CN111960966B - Preparation method of chromatographic grade acetonitrile - Google Patents
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- CN111960966B CN111960966B CN202010959152.XA CN202010959152A CN111960966B CN 111960966 B CN111960966 B CN 111960966B CN 202010959152 A CN202010959152 A CN 202010959152A CN 111960966 B CN111960966 B CN 111960966B
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Abstract
The invention provides a preparation method of chromatographic grade acetonitrile, belonging to the technical field of chemical production. The method comprises the steps of firstly oxidizing industrial acetonitrile by fuming sulfuric acid under a reflux condition, then oxidizing the middle distillate collected in the previous step by adopting a peroxide reagent under the reflux condition, and finally rectifying to obtain high-purity acetonitrile to meet the chromatographic grade requirement; because the adopted oxidant is fuming sulfuric acid and a peroxidation reagent, the waste liquid generated in the production process is a conventional acid-base solution, the generation of manganese salt-containing waste liquid or high-phosphorus waste liquid when potassium permanganate or phosphorus pentoxide is adopted as the oxidant is avoided, and a large amount of waste liquid treatment cost is saved for downstream. The invention can obtain the chromatographic grade acetonitrile by rectification after two-step oxidation treatment without using an adsorption process, thereby avoiding the generation of a large amount of adsorption waste residues and waste gases, and having relatively simple process and higher product yield.
Description
Technical Field
The invention relates to the technical field of chemical production, in particular to a preparation method of chromatographic grade acetonitrile.
Background
The chromatographic grade acetonitrile has the characteristics of low ultraviolet absorption, low solid particles and volatile residues, is used as a chromatographic mobile phase, has small background noise signal and few abnormal peaks in a spectrogram, and has large demand in the fields of chromatographic analysis, drug separation and the like.
At present, the raw material for producing chromatographic grade acetonitrile in China is industrial grade acetonitrile, most of the industrial grade acetonitrile is a byproduct from the production of acrylonitrile by propylene ammoxidation, the impurity components are complex, and the common purification method generally comprises an adsorption process, an oxidation process and a distillation process. However, most of the adsorbents adopted in the adsorption process are activated carbon, graphene or carbon fibers, the regeneration of the adsorbents needs high-temperature firing, the large-scale production difficulty is high, waste gas is generated in the high-temperature firing process, and a large amount of waste residues are generated if the waste gas is not generated; in addition, the adsorbent has selectivity on the adsorption of impurities, has poor adsorption effect on partial organic matters, and can adsorb a large amount of acetonitrile while adsorbing the impurities, so that the product yield is reduced. The oxidant adopted in the oxidation procedure is usually potassium permanganate or phosphorus pentoxide, and manganese salt waste liquid or phosphorus-containing waste liquid can be generated in the using process, so that the cost is high in downstream wastewater treatment.
Disclosure of Invention
The invention aims to provide a preparation method of chromatographic grade acetonitrile, which has the advantages of simple process, high product yield, no waste residue, low treatment cost and no generation of waste liquid in the production process, wherein the waste liquid is a conventional acid-base solution.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of chromatographic grade acetonitrile, which comprises the following steps:
(1) mixing industrial acetonitrile and fuming sulfuric acid, heating to 80-90 ℃, refluxing for 30-60 min, then starting to extract, discarding front fraction, and collecting middle fraction;
(2) mixing the middle fraction obtained in the step (1) with a peroxidation reagent, heating to 80-90 ℃, refluxing for 30-60 min, then starting to extract, discarding the front fraction, and collecting the middle fraction; the peroxidation reagent is sodium peroxide, potassium peroxide or aqueous hydrogen peroxide, and the mass fraction of hydrogen peroxide in the aqueous hydrogen peroxide is 50-60%;
(3) and (3) heating the middle distillate obtained in the step (2) to 80-90 ℃ for rectification to obtain chromatographic grade acetonitrile.
Preferably, the mass fraction of free sulfur trioxide in the oleum in the step (1) is 20-25%.
Preferably, the mass ratio of the industrial-grade acetonitrile to the oleum in the step (1) is 1000: (1-80).
