CN109456162B - Method for purifying chromatographically pure 4-methyl-2-pentanone - Google Patents
Method for purifying chromatographically pure 4-methyl-2-pentanone Download PDFInfo
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Abstract
The invention relates to a method for purifying chromatographically pure 4-methyl-2-pentanone, which comprises the following steps: the method comprises the steps of oxidizing 4-methyl-2-pentanone serving as a raw material by an IBX selective oxidant, and oxidizing 4-methyl-2-pentanol and other alcohol impurities in the 4-methyl-2-pentanone into ketones; secondly, acidic impurities are removed through adsorption of active alumina; drying and dewatering the three by calcium sulfate to obtain chromatographically pure 4-methyl-2-pentanone; fourthly, further removing moisture and acidic impurities in the sample through a ZSM-5 basic molecular sieve to obtain chromatographically pure 4-methyl-2-pentanone; the water content of the 4-methyl-2-pentanone product obtained through the rectification can reach below 0.02% and the purity is over 99.7%. According to the invention, IBX oxidant is adopted to effectively convert 4-methyl-2-pentanol impurities into 4-methyl-2-pentanone, so that other impurities are effectively avoided, then basic molecular sieve is adopted to adsorb and remove acidic impurities and a small amount of water, and a chromatographic 4-methyl-2-pentanone product with the purity of more than or equal to 99.7% is obtained through two-step rectification.
Description
Technical Field
The invention belongs to the field of chemical reagents, and relates to a purification method of chromatographically pure 4-methyl-2-pentanone.
Background
4-methyl-2-pentanone is a colorless, transparent, stable-performance liquid with aromatic odor, slightly soluble in water, easily soluble in a large amount of organic solvents, and widely applicable to medium-boiling-point solvents and chemical intermediates.
4-methyl-2-pentanone is a very common high-purity solvent and has the advantages of colorless and stable chemical properties; 4-methyl-2-pentanone has good solubility and is not easy to volatilize, and according to the characteristic, the 4-methyl-2-pentanone is widely applied to the industries of coatings, fuels, medicines, chemical engineering and the like.
At present, the domestic related explanations on the further purification method of high-purity 4-methyl-2-pentanone are less, the 4-methyl-2-pentanone raw material often contains alcohol impurities such as acetone, isopropanol, 4-methyl-2-pentanol and the like, and the standard (99.7%) of chromatographically pure 4-methyl-2-pentanone can not be achieved by using a common treatment method. Therefore, the invention aims to provide a method for purifying chromatographically pure 4-methyl-2-pentanone.
Disclosure of Invention
The invention aims to provide a method for purifying chromatographically pure 4-methyl-2-pentanone, which can obtain a chromatographically pure 4-methyl-2-pentanone product with the purity of more than or equal to 99.7 percent and the yield of more than or equal to 93 percent.
The technical scheme for realizing the purpose of the invention is as follows:
a method for purifying chromatographically pure 4-methyl-2-pentanone comprises the following steps
The method comprises the steps of adsorbing a raw material, namely 4-methyl-2-pentanone, by an IBX selective oxidant, and oxidizing 4-methyl-2-pentanol and other alcohol impurities in the 4-methyl-2-pentanone into ketones;
adsorbing and removing impurities by active alumina;
drying and dewatering the three by using calcium sulfate;
fourthly, further removing moisture and acidic impurities in the sample through a ZSM-5 basic molecular sieve to obtain chromatographically pure 4-methyl-2-pentanone;
the purity of the 4-methyl-2-pentanone product obtained by the rectification is more than 99.7%.
