CN113072419B - Hexafluorobutadiene purification method with high recovery rate - Google Patents
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Abstract
The invention relates to a method for purifying hexafluorobutadiene with high recovery rate, which comprises the following steps: introducing a hexafluorobutadiene raw material into a first-stage light component removal tower to remove light components, introducing a tower top extract of the first-stage light component removal tower into a recovery tower to concentrate the light components, and introducing a tower kettle extract into a second-stage light component removal tower to remove the light components; introducing the tower top extract of the secondary light component removal tower into a recovery tower for light component concentration, wherein the tower bottom extract is a purified hexafluorobutadiene product; the tower top extract of the recovery tower is the concentrated light component, and the tower bottom extract is mixed with the hexafluorobutadiene raw material and then circularly introduced into the first-stage light component removal tower to remove the light component. Compared with the prior art, the method adopts a two-stage rectification method to deeply remove the light component in the raw material of the hexafluorobutadiene, and utilizes single-stage high-efficiency rectification to recover the hexafluorobutadiene in the light component, so that the method has the advantages of safe and simple process, low maintenance cost, stable process and high recovery rate, and is very suitable for industrial production.
Description
Technical Field
The invention belongs to the technical field of purification of hexafluorobutadiene, and relates to a method for purifying hexafluorobutadiene with high recovery rate.
Background
Hexafluoro-1, 3-butadiene (C) 4 F 6 Hexafluorobutadiene for short) is a perfluorinated compound with a boiling point of about 6 ℃ at normal pressure, which was first used in the synthesis of fluorine-containing high molecular compounds. At present, the electron etching gas is mainly used in the etching process of SiO. Since hexafluorobutadiene has the largest C/F ratio among all electron etching gases and contains no H, the SiO etching has extremely high selectivity to Si or SiN on the substrate, and almost vertical etching can be realized. At the same time, the atmospheric lifetime of hexafluorobutadiene is less than 2 days, GWP 100 A value of only 290 is presently found to be satisfactory for etching techniquesThe requirement is developed, and the novel etching gas which has the influence on the environment can be reduced to the maximum extent.
The crude hexafluorobutadiene typically contains organic and inorganic impurities. Wherein, the organic impurities comprise C1-C5 halogenated olefin, halogenated alkane and halogenated alkyne, and the halogen is one or more of fluorine, chlorine, bromine and iodine according to different preparation process routes. Among the above organic impurities, the separation of light component impurities having a lower atmospheric boiling point than that of hexafluorobutadiene is difficult, especially hexafluorocyclobutene and hexafluoro-2-butyne.
The separation and purification method of hexafluorobutadiene reported at present basically comprises a molecular sieve adsorption process. For example, chinese patent CN107032949A discloses a method for purifying hexafluorobutadiene, which comprises an adsorption step and a rectification step, wherein in the adsorption step, an adsorbent is modified by at least one of an ion exchange method, a ball milling method or an impregnation method, and the adsorbent is at least one of a NaA type molecular sieve, a NaX type molecular sieve or a ZSM-5 type molecular sieve. Chinese patent CN108276246A discloses a method for refining hexafluorobutadiene, which comprises removing water from industrial grade hexafluorobutadiene by a molecular sieve adsorbent, and then feeding the hexafluorobutadiene into an adsorption tower filled with an amino modified layered double hydroxide adsorbent, wherein the temperature is 10-50 ℃, the pressure is 0.05-0.5 MPa, and the flow rate is 1-5 BV/h, so as to obtain a high-purity hexafluorobutadiene product.
However, isomerization of hexafluorobutadiene occurs during molecular sieve adsorption. Both patent US6544319 and patent WO2007/063938A1 report that type X molecular sieves have a strong isomerization effect on hexafluorobutadiene, isomerizing hexafluorobutadiene to hexafluoro-2-butyne with a rapid temperature rise of the system. Patent US6544319 reports that the purification of hexafluorobutadiene using 5A molecular sieves produces about 0.1% hexafluoro-2-butyne, affecting the production yield and purity. Chinese patent CN111285753A indicates that zeolite molecular sieves such as A-type molecular sieves, 2K-4, 2K-5, analcime, erionite, gmelinite and offretite have acid centers which can also catalyze the isomerization of hexafluorobutadiene to generate hexafluoro-2-butyne and hexafluorocyclobutene. Therefore, it is inevitably necessary to remove impurities generated by isomerization in the process for producing high-purity hexafluorobutadiene, but none of the above patent technologies can be effectively removed.