Preferably, during the extraction process in the step (1), when the absorbance of the extracted sample under the condition of 210nm is less than or equal to 0.10, starting to collect the middle fraction; when the temperature of the system is more than 90 ℃, the collection of the middle distillate is stopped.
Preferably, the mass ratio of the middle fraction to the peroxidation reagent in the step (1) is 950: (1-8.5).
Preferably, during the extraction process in the step (2), when the absorbance of the extracted sample under the condition of 210nm is less than or equal to 0.07, the collection of the middle distillate is started; when the temperature of the system is more than 90 ℃, the collection of the middle distillate is stopped.
Preferably, the reflux ratio in the rectification in the step (3) is 5: (0.5-2).
Preferably, the rectifying in the step (3) comprises: heating the middle fraction obtained in the step (2) to 80-90 ℃, refluxing for 60-90 min, then starting to collect, discarding the front fraction, and collecting the middle fraction as chromatographic grade acetonitrile.
Preferably, during the extraction process in the step (3), when the absorbance of the extracted sample at 210nm is less than or equal to 0.04, starting to collect the middle fraction; when the temperature of the system is more than 90 ℃, the collection of the middle distillate is stopped.
Preferably, the step (3) further comprises, after collecting the middle distillate: filtering the middle fraction; the pore size of the filtration membrane used for filtration was 0.22. mu.m.
The invention provides a preparation method of chromatographic grade acetonitrile, which comprises the following steps: (1) mixing industrial acetonitrile and fuming sulfuric acid, heating to 80-90 ℃, refluxing for 30-60 min, then starting to extract, discarding front fraction, and collecting middle fraction; (2) mixing the middle fraction obtained in the step (1) with a peroxidation reagent, heating to 80-90 ℃, refluxing for 30-60 min, then starting to extract, discarding the front fraction, and collecting the middle fraction; the peroxidation reagent is sodium peroxide, potassium peroxide or aqueous hydrogen peroxide, and the mass fraction of hydrogen peroxide in the aqueous hydrogen peroxide is 50-60%; (3) and (3) heating the middle distillate obtained in the step (2) to 80-90 ℃ for rectification to obtain chromatographic grade acetonitrile.
The method comprises the steps of firstly, oxidizing industrial acetonitrile by fuming sulfuric acid under a reflux condition, opening double bonds in unsaturated compounds such as pyridine, oxazole and the like in the industrial acetonitrile, enabling impurities and impurities to have polymerization reaction, generating high molecular substances or high boiling point substances, and removing the high molecular substances or the high boiling point substances through distillation; then, oxidizing the intermediate fraction collected in the previous step again by using a peroxide reagent under the reflux condition, so that the unoxidized impurities in the intermediate fraction can be further oxidized, and particularly if sodium peroxide or potassium peroxide is used, the acidic impurities such as hydrocyanic acid and organic acids generated by oxidizing aldehyde substances remained in the intermediate fraction can be neutralized by alkaline substances (such as sodium hydroxide or potassium hydroxide) generated by oxidation; finally, high-purity acetonitrile is obtained through rectification, and the requirements of chromatographic grade are met.
In addition, the method provided by the invention adopts fuming sulfuric acid and a peroxidation reagent as the oxidant, and the waste liquid generated in the production process is a conventional acid-base solution, so that the problem of generating manganese salt-containing waste liquid or high-phosphorus waste liquid when potassium permanganate or phosphorus pentoxide is adopted as the oxidant can be effectively solved, and a large amount of waste liquid treatment cost is saved for downstream.
Furthermore, the invention can obtain the chromatographic grade acetonitrile by rectification after two-step oxidation treatment without using an adsorption process, thereby avoiding the generation of a large amount of adsorption waste residues and waste gases, and having relatively simple process and higher product yield.
Drawings
FIG. 1 is a GC spectrum of a semi-finished product prepared in example 1;
FIG. 2 is a GC spectrum of the final product prepared in example 1.