Moreover, the specific purification scheme is as follows:
the method comprises the following steps of: adding a proper amount of IBX oxidant into a 4-methyl-2-pentanone raw material to oxidize 4-methyl-2-pentanol and some alcohol impurities;
the first adsorption step: pumping the oxidized 4-methyl-2-pentanone product into an activated alumina adsorption column, wherein the filtration flow rate is 200-300 mL/min;
drying: using anhydrous calcium sulfate as a drying agent to adsorb and remove water;
fourth, an adsorption step two: introducing the dried 4-methyl-2-pentanone into an alkaline molecular sieve adsorption column for filtering, and pouring the 4-methyl-2-pentanone after further removing water and acidic impurities into a rectifying still for later use;
step I of rectification: the rectification conditions are adjusted as follows: the temperature of the bottom of the rectifying kettle is 100-120 ℃, the temperature of liquid in the kettle is controlled between 80-100 ℃, and low-boiling-point impurities are removed;
sixthly, rectification step two: the rectification conditions are adjusted as follows: the temperature of the bottom of the rectifying kettle is 200-300 ℃, the temperature of liquid in the rectifying kettle is controlled to be 120-150 ℃, the temperature of the top of the rectifying kettle is 117-118 ℃, the reflux ratio is controlled to be 1: 0.5-4, front fractions are discarded, and fractions at 115-116 ℃ are collected after the light absorption value is detected to be qualified; and filling nitrogen into the distillate and filling.
The purity of the starting material, 4-methyl-2-pentanone, was about 98.5%, and the water content was 0.5%.
Moreover, the drying agent is analytically pure anhydrous calcium sulfate.
Furthermore, the IBX oxidant is chemically named 2-iodoxybenzoic acid.
The height of the molecular sieve adsorption column is 1.0m, the diameter of the molecular sieve adsorption column is 4.2cm, the molecular sieve subjected to alkali treatment is used as a drying agent in the molecular sieve adsorption column, and the drying agent accounts for 2/3 of the drying column.
And the alkaline molecular sieve adsorption column is used for adsorption of a modified ZSM-5 molecular sieve.
And the modified ZSM-5 molecular sieve is soaked at high temperature for 60-120 min by taking sodium hydroxide as an alkali source and then heated and dried at 120 ℃.
The chromatographic pure 4-methyl-2-pentanone has the following detection indexes:
the invention has the advantages that:
1. the 4-methyl-2-pentanone raw material is often accompanied with some acidic impurities, and the ZSM-5 basic molecular sieve adsorption column is adopted in the invention, so that the acidic impurities can be removed, and the water content in the 4-methyl-2-pentanone raw material can be reduced.
2. According to the invention, the IBX oxidant is adopted, the oxidant has good selectivity, 4-methyl-2-pentanol impurities in 4-methyl-2-pentanone are reduced into 4-methyl-2-pentanone, the yield of the 4-methyl-2-pentanone is improved, the reaction can be carried out at normal temperature, the reaction is mild, and the safety is high.
3. The invention can obtain the chromatographic 4-methyl-2-pentanone product with the purity of more than or equal to 99.7 percent and the yield of more than or equal to 93 percent.
Detailed description of the preferred embodiments
The features of the present invention and other related features are described in further detail below by way of examples for the understanding of the skilled person:
a method for purifying chromatographically pure 4-methyl-2-pentanone comprises the following production processes:
the method has the advantages that 4-methyl-2-pentanol and other alcohol impurities in 4-methyl-2-pentanone are oxidized into ketones through the IBX selective oxidant, so that the recovery rate of the 4-methyl-2-pentanone can be improved, and a part of impurities can be removed.
Adsorbable acidic impurities are removed through two-step adsorption of active alumina and a ZSM-5 basic molecular sieve.
And thirdly, the calcium sulfate and the ZSM-5 basic molecular sieve are used for two-step drying and water removal, so that the water content in the 4-methyl-2-pentanone is reduced, and the 4-methyl-2-pentanone and water are prevented from forming an azeotrope.
The water content of the purified 4-methyl-2-pentanone product can reach below 0.02 percent, and the purity of the product is more than 99.7 percent.
A method for purifying chromatographically pure 4-methyl-2-pentanone comprises the following specific purification scheme:
the method comprises the following steps of: adding proper IBX oxidant into 4-methyl-2-pentanone material to oxidize 4-methyl-2-pentanol and some alcohol impurity.
The first adsorption step: and (3) pumping the oxidized 4-methyl-2-pentanone product into an activated alumina adsorption column to remove acidic impurities, wherein the filtering flow rate is 200-300 mL/min.
Drying: the Karl Fischer method is used for detecting the water content in the 4-methyl-2-pentanone raw material, if the water content is high, a drying agent is used for removing water, 4-methyl-2-pentanone and water easily form an azeotrope, the boiling point of the azeotrope is 87.9 ℃, the boiling point of 4-methyl-2-pentanone is 115.85 ℃, and if the water content is not removed firstly, the azeotropic phenomenon is easily caused.