Chinese patent CN111285753A discloses a method for effectively controlling the content of an isomerized product, which uses an iridium pincer catalyst to reversely isomerize hexafluoro-2-butyne and hexafluoro-cyclobutene into hexafluorobutadiene, the total amount of hexafluoro-2-butyne and hexafluoro-cyclobutene after the reaction is less than 100ppm, but the catalyst is sensitive to moisture, and moisture needs to be removed to ppm level, which increases the difficulty of actual production. Meanwhile, the catalyst contains rare earth elements, wherein one kind of plutonium metal even has radioactivity, and belongs to a class of carcinogens, so that the catalyst is high in industrial use cost and has certain danger.
In addition, the related methods disclosed so far remove light components from the hexafluorobutadiene, but obviously, the hexafluorobutadiene is still the main component in the removed light components, and the content is very high, even more than 95%. None of the presently disclosed processes, however, include a process for recovering hexafluorobutadiene therefrom, resulting in lower recovery of hexafluorobutadiene.
Disclosure of Invention
The invention aims to provide a method for purifying hexafluorobutadiene with high recovery rate, which is used for simply, efficiently and inexpensively removing light components in the hexafluorobutadiene, particularly hexafluoro-2-butyne and hexafluoro-cyclobutene, recovering the hexafluorobutadiene from the removed light components and improving the recovery rate of the hexafluorobutadiene.
The purpose of the invention can be realized by the following technical scheme:
a process for the purification of hexafluorobutadiene with high recovery, which comprises:
introducing a hexafluorobutadiene raw material into a primary light component removal tower to remove light components, introducing a tower top extract of the primary light component removal tower into a recovery tower to perform light component concentration, and introducing a tower bottom extract into a secondary light component removal tower to remove the light components;
introducing the tower top extract of the secondary light component removal tower into a recovery tower for light component concentration, wherein the tower bottom extract is a purified hexafluorobutadiene product;
the tower top extract of the recovery tower is the concentrated light component, and the tower bottom extract is mixed with the hexafluorobutadiene raw material and then circularly introduced into the first-stage light component removal tower to remove the light component.
Further, the raw material of the hexafluorobutadiene contains hexafluorobutadiene and a light component, the volume fraction of the hexafluorobutadiene is more than or equal to 95%, and the light component is an organic matter which is contained in the raw material of the hexafluorobutadiene and has a lower normal-pressure boiling point than that of the hexafluorobutadiene.
Furthermore, the tower top and the tower kettle of the first-stage light component removal tower are continuously extracted; the top of the second-stage lightness-removing tower is intermittently extracted, and the bottom of the tower is continuously extracted; the top and the bottom of the recovery tower are continuously extracted.
Further, when the volume fraction of light components at the top of the secondary light component removal tower is higher than the upper content limit, the light components are extracted; when the volume fraction of the light components at the top of the secondary light component removal tower is lower than the lower limit of the content, stopping extracting, and carrying out total reflux; the upper limit of the content is 1000-5000ppm, and the lower limit of the content is 500-4000ppm.
Furthermore, the position of the tower top extract of the first-stage lightness-removing tower entering the recovery tower is higher than the position of the tower top extract of the second-stage lightness-removing tower entering the recovery tower.
Further, the tower top distillation rate of the first-stage light component removal tower is 5% -30%, the tower top distillation rate of the second-stage light component removal tower is 1% -10%, and the tower top distillation rate of the recovery tower is 8% -18%. In the tower kettle extract of the recovery tower, the volume fraction of the light components is lower than that in the tower top extract of the secondary light component removal tower.
Further, the tower kettle temperature of the first-stage light component removal tower is-5 ℃ to 40 ℃, the tower top temperature is-10 ℃ to 35 ℃, the operation pressure is 70 kPaA to 250kPaA, and the reflux ratio is 4 to 50; the tower kettle temperature of the secondary lightness-removing tower is-5 ℃ to 40 ℃, the tower top temperature is-10 ℃ to 35 ℃, the operation pressure is 70-250kPaA, and the reflux ratio is 10-125; the temperature of the tower bottom of the recovery tower is-5 ℃ to 40 ℃, the temperature of the tower top is-15 ℃ to 30 ℃, the operation pressure is 70 kPaA to 250kPaA, and the reflux ratio is 50 to 200.
