurities and a small amount of epoxybutane is discharged through a low-boiling impurity shell side outlet, and at least part of condensate is returned into a low-boiling impurity rectifying section through a low-boiling impurity inlet to participate in the first rectifying treatment again.
And a tube side is arranged in the low-boiling product condensation section, the circulating cooling water enters the low-boiling product condensation section through a tube side inlet for heat exchange treatment, and then leaves the low-boiling product condensation section through a tube side outlet to be output as circulating cooling water return. It can be understood that the circulating cooling water also enters the product condensation gas-liquid separation unit 02 to perform heat exchange treatment, and specifically, the first temperature control unit 022 may be disposed on a pipeline connected between the circulating cooling water and a water supply pipe inlet of the product condensation gas-liquid separation unit 02, so as to realize adjustment of the working temperature of the product condensation separation treatment.
In one embodiment, the material to be separated is a crude butylene oxide product; wherein, the weight ratio of the crude butylene oxide to the extractant is 1:0.25 to 3.50; the operating pressure of the extraction section is 0.05-0.8Mpa, and the operating temperature is 55-70 ℃; the operation pressure of the condensing section of the low-boiling product is 0.05-0.8Mpa, and the operation temperature is-50-40 ℃; the operating pressure of the low-boiling impurity rectifying section is 0.05-0.8Mpa, and the operating temperature is-20-55 ℃; the operating pressure of the low-boiling impurity stripping section is 0.05-0.8Mpa, and the operating temperature is 70-90 ℃; the operating pressure of the stripping section of the product is 0.05-0.8Mpa, and the operating temperature is 90-150 ℃; the operating pressure of the rectifying section of the product is 0.05-0.8Mpa, and the operating temperature is 0-90 ℃;
in another specific embodiment, the operation temperature of the condensed gas-liquid separation treatment is 0-40 ℃;
in still another embodiment, the reflux ratio of the first rectification treatment is 2 to 12.
By further defining the parameters of each part in the separator, the epoxybutane can be separated from the low-boiling-point substances better; it can be understood that the reflux ratio refers to the ratio of the reflux part to the output part, and the circulation amount of the materials in the tower can be controlled in a proper range by limiting the reflux ratio, so that the separation efficiency is further improved, the energy is saved, and the output is increased.
Further, the operating pressure of the separation unit is 0.06-0.9 Mpa and the temperature is-10-160 ℃. The solubility of the epoxybutane is lower at low temperature, so that the operation temperature of the high-boiling-point substance condensation phase separation unit is further limited, and the efficient separation of the epoxybutane and the water phase is facilitated; also, further limiting the execution parameters of the separation unit is advantageous for efficient performance of the water purification treatment, preferably, the reflux ratio of the second rectification treatment is 0.2 to 5; the operation temperature of the first reboiling treatment is 115-160 ℃, and the operation pressure is 0.06-0.9 MPa; the operation temperature of the second reboiling treatment is 110-180 ℃ and the operation pressure is 0.05-0.8 MPa; the operation temperature of the separation treatment of the condensed phase of the product is-10 to 50 ℃.
Hereinafter, a separation method according to the present invention will be described in detail by way of specific examples.
The following examples employed crude butylene oxide feedstock of the weight composition: 1.1% of carbon dioxide, 1.2% of propylene oxide, 0.6% of acetone and propionaldehyde, 0.8% of methanol, 90.5% of butylene oxide, 4.0% of water, and the balance of butyraldehyde and butanone.