Detailed Description
The invention provides a preparation method of chromatographic grade acetonitrile, which comprises the following steps:
(1) mixing industrial acetonitrile and fuming sulfuric acid, heating to 80-90 ℃, refluxing for 30-60 min, then starting to extract, discarding front fraction, and collecting middle fraction;
(2) mixing the middle fraction obtained in the step (1) with a peroxidation reagent, heating to 80-90 ℃, refluxing for 30-60 min, then starting to extract, discarding the front fraction, and collecting the middle fraction; the peroxidation reagent is sodium peroxide, potassium peroxide or aqueous hydrogen peroxide, and the mass fraction of hydrogen peroxide in the aqueous hydrogen peroxide is 50-60%;
(3) and (3) heating the middle distillate obtained in the step (2) to 80-90 ℃ for rectification to obtain chromatographic grade acetonitrile.
In the present invention, unless otherwise specified, all reagents used are commercially available products well known to those skilled in the art.
According to the invention, industrial acetonitrile and fuming sulfuric acid are mixed and heated to 80-90 ℃, reflux is carried out for 30-60 min, then extraction is started, front fraction is discarded, and middle fraction is collected. In the present invention, the industrial grade acetonitrile is preferably purchased from Shanghai Saikeke petrochemical Co., Ltd or Qilu petrochemical Co., Ltd. In the invention, the mass fraction of free sulfur trioxide in the oleum is preferably 20-25%; the oleum is preferably purchased from Populus state Fungification chemical Co., Ltd or Jingteng chemical Co., Ltd. In the present invention, the mass ratio of the technical grade acetonitrile to oleum is preferably 1000: (1 to 80), more preferably 1000: (10-80). In the present invention, the technical grade acetonitrile is preferably mixed with oleum in such a manner that oleum is added to the technical grade acetonitrile.
In the invention, the temperature of the reflux (marked as first reflux) is 80-90 ℃, and the reflux is started to be extracted after 30-60 min; in the extraction process, when the absorbance of the extracted sample under the condition of 210nm is less than or equal to 0.10, preferably starting to collect the middle fraction (marked as a first middle fraction); when the system temperature is >90 ℃, collection of the first middle distillate is preferably stopped. In the invention, the first reflux is specifically total reflux, and the reflux ratio is not required to be controlled. In the present invention, the first reflux is preferably carried out under stirring conditions, and the stirring rate is not particularly limited in the present invention, and may be a stirring rate well known to those skilled in the art.
In the invention, main impurities in industrial acetonitrile are hydrocyanic acid, propionitrile, benzonitrile, acetone, acrolein, pyridine, oxazole and the like, and fuming sulfuric acid is used as an oxidant to oxidize the industrial acetonitrile under a reflux condition, so that double bonds in unsaturated compounds such as pyridine, oxazole and the like can be opened, polymerization reaction is carried out between the impurities, high molecular substances or high boiling point substances are generated, and the high molecular substances or the high boiling point substances are removed by distillation; oleum can also oxidize aldehydes to organic acids, which are removed by distillation.
After the first intermediate fraction is obtained, the first intermediate fraction and a peroxidation reagent are mixed and heated to 80-90 ℃, reflux is carried out for 30-60 min, then, extraction is carried out, the front fraction is discarded, and the intermediate fraction is collected; the peroxidation reagent is sodium peroxide, potassium peroxide or aqueous hydrogen peroxide, and the mass fraction of hydrogen peroxide in the aqueous hydrogen peroxide is 50-60%. In the present invention, the mass ratio of the first intermediate fraction to the peroxidation agent is preferably 950: (1 to 8.5), more preferably 950: (7.5-8).
In the invention, the temperature of the reflux (marked as second reflux) is 80-90 ℃, and the extraction is started after 30-60 min of reflux; in the extraction process, when the absorbance of the extracted sample under the condition of 210nm is less than or equal to 0.07, preferably starting to collect the middle fraction (marked as a second middle fraction); when the system temperature is >90 ℃, collection of the second middle distillate is preferably stopped. In the present invention, the second reflux is specifically a full reflux, and the reflux ratio does not need to be controlled. In the present invention, the second reflux is preferably carried out under stirring conditions, and the stirring rate is not particularly limited in the present invention, and may be a stirring rate well known to those skilled in the art.
The invention adopts a peroxidation reagent as an oxidant, and the collected first middle distillate is oxidized under reflux conditions, so that the unoxidized impurities in the first middle distillate can be further oxidized, and particularly if sodium peroxide or potassium peroxide is adopted, the sodium hydroxide or potassium hydroxide generated by oxidation can neutralize the acid impurities such as hydrocyanic acid and organic acid generated by oxidizing aldehyde substances in the first middle distillate.