Preferably, the operating pressure of the first-stage lightness-removing column and the second-stage lightness-removing column is 90-120kPaA, and the operating pressure of the recovery column is 90-150kPaA.
Furthermore, the tower kettle extract of the recovery tower is mixed with the hexafluorobutadiene raw material, and then is subjected to adsorption treatment, and then is introduced into the first-stage light component removal tower to remove light components, so that the light components can be removed more easily.
Further, the adsorption treatment is performed in an adsorption apparatus filled with an adsorbent. The adsorbent comprises one or more of zeolite molecular sieve, activated alumina or activated carbon, preferably a type a molecular sieve.
Furthermore, the operating pressure of the adsorption device is reduced pressure, normal pressure or micro-positive pressure, the operating temperature is 0-25 ℃, preferably 10-20 ℃, and the operating space velocity is 500-5000h -1 。
Compared with the prior art, the invention has the following characteristics:
1) According to the invention, a two-stage rectification method is adopted to deeply remove light components such as hexafluorocyclobutene, hexafluoro-2-butyne and the like in a hexafluorobutadiene raw material, the volume fraction of the light components can be reduced to below 10ppm, and single-stage high-efficiency rectification is utilized to recover the hexafluorobutadiene in the light components, so that the recovery rate of the hexafluorobutadiene is up to above 95%. The method has the advantages of safe and simple process, low maintenance cost, stable process and high recovery rate, and is very suitable for industrial production.
2) In the invention, the top of the secondary rectifying tower adopts an intermittent extraction mode, the process robustness is high, and the influence of the fluctuation of the raw materials on the treatment process is small.
Drawings
FIG. 1 is a schematic diagram of the purification scheme for hexafluorobutadiene in example 1;
FIG. 2 is a schematic diagram of the purification scheme for hexafluorobutadiene in example 2;
the notation in the figure is:
1-adsorption device, 2-first-stage lightness-removing tower, 3-second-stage lightness-removing tower and 4-recovery tower.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments. The present embodiment is implemented on the premise of the technical solution of the present invention, and a detailed implementation manner and a specific operation process are given, but the scope of the present invention is not limited to the following embodiments.
The purification method of the hexafluorobutadiene with high recovery rate comprises the following steps:
introducing a hexafluorobutadiene raw material into a primary light component removal tower 2 to remove light components, introducing a tower top extract of the primary light component removal tower 2 into a recovery tower 4 to concentrate the light components, and introducing a tower kettle extract into a secondary light component removal tower 3 to remove the light components; the tower top extract of the secondary light component removal tower 3 is fed into a recovery tower 4 for light component concentration, and the tower bottom extract is a purified hexafluorobutadiene product; the tower top extract of the recovery tower 4 is the concentrated light component, and the tower bottom extract is mixed with the hexafluorobutadiene raw material and then circularly introduced into the first-stage light component removal tower 2 to remove the light component. The volume fraction of the hexafluobutadiene in the raw material is more than 95 percent, and the light component is an organic matter which has a boiling point at normal pressure and is lower than that of the hexafluobutadiene in the raw material.
The raw material of the hexafluorobutadiene contains the hexafluorobutadiene and a light component, the volume fraction of the hexafluorobutadiene is more than or equal to 95%, and the light component is an organic matter which is contained in the raw material of the hexafluorobutadiene and has a lower normal-pressure boiling point than the hexafluorobutadiene.
The tower top and the tower kettle of the first-stage light component removal tower 2 are continuously extracted; the top of the second-stage lightness-removing tower 3 is intermittently extracted, and the bottom of the tower is continuously extracted; the top and the bottom of the recovery tower 4 are continuously extracted.
When the volume fraction of the light components at the top of the secondary light component removal tower 3 is higher than the upper limit of the content, the light components are extracted; when the volume fraction of the light components at the top of the secondary light component removal tower 3 is lower than the lower content limit, stopping extracting, and performing total reflux; the upper limit of the content is 1000-5000ppm, and the lower limit of the content is 500-4000ppm.