Example 1
The embodiment adopts the separation device shown in fig. 1, which comprises an extraction section, a low-boiling product condensation section, a low-boiling impurity rectification section, a low-boiling impurity stripping section, a product stripping section and a product rectification section, wherein the separation device is provided with a coupling refining unit as a separator, and comprises the following steps:
the crude epoxybutane and the extractant are respectively added into an extraction section in a coupling refining unit 01 for extraction treatment, and the weight ratio of the crude epoxybutane to the extractant is 1:0.4, generating an extract liquid and raffinate gas; the extract liquid goes down to a low-boiling impurity stripping section for first stripping treatment to generate first stripping gas and first stripping liquid; the first stripping liquid goes down to enter a product stripping section for second stripping treatment to generate second stripping gas and recover extractant, and part of the second stripping gas goes up to enter a low-boiling impurity stripping section to participate in the first stripping treatment;
allowing the raffinate gas to go into a low-boiling impurity rectifying section for first rectifying treatment to generate a first rectifying liquid and a first rectifying gas; the first rectifying liquid returns to the extraction section to participate in the extraction treatment; the first rectifying gas goes upward to enter a condensing section of the low-boiling product for condensation treatment, the condensation treatment temperature is-15 ℃, condensate and non-condensable gas are generated, at least part of condensate returns to the low-boiling impurity rectifying section to participate in the first rectifying treatment, and the reflux ratio of the first rectifying treatment is 5.
The remaining second stripping gas goes into a product rectifying section to carry out second rectifying treatment to generate second rectifying gas and second rectifying liquid; and introducing the second rectifying gas into a product condensation gas-liquid separation unit 02 outside the separator to perform product condensation gas-liquid separation treatment to obtain the epoxybutane.
The operating pressure of the extraction section is 0.10Mpa, and the operating temperature is 55 ℃; the operation pressure of the condensing section of the low-boiling product is 0.12Mpa, and the operation temperature is-20 ℃; the operating pressure of the low-boiling impurity rectifying section is 0.10Mpa, and the operating temperature is-20 ℃; the operating pressure of the low-boiling impurity stripping section is 0.10Mpa, and the operating temperature is 70 ℃; the operating pressure of the stripping section of the product is 0.15Mpa, and the operating temperature is 90 ℃; the operating pressure of the product rectifying section is 0.15Mpa, and the operating temperature is 0 ℃;
in this example, the chemical purity (mass ratio) of the obtained butylene oxide product was 99.7%, and the yield of butylene oxide was 99.5%.
Example 2
The embodiment adopts the separation device shown in fig. 2, which is provided with an extraction section, a low-boiling product condensation section, a low-boiling impurity rectification section, a low-boiling impurity stripping section, a product stripping section and a product rectification section, wherein the coupling refining unit is a separator, and the embodiment further comprises the following steps based on the embodiment 1:
1) Introducing a gas phase obtained through product condensation gas-liquid separation treatment into a low-boiling impurity rectifying section to participate in first rectifying treatment; part of the liquid phase product is introduced into a product rectifying section to participate in the second rectifying treatment; the reflux ratio of the second rectification treatment is 3.
2) Introducing the second rectification liquid into a high-boiling-point substance condensation phase separation unit outside the separator, and performing condensation phase separation treatment to obtain an organic phase and a water phase; the organic phase is introduced into a product rectifying section to participate in second rectifying treatment; the operating temperature of the product condensed phase separation treatment is 10 ℃.
3) The water phase enters a separation unit outside the separator for separation treatment to obtain a crude product, high-boiling impurities and inorganic purified matters; introducing the crude product into a low-boiling impurity stripping section to participate in first stripping treatment; the operating pressure of the separation treatment was 0.10MPa and the operating temperature was-10 ℃.
4) The inorganic purified material is subjected to a first reboiling treatment to obtain a first reboiling gas phase, the first reboiling gas phase is circulated to participate in the first reboiling treatment, the temperature of the first reboiling treatment is 102.3 ℃, and the operating pressure is 0.8MPa.
5) Introducing the recovered extractant into the outside of the separator for second reboiling treatment to obtain a second reboiling gas phase and a second reboiling liquid phase; the second reboiling gas phase is introduced into a product stripping section to participate in the second stripping treatment, and the second reboiling liquid phase is introduced into an extraction section to participate in the extraction treatment; the temperature of the second reboiling treatment was 124.3℃and the operating pressure was 0.8MPa.