After the second intermediate fraction is obtained, heating the second intermediate fraction to 80-90 ℃ for rectification to obtain chromatographic grade acetonitrile. In the present invention, the rectification preferably comprises: and heating the second intermediate fraction to 80-90 ℃, refluxing for 60-90 min, then starting to extract, discarding the front fraction, and collecting the intermediate fraction as chromatographic grade acetonitrile.
In the invention, the temperature of the reflux (marked as third reflux) is 80-90 ℃, and the reflux is started to be extracted after 60-90 min; in the extraction process, when the absorbance of the extracted sample under the condition of 210nm is less than or equal to 0.04, preferably starting to collect the middle fraction (marked as a third middle fraction); when the system temperature is >90 ℃, the collection of the third middle distillate is preferably stopped. In the present invention, in the rectification, the reflux ratio at the time of withdrawal is preferably 5: (0.5 to 2), more preferably 5: (1-2).
In the present invention, it is preferable that the collecting of the third middle fraction further comprises: filtering the third middle fraction to obtain a filtrate of chromatographic grade acetonitrile; the pore size of the filtration membrane used for filtration is preferably 0.22. mu.m. The absorbance of the chromatographic grade acetonitrile prepared by the method is less than or equal to 0.037 under the wavelength condition of 190nm, less than or equal to 0.002 under the wavelength condition of 200nm, less than or equal to 0.002 under the wavelength condition of 210nm, less than or equal to 0.001 under the wavelength condition of 220nm, and 0 under the wavelength condition of 230nm to 254 nm.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Adding 10g of oleum (20-25% by mass of free sulfur trioxide purchased from Yang Zhou Hua Fuji Co., Ltd.) into 1000g of industrial acetonitrile (purchased from Qilu petrochemical Co., Ltd.), heating and refluxing for 60min under stirring, and controlling the temperature of the system to be 80-90 ℃; then, the extraction is started, 10mL of front cut fraction is discarded, and the absorbance of the front cut fraction under the condition of 210nm is more than 0.10; when the absorbance of the sample to be extracted under the condition of 210nm is less than or equal to 0.10, starting to collect middle distillate, and when the temperature of the system is higher than 90 ℃, stopping collecting the middle distillate, and collecting 950g of the middle distillate;
adding 7.5g of sodium peroxide into the middle distillate, heating and refluxing for 60min under the stirring condition, and controlling the temperature of the system to be 80-90 ℃; then, the extraction is started, 10mL of front fraction is discarded, and the absorbance of the front fraction at 210nm is more than 0.07; when the absorbance of the extracted sample under the condition of 210nm is less than or equal to 0.07, starting to collect the middle fraction, when the temperature of the system is higher than 90 ℃, stopping collecting the middle fraction, and collecting 900g of the middle fraction in total to obtain a semi-finished product;
transferring the semi-finished product into a rectifying tower, controlling the temperature of the system to be 80-90 ℃, and refluxing for 70 min; then, production is started, and the reflux ratio is controlled to be 5: 1, discarding 10mL of the front fraction, wherein the absorbance of the front fraction at 210nm is more than 0.04; and when the absorbance of the extracted sample under the condition of 210nm is less than or equal to 0.04, starting to collect the middle fraction, stopping collecting the middle fraction when the temperature of the system is higher than 90 ℃, collecting 820g of the middle fraction totally, and filtering the mixture by a 0.22-micrometer filtering membrane to obtain a finished product, wherein the yield is 82%.
And performing GC analysis on the semi-finished product and the finished product, wherein the result is shown in a figure 1-2, wherein the figure 1 is a GC spectrogram of the semi-finished product, and the figure 2 is a GC spectrogram of the finished product. The data information for each component in fig. 1 and 2 is shown in fig. 1 and table 2.