The position of the top extract of the first-stage lightness-removing column 2 entering the recovery column 4 is higher than the position of the top extract of the second-stage lightness-removing column 3 entering the recovery column 4.
The tower top distillation rate of the first-stage light component removal tower 2 is 5-30%, the tower top distillation rate of the second-stage light component removal tower 3 is 1-10%, and the tower top distillation rate of the recovery tower 4 is 8-18%.
The temperature of the tower kettle of the first-stage lightness-removing tower 2 is-5 ℃ to 40 ℃, the temperature of the tower top is-10 ℃ to 35 ℃, the operation pressure is 70-250kPaA, and the reflux ratio is 4-50; the temperature of the tower kettle of the secondary lightness-removing tower 3 is-5 ℃ to 40 ℃, the temperature of the tower top is-10 ℃ to 35 ℃, the operation pressure is 70-250kPaA, and the reflux ratio is 10-125; the temperature of the bottom of the recovery tower 4 is-5 ℃ to 40 ℃, the temperature of the top of the recovery tower is-15 ℃ to 30 ℃, the operation pressure is 70 kPaA to 250kPaA, and the reflux ratio is 50 to 200.
The tower kettle extract of the recovery tower 4 is mixed with the hexafluorobutadiene raw material, and then is subjected to adsorption treatment, and then is introduced into the first-stage light component removal tower 2 to remove light components.
The adsorption treatment is performed in the adsorption apparatus 1, and the adsorption apparatus 1 is filled with an adsorbent.
The operating pressure of the adsorption device 1 is reduced pressure, normal pressure or micro-positive pressure, the operating temperature is 0-25 ℃, and the operating airspeed is 500-5000h -1 。
The adsorption device 1 is added before the first-stage light component removal tower 2, so that light components can be removed from the raw materials, and the adsorbent in the adsorption device 1 can remove a large amount of halogenated hydrocarbons, so that the pressure of a subsequent light component removal tower is reduced, and the efficiency of the light component removal tower is improved. Meanwhile, the adsorption device 1 also has a removing capability on part of organic matters with the normal pressure boiling point higher than that of the hexafluorobutadiene.
Although isomerization reaction of hexafluorobutadiene also occurs inevitably in the adsorption apparatus 1, it can be controlled by the following measures: 1) Keeping the space velocity at 500h -1 The above; 2) Keeping the adsorption temperature below 25 ℃; 3) Using a type a molecular sieve; 4) The molecular sieve is roasted for more than 2 hours at 400-450 ℃ before use. After the above control method, the isomerization reaction occurs only limitedly in the adsorption operation. In addition, it has been found through repeated experiments that the volume fraction of hexafluoro-2-butyne and hexafluoro-cyclobutene produced by the isomerization can be controlled to 200ppm or less by the above-mentioned method. Even if hexafluoro-2-butyne and hexafluoro-cyclobutene are produced in the adsorption apparatus 1, most of them can be concentrated at the top of the column by the first-stage lightness-removing column 2 and the second-stage lightness-removing column 3, and the volume fraction of light components in the processed hexafluorobutadiene is still 10ppm or less.
In the above process, the intermittent extraction method of the secondary lightness-removing column 3 can improve the treatment efficiency and the recovery rate because the volume fraction of the light components in the feed of the column is very low, and in this case, the intermittent extraction can improve the volume fraction of the light components at the top of the column to the maximum extent, thereby exerting the efficiency of the secondary lightness-removing column 3 to the maximum extent. Another advantage of using the batch extraction method is that when the fluctuation of the light component content in the raw material is large, the secondary lightness-removing column 3 can stably obtain the qualified hexafluorobutadiene from the column bottom without being affected basically by adjusting the batch extraction time. If the top of the tower is continuously extracted, the flow needs to be controlled at a very small flow, so that the volume fraction of the enriched light component cannot reach the intermittent extraction degree, the recovery rate is low, and the light component is difficult to stably control in actual production and is greatly influenced by the fluctuation of raw materials.
In addition, any process and device which do not produce extra light components can be added before and after the adsorption device 1, the primary light component removal tower 2 and the secondary light component removal tower 3, and the final light component removal effect is not affected.
In the following examples, the composition of the hexafluorobutadiene feedstock to be treated is shown in Table 1 on a volume basis.