6) Carrying out first temperature monitoring treatment on the gas phase, and adjusting the working temperature of condensation and separation treatment of the product according to the temperature signal of the first temperature monitoring treatment;
and carrying out second temperature monitoring treatment on the second rectifying liquid led out of the separator, regulating the working temperature of condensation separation treatment of the product according to the temperature signals of the second temperature monitoring treatment and the first temperature monitoring treatment, and regulating the flow of the second rectifying liquid led out of the separator according to the temperature signals of the first temperature monitoring treatment.
In this example, the chemical purity (mass ratio) of the obtained butylene oxide product was 99.995%, and the yield of butylene oxide was 99.75%.
Example 3
Step 3) in example 2 was removed, and the rest was the same as example 2.
In this example, the chemical purity (mass ratio) of the obtained butylene oxide product was 99.87%, and the yield of butylene oxide was 99.6%.
Example 4
Step 6) in example 2 was removed, and the rest was the same as in example 2.
In this example, the chemical purity (mass ratio) of the obtained butylene oxide product was 99.85%, and the yield of butylene oxide was 99.65%.
Comparative example 1
The embodiment adopts a separating device with a rectifying tower as a separator, and comprises the following steps:
respectively adding the crude epoxybutane and the extractant into a rectifying tower for extraction and rectification treatment, wherein the weight ratio of the crude epoxybutane to the extractant is 1:0.4, generating an extract liquid and raffinate gas; and introducing the raffinate gas into a product condensation gas-liquid separation unit outside the rectifying tower to perform product condensation gas-liquid separation treatment, so as to obtain the epoxybutane product.
The operating pressure of the rectifying tower is 0.10Mpa, and the operating temperature is 70 ℃;
in this example, the chemical purity (mass ratio) of the obtained butylene oxide product was 99.2%, and the yield of butylene oxide was 92.5%
The invention provides a separation method, which adopts a coupling refining unit with an extraction section, a low-boiling product condensation section, a low-boiling impurity rectification section, a low-boiling impurity stripping section, a product stripping section and a product rectification section as a separator, and has the advantages of simple operation, high load adjustment elasticity, capability of obtaining a high-purity product, capability of uniformly carrying out extraction, rectification and stripping, ingenious design, effective reduction of energy consumption and cost and easy industrialization.
Claims (10)
1. The separation method is characterized in that a coupling refining unit with an extraction section, a low-boiling product condensation section, a low-boiling impurity rectification section, a low-boiling impurity stripping section, a product stripping section and a product rectification section is adopted as a separator, and the method comprises the following steps:
allowing the to-be-separated matter and the extractant to enter an extraction section for extraction treatment to generate an extract liquid and raffinate gas; the extract liquid downwards enters a low-boiling impurity stripping section to carry out first stripping treatment to generate first stripping gas and first stripping liquid; the first stripping liquid goes down to enter the product stripping section for second stripping treatment to generate second stripping gas and recover extractant, and part of the second stripping gas goes up to enter the low-boiling impurity stripping section to participate in the first stripping treatment;
the raffinate gas goes upward to enter the low-boiling impurity rectifying section to carry out first rectifying treatment to generate first rectifying liquid and first rectifying gas; the first rectifying liquid returns to the extraction section to participate in the extraction treatment; the first rectifying gas goes upward to enter a condensing section of the low-boiling product for condensation treatment to generate condensate and non-condensable gas, and at least part of the condensate returns to the low-boiling impurity rectifying section to participate in the first rectifying treatment;
the rest of the second stripping gas goes upward to enter the product rectifying section for second rectifying treatment to generate second rectifying gas and second rectifying liquid; and introducing the second rectifying gas into a product condensation gas-liquid separation unit outside the separator to perform product condensation gas-liquid separation treatment, so as to obtain a liquid phase product.
2. The method according to claim 1, wherein a gas phase obtained by the product condensed gas-liquid separation treatment is introduced into the low boiling impurity rectifying section to participate in the first rectifying treatment; and/or the number of the groups of groups,
part of the liquid phase product is introduced into the product rectification section to participate in the second rectification treatment.