TABLE 1 data information on the GC spectra of the intermediates of example 1
| Retention time/min | Type (B) | Peak width/min | Peak area | Height | Peak area/% | Name (R) |
| 2.831 | BB | 0.06 | 0.32 | 0.21 | 0.001 | - |
| 2.888 | BV | 0.03 | 0.23 | 0.21 | 0.001 | - |
| 2.942 | VV | 0.50 | 24936.03 | 13663.18 | 99.996 | Acetonitrile |
| 4.053 | VB | 0.10 | 0.45 | 0.22 | 0.002 | - |
TABLE 2 data information for each component in GC spectra of the finished product in example 1
| Retention time/min | Type (B) | Peak width/min | Peak area | Height | Peak area/% | Name (R) |
| 2.939 | VV | 0.35 | 26462.57 | 13168.82 | 99.995 | Acetonitrile |
| 3.249 | VV | 0.17 | 1.35 | 0.22 | 0.005 | - |
The semi-finished and finished products were subjected to absorbance measurements and compared with commercially available products (purchased from merck) and the results are shown in table 3;
TABLE 3 absorbance values of semi-finished, finished and commercial products of example 1
As can be seen from Table 3 and the results of FIGS. 1-2, the mass of the chromatographic grade acetonitrile prepared by the method of the present invention is substantially equivalent to that of Merck.
Example 2
Adding 800g of fuming sulfuric acid (the mass fraction of free sulfur trioxide is 20-25%, purchased from Jingteng chemical Co., Ltd.) into 10.0kg of industrial acetonitrile (purchased from Shanghai Seisaku petrochemical Co., Ltd.), heating and refluxing for 60min under the stirring condition, and controlling the system temperature to be 80-90 ℃; then, starting to produce, and discarding 100mL of front fraction, wherein the absorbance of the front fraction at 210nm is more than 0.10; when the absorbance of the extracted sample under the condition of 210nm is less than or equal to 0.10, starting to collect the middle fraction, and when the temperature of the system is higher than 90 ℃, stopping collecting the middle fraction, and collecting 9.5kg of the middle fraction in total;
adding 80.0g of potassium peroxide into the middle distillate, heating and refluxing for 60min under the stirring condition, and controlling the temperature of the system to be 80-90 ℃; then, the extraction is started, 10mL of front fraction is discarded, and the absorbance of the front fraction at 210nm is more than 0.07; when the absorbance of the extracted sample under the condition of 210nm is less than or equal to 0.07, starting to collect the middle fraction, when the temperature of the system is higher than 90 ℃, stopping collecting the middle fraction, and collecting 9.1kg of the middle fraction in total to obtain a semi-finished product;
transferring the semi-finished product into a rectifying tower, controlling the temperature of the system to be 80-90 ℃, and refluxing for 30 min; then, production is started, and the reflux ratio is controlled to be 5: 2, discarding 100mL of the front fraction, wherein the absorbance of the front fraction at 210nm is more than 0.04; and when the absorbance of the extracted sample under the condition of 210nm is less than or equal to 0.04, starting to collect the middle fraction, stopping collecting the middle fraction when the temperature of the system is higher than 90 ℃, collecting 8.35kg of the middle fraction totally, and filtering the middle fraction by a 0.22-micrometer filtering membrane to obtain a finished product, wherein the yield is 83.5%.
The semi-finished and finished products were measured for absorbance and compared to commercially available products (purchased from merck) and the results are shown in table 4.
TABLE 4 absorbance values of semi-finished, finished and commercial products of example 2
As can be seen from Table 4, the chromatographic grade acetonitrile prepared by the process of the present invention has a substantially equivalent mass to that of Merck.