Fourth, an adsorption step two: and (3) introducing the dried 4-methyl-2-pentanone into a ZSM-5 basic molecular sieve adsorption column for filtering, and pouring the 4-methyl-2-pentanone after further removing water and acidic impurities into a rectifying still for later use.
Step I of rectification: the rectification conditions are adjusted as follows: the temperature of the bottom of the rectifying kettle is 100-120 ℃, the liquid temperature in the kettle is controlled between 80-100 ℃, and low-boiling-point impurities such as acetone, isopropanol and the like are removed.
Sixthly, rectification step two: the rectification conditions are adjusted as follows: the temperature of the bottom of the rectifying kettle is 200-300 ℃, the temperature of liquid in the rectifying kettle is controlled to be 120-150 ℃, the temperature of the top of the rectifying kettle is 117-118 ℃, the reflux ratio is controlled to be 1: 0.5-4, front fractions are discarded, fractions at the temperature of 115-116 ℃ are collected after the light absorption value is detected to be qualified, and some high-boiling-point impurities in the bottom of the rectifying kettle are discarded.
Filling with nitrogen and killing: the product is automatically filled with nitrogen and packaged into 500mL, 1L and 4L to obtain the chromatographic pure 4-methyl-2-pentanone finished product.
The purity of the raw material 4-methyl-2-pentanone is about 98.5%, and the water content is 0.5%. The drying agent is analytically pure anhydrous calcium sulfate. The IBX oxidant is chemically named 2-iodoxybenzoic acid and is a very good selective oxidant, and IBX can oxidize various types of alcohols into corresponding aldehydes or ketones under room temperature conditions. High yield and convenient operation.
The purity of the activated alumina was 97%. The height of the molecular sieve adsorption column is 1.0m, the diameter is 4.2cm, the molecular sieve subjected to alkali treatment is used as a drying agent in the molecular sieve adsorption column, and the drying agent accounts for 2/3 of the drying column.
The alkaline molecular sieve adsorption column is used for adsorbing a ZSM-5 molecular sieve, the ZSM-5 molecular sieve is obtained by modifying a zeolite molecular sieve, the zeolite molecular sieve is a crystalline aluminosilicate microporous material and has a regular pore channel structure, strong acidity and high hydrothermal stability, and the size of a pore channel of the zeolite molecular sieve is generally 0.3-1.0 nm, so that the diffusion speed of molecules in the pore channel of the zeolite is low, and the effective utilization rate of the zeolite is reduced. By using sodium hydroxide as an alkali source and soaking for 60-120 min at high temperature, the molecular sieve is subjected to framework silicon removal, so that the pore diameter is enlarged, and the adsorption performance of the molecular sieve is enhanced.
Example 1:
a method for purifying chromatographically pure 4-methyl-2-pentanone comprises the following steps: the purification steps are as follows:
1) and (3) oxidation: the method comprises the steps of putting a 4-methyl-2-pentanone raw material into a rectifying still, adding IBX oxidant according to 0.2-0.5% of the raw material by mass, and stirring and reacting for 30-60 min.
2) A first adsorption step: and (3) adsorbing and removing impurities from the oxidized 4-methyl-2-pentanone through an activated alumina adsorption column, and adsorbing and filtering the impurities through activated alumina with the height of 1m and the diameter of 10cm at the filtering speed of 100-200 mL/min.
3) And (3) drying: and (3) filtering the adsorbed 4-methyl-2-pentanone raw material through a calcium sulfate filter column with the height of 1m and the diameter of 10cm at a filtering speed of 50-100 mL/min until the water content is below 0.1%.
4) And (2) an adsorption step II: and (3) introducing the dried 4-methyl-2-pentanone into an alkaline molecular sieve adsorption column for filtration, and pouring the 4-methyl-2-pentanone subjected to further moisture and acidic impurities removal into a rectifying still for later use. The height of the adsorption column is 1m, the diameter is 4.2cm, the built-in adsorbent is an alkaline molecular sieve, the volume of the built-in adsorbent is 2/3 of the volume of the adsorption column, and the flow rate is controlled to be 50-100 mL/min.