3. The method according to claim 1 or 2, wherein the second rectification liquid is introduced into a high-boiling-point substance condensation phase separation unit outside the separator, and subjected to condensation phase separation treatment to obtain an organic phase and an inorganic phase; the organic phase is introduced into the product rectification section to participate in the second rectification treatment.
4. A method according to any one of claims 3, wherein the inorganic phase enters a separation unit outside the separator for separation treatment to obtain a crude product, high-boiling impurities and inorganic purified matters; the crude product is introduced into the low-boiling impurity stripping section to participate in the first stripping treatment.
5. The method according to claim 4, wherein a first reboiling gas phase is obtained after the first reboiling treatment of the inorganic purified product, and the first reboiling gas phase is recycled to participate in the first reboiling treatment.
6. The method of claim 5, wherein the recovered extractant is introduced outside the separator for a second reboiling process to provide a second reboiled vapor phase and a second reboiled liquid phase; the second reboiling gas phase is introduced into the product stripping section to participate in the second stripping treatment, and the second reboiling liquid phase is introduced into the extraction section to participate in the extraction treatment.
7. The method of claim 2, further comprising the step of subjecting said gas phase to a first temperature monitoring process and adjusting the operating temperature of said product condensation separation process based on a temperature signal of said first temperature monitoring process.
8. The method of claim 7, further comprising the steps of performing a second temperature monitoring process on the second rectification liquid exiting the exterior of the separator, adjusting the operating temperature of the product condensation separation process based on the temperature signals of the second temperature monitoring process and the first temperature monitoring process, and adjusting the flow rate of the second rectification liquid exiting the exterior of the separator based on the temperature signals of the first temperature monitoring process.
9. The method according to claim 6, wherein the substance to be separated is crude butylene oxide; wherein, the weight ratio of the crude butylene oxide to the extractant is 1:0.25 to 3.50; and/or the number of the groups of groups,
the operating pressure of the extraction section is 0.05-0.8Mpa, and the operating temperature is 55-70 ℃; and/or the number of the groups of groups,
the operation pressure of the condensing section of the low-boiling product is 0.05-0.8Mpa, and the operation temperature is-50-40 ℃; and/or the number of the groups of groups,
the operating pressure of the low-boiling impurity rectifying section is 0.05-0.8Mpa, and the operating temperature is-20-55 ℃; and/or the number of the groups of groups,
the operating pressure of the low-boiling impurity stripping section is 0.05-0.8Mpa, and the operating temperature is 70-90 ℃; and/or the number of the groups of groups,
the operating pressure of the stripping section of the product is 0.05-0.8Mpa, and the operating temperature is 90-150 ℃; and/or the number of the groups of groups,
the operating pressure of the rectifying section of the product is 0.05-0.8Mpa, and the operating temperature is 0-90 ℃; and/or the number of the groups of groups,
the operation temperature of the condensed gas-liquid separation treatment is 0-40 ℃; and/or the number of the groups of groups,
the reflux ratio of the first rectification treatment is 2-12.
10. The method of claim 4, wherein the step of determining the position of the first electrode is performed,
the operating pressure of the separation unit is 0.06-0.9 Mpa, and the temperature is-10-160 ℃.
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| CN203750202U (en) * | 2014-03-24 | 2014-08-06 | 华陆工程科技有限责任公司 | Device for recovering hydrogen chloride from hydrochloric acid |
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| CN1433392A (en) * | 2000-05-09 | 2003-07-30 | 巴斯福股份公司 | Method and device for treating C4 fraction |
| US20030181772A1 (en) * | 2000-05-09 | 2003-09-25 | Gerald Meyer | Method and device for treating a c4 fraction |
| CN102188837A (en) * | 2010-03-03 | 2011-09-21 | 中国石油化工股份有限公司 | Extractive distillation method |
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