Comparative example 1
Adding 10g of concentrated sulfuric acid (with the concentration of 92.5-98 wt%) into 1000g of industrial-grade acetonitrile (purchased from Qilu petrochemical company Limited), heating and refluxing for 60min under the condition of stirring, and controlling the temperature of the system to be 80-90 ℃; then, the extraction is started, 10mL of front cut fraction is discarded, and the absorbance of the front cut fraction under the condition of 210nm is more than 0.10; when the absorbance of the sample to be extracted under the condition of 210nm is less than or equal to 0.10, starting to collect middle distillate, and when the temperature of the system is higher than 90 ℃, stopping collecting the middle distillate, and collecting 950g of the middle distillate;
adding 7.5g of sodium peroxide into the middle distillate, heating and refluxing for 60min under the stirring condition, and controlling the temperature of the system to be 80-90 ℃; then, the extraction is started, 10mL of front fraction is discarded, and the absorbance of the front fraction at 210nm is more than 0.07; when the absorbance of the extracted sample under the condition of 210nm is less than or equal to 0.07, starting to collect the middle fraction, when the temperature of the system is higher than 90 ℃, stopping collecting the middle fraction, and collecting 900g of the middle fraction in total to obtain a semi-finished product;
transferring the semi-finished product into a rectifying tower, controlling the temperature of the system to be 80-90 ℃, and refluxing for 70 min; then, production is started, and the reflux ratio is controlled to be 5: 1, discarding 10mL of the front fraction, wherein the absorbance of the front fraction at 210nm is more than 0.04; and when the absorbance of the extracted sample under the condition of 210nm is less than or equal to 0.04, starting to collect the middle fraction, stopping collecting the middle fraction when the temperature of the system is higher than 90 ℃, collecting 810g of the middle fraction totally, and filtering the middle fraction by using a 0.22-micrometer filtering membrane to obtain a finished product, wherein the yield is 81%.
The semi-finished and finished products were subjected to absorbance measurements and compared with the product of example 1, and the results are shown in Table 5.
TABLE 5 absorbance values for semi-finished, finished and commercial products of comparative example 1
As can be seen from Table 5, the method firstly adopts fuming sulfuric acid to oxidize the industrial acetonitrile under the reflux condition, and then adopts a peroxidation reagent to oxidize the industrial acetonitrile, so that the method has good effect of removing impurities in the industrial acetonitrile by oxidation and is far superior to concentrated sulfuric acid.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (8)
1. A method for preparing chromatographic grade acetonitrile comprises the following steps:
(1) mixing industrial acetonitrile and fuming sulfuric acid, heating to 80-90 ℃, refluxing for 30-60 min, then starting to extract, discarding front fraction, and collecting middle fraction; the mass fraction of free sulfur trioxide in the oleum in the step (1) is 20-25%;
(2) mixing the middle fraction obtained in the step (1) with a peroxidation reagent, heating to 80-90 ℃, refluxing for 30-60 min, then starting to extract, discarding the front fraction, and collecting the middle fraction; the peroxidation reagent is sodium peroxide, potassium peroxide or aqueous hydrogen peroxide, and the mass fraction of hydrogen peroxide in the aqueous hydrogen peroxide is 50-60%;
(3) heating the middle distillate obtained in the step (2) to 80-90 ℃ for rectification to obtain chromatographic grade acetonitrile; the reflux ratio during rectification is 5: (0.5-2).
2. The preparation method according to claim 1, wherein the mass ratio of the industrial-grade acetonitrile to the oleum in the step (1) is 1000: (1-80).
3. The preparation method according to claim 1, wherein during the extraction in the step (1), when the absorbance of the extracted sample at 210nm is less than or equal to 0.10, the collection of the middle distillate is started; when the temperature of the system is more than 90 ℃, the collection of the middle distillate is stopped.
4. The preparation method according to claim 1, wherein the mass ratio of the middle fraction to the peroxidation reagent in the step (1) is 950: (1-8.5).
5. The preparation method according to claim 1, wherein during the extraction in the step (2), when the absorbance of the extracted sample at 210nm is less than or equal to 0.07, the collection of the middle distillate is started; when the temperature of the system is more than 90 ℃, the collection of the middle distillate is stopped.
6. The production method according to claim 1, wherein the rectifying in the step (3) comprises: heating the middle fraction obtained in the step (2) to 80-90 ℃, refluxing for 60-90 min, then starting to collect, discarding the front fraction, and collecting the middle fraction as chromatographic grade acetonitrile.
7. The preparation method according to claim 6, wherein during the extraction in the step (3), when the absorbance of the extracted sample at 210nm is less than or equal to 0.04, the collection of the middle distillate is started; when the temperature of the system is more than 90 ℃, the collection of the middle distillate is stopped.
8. The method according to claim 7, wherein the step (3) further comprises, after collecting the middle distillate: filtering the middle fraction; the pore size of the filtration membrane used for filtration was 0.22. mu.m.
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