5) A first rectification step: the temperature of the bottom of the rectifying kettle is 100-120 ℃, the liquid temperature in the kettle is controlled between 80-100 ℃, the time is 4-6 hours, low boiling point impurities such as acetone, isopropanol and the like are removed by rectification, and the rectified finished product is poured into a recovery barrel.
6) And a second rectification step: the rectification conditions are adjusted as follows: the temperature of the bottom of the rectifying kettle is 200-300 ℃, the temperature of liquid in the rectifying kettle is controlled to be 120-150 ℃, the temperature of the top of the rectifying kettle is 117-118 ℃, the reflux ratio is controlled to be 1: 1-5, front fractions are discarded, after the light absorption value and the water content are detected to be qualified, fractions at 115-116 ℃ are collected, heating rectification is stopped when the balance of the rectifying liquid is about 5-8%, the residual liquid is residual liquid, and the residual liquid is removed by discharging the bottom.
7) Filling nitrogen and filling: and (3) filling nitrogen automatically by using an automatic filling machine, and packaging 500mL of the product, wherein the purity of the obtained product is 99.91%, the moisture content is 0.021%, and all detection results meet the index requirements. Can meet the customer requirements of chromatographically pure 4-methyl-2-pentanone. The results of the tests of the product are shown in table 1. (the absorbance measurement is the result of a 1cm quartz cuvette using water as a reference)
Table 1: detection results of various indexes of 4-methyl-2-pentanone
Example 2:
a method for purifying chromatographically pure 4-methyl-2-pentanone comprises the following steps: the purification steps are as follows:
1) and (3) oxidation: the method comprises the steps of putting a 4-methyl-2-pentanone raw material into a rectifying still, adding IBX oxidant according to 0.2-0.5% of the raw material by mass, and stirring and reacting for 30-60 min.
2) A first adsorption step: and (3) adsorbing and removing impurities from the oxidized 4-methyl-2-pentanone through an activated alumina adsorption column, and adsorbing and filtering through an activated alumina column with the height of 1m and the diameter of 10cm at the filtering speed of 150-300 mL/min.
3) And (3) drying: and (3) filtering the sample liquid after adsorption treatment through a calcium sulfate filter column with the height of 1m and the diameter of 10cm at the filtering speed of 50-100 mL/min until the water content is below 0.1%.
4) And (2) an adsorption step II: and (3) introducing the dried 4-methyl-2-pentanone into an alkaline molecular sieve adsorption column for filtration, and pouring the 4-methyl-2-pentanone subjected to further moisture and acidic impurities removal into a rectifying still for later use. The height of the adsorption column is 1m, the diameter is 4.2cm, the built-in adsorbent is an alkaline molecular sieve, the volume of the built-in adsorbent is 2/3 of the volume of the adsorption column, and the flow rate is controlled to be 50-100 mL/min.
5) A first rectification step: the temperature of the bottom of the rectifying kettle is 100-120 ℃, the liquid temperature in the kettle is controlled at 80-100 ℃, low boiling point impurities such as acetone, isopropanol and the like are removed by rectification, and the rectified finished product is poured into a recovery barrel.
6) And a second rectification step: the rectification conditions are adjusted as follows: the temperature of the bottom of the rectifying kettle is 200-300 ℃, the temperature of liquid in the rectifying kettle is controlled to be 120-150 ℃, the temperature of the top of the rectifying kettle is 117-118 ℃, the reflux ratio is controlled to be 1: 1-5, front fractions are discarded, after the light absorption value and the water content are detected to be qualified, fractions at 115-116 ℃ are collected, heating rectification is stopped when the balance of the rectifying liquid is about 5-8%, the residual liquid is residual liquid, and the residual liquid is removed by discharging the bottom.