TABLE 1 raw material composition (volume fraction)
| Composition of raw materials | R-1 |
| Hexafluorobutadiene | 97％ |
| Light component organic matter | 2.5％ |
| Heavy organic fraction | 0.4％ |
| Others | 0.1％ |
Example 1:
the feed R-1 in Table 1 was processed using the scheme shown in FIG. 1.
The raw material is mixed with the tower bottom extract of the recovery tower 4 and then enters the 2/3 position of the rectifying column of the first-stage light component removing tower 2, the tower bottom extract of the first-stage light component removing tower 2 enters the 2/3 position of the rectifying column of the second-stage light component removing tower 3, the tower top extract of the first-stage light component removing tower 2 enters the 2/3 position of the rectifying column of the recovery tower 4, and the tower top extract of the second-stage light component removing tower 3 enters the 4/5 position of the rectifying column of the recovery tower. The tower top of the recovery tower 4 extracts the concentrated light components, and the tower bottom of the secondary light component removal tower 3 extracts the purified hexafluorobutadiene.
The operation pressure of the first-stage light component removal tower 2 and the second-stage light component removal tower 3 is 100kPaA, and the pressure of the recovery tower 4 is 120kPaA. The tower top distillation rates of the first-stage light component removal tower 2 and the recovery tower 4 are respectively 30% and 12.5%. The reflux ratio of the first-stage lightness-removing column 2 and the reflux ratio of the recovery column 4 are respectively 20 and 100. The second-stage rectifying tower 3 adopts an intermittent extraction mode, extraction is started when the volume fraction of light components at the top of the tower is higher than 4000ppm, the distillation rate at the top of the tower is 10 percent, the reflux ratio is 50, extraction is stopped when the volume fraction of the light components at the top of the tower is lower than 2500ppm, and total reflux is started.
The raw materials are processed according to the conditions that the temperatures of the tower kettle and the tower top of the first-stage light component removal tower 2 are respectively 6.5 ℃ and 4 ℃, the temperatures of the tower kettle and the tower top of the second-stage light component removal tower 3 are respectively 7 ℃ and 5 ℃, and the temperatures of the tower kettle and the tower top of the recovery tower 4 are respectively 10.5 ℃ and 6.5 ℃. The treated hexafluorobutadiene was withdrawn from the bottom of the second-stage lightness-removing column 3 and had a composition of P-1 (see Table 2), and the recovery rate was 95.3%.
Example 2:
the feed R-1 in Table 1 was processed using the scheme shown in FIG. 2.
The raw material and the tower bottom extract of the recovery tower 4 are mixed and then enter an adsorption device 1, the adsorbed material enters the 2/3 position of a rectifying column of a first-stage light component removal tower 2, the tower bottom extract of the first-stage light component removal tower 2 enters the 2/3 position of a rectifying column of a second-stage light component removal tower 3, the tower top extract of the first-stage light component removal tower 2 enters the 2/3 position of the rectifying column of the recovery tower 4, and the tower top extract of the second-stage light component removal tower 3 enters the 4/5 position of the rectifying column of the recovery tower. The tower top of the recovery tower 4 extracts the concentrated light components, and the tower kettle of the secondary light component removal tower 3 extracts the processed hexafluorobutadiene.
The adsorption apparatus 1 was charged with a spherical 5A molecular sieve having a diameter of 1mm and calcined at 450 ℃ for 4 hours before use. The operating pressure of the adsorption device 1 is 110kPaA, the operating temperature is 20 ℃, and the operating space velocity is 5000h -1 。
The operation pressure of the first-stage lightness-removing column 2 and the second-stage lightness-removing column 3 is 100kPaA, and the pressure of the recovery column 4 is 120kPaA. The tower top distillation rates of the first-stage light component removal tower 2 and the recovery tower 4 are respectively 20% and 10%. The reflux ratios of the first-stage lightness-removing column 2 and the recovery column 4 are 45 and 100 respectively. The second-stage rectifying tower 3 adopts an intermittent extraction mode, extraction is started when the volume fraction of light components at the top of the tower is higher than 3000ppm, the distillation rate at the top of the tower is 10 percent, the reflux ratio is 100, extraction is stopped when the volume fraction of the light components at the top of the tower is lower than 1500ppm, and total reflux is started.