7) Filling nitrogen and filling: the product is filled with nitrogen automatically by an automatic filling machine and is packaged by 500mL, the purity of the obtained product is 99.90 percent, the moisture content is 0.016 percent, and all detection results meet the index requirements. Can meet the customer requirements of chromatographically pure 4-methyl-2-pentanone. The results of the tests of this product are shown in Table 2. (the absorbance measurement is the result of a 1cm quartz cuvette using water as a reference)
Table 2: detection results of various indexes of 4-methyl-2-pentanone
Claims (4)
1. A method for purifying chromatographically pure 4-methyl-2-pentanone is characterized by comprising the following steps: the steps are as follows
The method comprises the following steps of: adding a proper amount of IBX selective oxidant into a 4-methyl-2-pentanone raw material to oxidize 4-methyl-2-pentanol and some alcohol impurities;
the first adsorption step: pumping the oxidized 4-methyl-2-pentanone product into an activated alumina adsorption column, wherein the filtration flow rate is 200-300 mL/min;
drying: using anhydrous calcium sulfate as a drying agent to adsorb and remove water;
fourth, an adsorption step two: introducing the dried 4-methyl-2-pentanone into an alkaline molecular sieve adsorption column for filtration, and pouring the 4-methyl-2-pentanone after further removing moisture and acidic impurities into a rectifying still for later use;
step I of rectification: the rectification conditions are adjusted as follows: the temperature of the bottom of the rectifying kettle is 100-120 ℃, the temperature of liquid in the kettle is controlled between 80-100 ℃, and low-boiling-point impurities are removed;
sixthly, rectification step two: the rectification conditions are adjusted as follows: the temperature of the bottom of the rectifying kettle is 200-300 ℃, the temperature of liquid in the rectifying kettle is controlled to be 120-150 ℃, the temperature of the top of the rectifying kettle is 117-118 ℃, the reflux ratio is controlled to be 1: 0.5-4, front fractions are discarded, and fractions at 115-116 ℃ are collected after the light absorption value is detected to be qualified; filling nitrogen into the distillate and filling;
the height of the alkaline molecular sieve adsorption column is 1.0m, the diameter is 4.2cm, the modified ZSM-5 molecular sieve is filled in the alkaline molecular sieve adsorption column and is used as a drying agent, and the drying agent accounts for 2/3 of the drying column;
the modified ZSM-5 molecular sieve is prepared by taking sodium hydroxide as an alkali source, soaking at high temperature for 60-120 min, and then heating and drying at 120 ℃.
2. Process for the purification of chromatographically pure 4-methyl-2-pentanone according to claim 1, characterized in that: the purity of the raw material 4-methyl-2-pentanone is 98.5%, and the water content is 0.5%.
3. Process for the purification of chromatographically pure 4-methyl-2-pentanone according to claim 1, characterized in that: the drying agent is analytically pure anhydrous calcium sulfate.
4. Process for the purification of chromatographically pure 4-methyl-2-pentanone according to claim 1, characterized in that: the IBX selective oxidant is chemically named 2-iodoxybenzoic acid.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102040496A (en) * | 2010-12-29 | 2011-05-04 | 天津市康科德科技有限公司 | Purification method of high-purity organic solvent 4-methyl-2-pentanone |
| CN107324984A (en) * | 2017-08-29 | 2017-11-07 | 湖北工程学院 | Chromatogram pure acetone and preparation method thereof, production system |
| CN107501056A (en) * | 2017-08-29 | 2017-12-22 | 湖北工程学院 | A kind of chromatogram absolute ether and preparation method thereof, production system |
| CN107501066A (en) * | 2017-08-29 | 2017-12-22 | 湖北工程学院 | Chromatographically pure butanone and preparation method thereof, production system |
| CN208104260U (en) * | 2017-09-11 | 2018-11-16 | 湖北工程学院 | Hexone process units and hexone production system |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102040496A (en) * | 2010-12-29 | 2011-05-04 | 天津市康科德科技有限公司 | Purification method of high-purity organic solvent 4-methyl-2-pentanone |
| CN107324984A (en) * | 2017-08-29 | 2017-11-07 | 湖北工程学院 | Chromatogram pure acetone and preparation method thereof, production system |
| CN107501056A (en) * | 2017-08-29 | 2017-12-22 | 湖北工程学院 | A kind of chromatogram absolute ether and preparation method thereof, production system |
| CN107501066A (en) * | 2017-08-29 | 2017-12-22 | 湖北工程学院 | Chromatographically pure butanone and preparation method thereof, production system |
| CN208104260U (en) * | 2017-09-11 | 2018-11-16 | 湖北工程学院 | Hexone process units and hexone production system |
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