The raw materials are processed according to the conditions that the temperatures of the tower kettle and the tower top of the first-stage lightness-removing tower 2 are respectively 6.5 ℃ and 4.5 ℃, the temperatures of the tower kettle and the tower top of the second-stage lightness-removing tower 3 are respectively 7 ℃ and 5 ℃, and the temperatures of the tower kettle and the tower top of the recovery tower 4 are respectively 10.5 ℃ and 6 ℃. The treated hexafluorobutadiene was withdrawn from the bottom of the second-stage lightness-removing column 3 and had a composition of P-2 (see Table 2), and the recovery rate was 97.2%.
TABLE 2 composition of the treated hexafluorobutadiene (volume fraction)
| Composition of treated hexafluorobutadiene | P-1 | P-2 |
| Hexafluorobutadiene | ＞99％ | ＞99％ |
| Light component | 10ppm | 7.5ppm |
| Heavy fraction | 0.4％ | 0.2％ |
| Others | 0.1％ | 0.1％ |
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make modifications and alterations without departing from the scope of the present invention.
Claims (7)
1. A method for purifying hexafluorobutadiene with high recovery rate is characterized in that the method comprises the following steps:
introducing a hexafluorobutadiene raw material into a first-stage light component removal tower to remove light components, introducing a tower top extract of the first-stage light component removal tower into a recovery tower to concentrate the light components, and introducing a tower kettle extract into a second-stage light component removal tower to remove the light components;
introducing the tower top extract of the secondary light component removal tower into a recovery tower for light component concentration, wherein the tower bottom extract is a purified hexafluorobutadiene product;
the tower top extract of the recovery tower is the concentrated light component, and the tower bottom extract is mixed with the hexafluorobutadiene raw material and then circularly introduced into the first-stage light component removal tower to remove the light component;
the raw material of the hexafluorobutadiene contains hexafluorobutadiene and a light component, the volume fraction of the hexafluorobutadiene is more than or equal to 95%, and the light component is an organic matter which is contained in the raw material of the hexafluorobutadiene and has a lower normal-pressure boiling point than that of the hexafluorobutadiene;
the top and the kettle of the first-stage lightness-removing tower are continuously extracted; the top of the second-stage lightness-removing tower is intermittently extracted, and the bottom of the tower is continuously extracted; the tower top and the tower kettle of the recovery tower are continuously extracted;
when the volume fraction of the light components at the top of the secondary light component removal tower is higher than 3000ppm, the light components are extracted; stopping extracting when the volume fraction of the light components at the top of the secondary light component removal tower is lower than 1500ppm, and carrying out total reflux.
2. The method for purifying hexafluorobutadiene with high recovery rate as claimed in claim 1, wherein the top extract of the primary lightness-removing column is fed into the recovery column at a position higher than that of the secondary lightness-removing column.
3. The method of claim 1, wherein the first-stage light component removal column has an overhead distillation rate of 5% to 30%, the second-stage light component removal column has an overhead distillation rate of 1% to 10%, and the recovery column has an overhead distillation rate of 8% to 18%.
4. The process of claim 1, wherein the column bottom temperature of the first-stage light component removal column is-5 ℃ to 40 ℃, the column top temperature is-10 ℃ to 35 ℃, the operation pressure is 70 kPaA to 250kPaA, and the reflux ratio is 4 to 50; the tower kettle temperature of the secondary lightness-removing tower is-5 ℃ to 40 ℃, the tower top temperature is-10 ℃ to 35 ℃, the operation pressure is 70-250kPaA, and the reflux ratio is 10-125; the temperature of the tower bottom of the recovery tower is-5 ℃ to 40 ℃, the temperature of the tower top is-15 ℃ to 30 ℃, the operation pressure is 70 kPaA to 250kPaA, and the reflux ratio is 50 to 200.
5. The method for purifying hexafluorobutadiene with high recovery rate as claimed in claim 1, wherein the mixture of the column bottom extract of the recovery column and the raw material of hexafluorobutadiene is first subjected to adsorption treatment, and then introduced into the first-stage lightness-removing column to remove light components.
6. The process according to claim 5, wherein the adsorption treatment is carried out in an adsorption apparatus packed with an adsorbent.
7. The process of claim 6, wherein the adsorption unit is operated at a reduced pressure, atmospheric pressure or slightly positive pressure, at a temperature of 0-25 ℃ and at a space velocity of 500-5000h -1 。
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