CN112898154A - Method for removing water in ethyl lactate - Google Patents
Method for removing water in ethyl lactate Download PDFInfo
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- CN112898154A CN112898154A CN202110082687.8A CN202110082687A CN112898154A CN 112898154 A CN112898154 A CN 112898154A CN 202110082687 A CN202110082687 A CN 202110082687A CN 112898154 A CN112898154 A CN 112898154A
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- ethyl lactate
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/60—Separation; Purification; Stabilisation; Use of additives by treatment giving rise to chemical modification
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Abstract
The invention is applicable to the technical field of semiconductors, and provides a method for removing water in ethyl lactate, which comprises the following steps: providing a crude product of ethyl lactate and a dehydrating agent, adding the dehydrating agent into the crude product of ethyl lactate to form a precursor solution, and then carrying out first heat treatment on the precursor solution to form a pure product of ethyl lactate, wherein the moisture content of the crude product of ethyl lactate is greater than that of the pure product of ethyl lactate. In the invention, the water content of the obtained pure ethyl lactate product is less than that of the crude ethyl lactate product by dissolving the crude ethyl lactate product in the dehydrating agent, so that the water content of the ethyl lactate product is reduced.
Description
Technical Field
The invention belongs to the technical field of semiconductors, and particularly relates to a method for removing water in ethyl lactate.
Background
Ethyl lactate, CAS No.: 97-64-3, also known as ethyl 2-hydroxypropionate, is a colorless liquid, has a relative density of 1.024-1.036 (15 ℃), a boiling point of 154 ℃, and can be mixed with water, and can be used in the fields of spices, foods, lubricants and the like, and also can be used in the fields of coatings, inks and the like, and is a commonly used environment-friendly solvent which can also be used in the fields of semiconductors such as the electronic industry and the like.
However, the purity of the ethyl lactate prepared by the method or purified by the method is lower but not higher than the high requirement of the semiconductor industry, for example, the moisture content in the ethyl lactate is as high as 0.04% or more.
Therefore, there is an urgent need for a method for reducing the moisture content in ethyl lactate.
Disclosure of Invention
The embodiment of the invention provides a method for removing water in ethyl lactate, which aims to solve the problem of high water content in ethyl lactate in the prior art.
The embodiment of the invention is realized in such a way that a method for removing water in ethyl lactate is provided, which comprises the following steps:
providing a crude product of ethyl lactate and a dehydrating agent, and adding the dehydrating agent into the crude product of ethyl lactate to form a precursor solution;
and carrying out first heat treatment on the precursor solution to form a pure ethyl lactate product, wherein the moisture content of the crude ethyl lactate product is greater than that of the pure ethyl lactate product.
Further, the temperature of the first heat treatment is 5-19 ℃.
Further, the mass ratio of the dehydrating agent to the crude ethyl lactate is 1: 10-10000.
Still further, the dehydrating agent comprises one or a combination of several of trimethylboron, trimethylaluminum, trimethylgallium, trimethylindium and trimethylthallium.
Further, the step of performing a first heat treatment on the precursor solution to form a pure product of ethyl lactate includes:
and carrying out first stirring treatment and first heat treatment on the precursor liquid to form a first intermediate product.
Further, the stirring time of the first stirring treatment is 1 hour to 5 hours.
Further, the stirring speed of the first stirring treatment is 60r/min-100 r/min.
Still further, after the step of performing the first stirring treatment and the first heat treatment on the precursor liquid to form the first intermediate product, the method further includes:
and carrying out suction filtration treatment on the first intermediate product to form a second intermediate product.
Further, the suction filtration treatment time is 1 hour to 3 hours.
Further, after the step of performing suction filtration treatment on the first intermediate product to form a second intermediate product, the method further comprises the following steps:
and carrying out second stirring treatment on the second intermediate product to form a pure ethyl lactate product.
Further, the stirring time of the second stirring treatment is 1 hour to 3 hours.
Further, the step of performing a second stirring treatment on the second intermediate product to form a pure product of ethyl lactate comprises:
and carrying out second heat treatment on the second intermediate product, and recovering the dehydrating agent, wherein the temperature of the second heat treatment is 60-80 ℃.
The invention provides a method for removing water in ethyl lactate, which comprises the following steps: providing a crude product of ethyl lactate and a dehydrating agent, adding the dehydrating agent into the crude product of ethyl lactate to form a precursor solution, and then carrying out first heat treatment on the precursor solution to form a pure product of ethyl lactate, wherein the moisture content of the crude product of ethyl lactate is greater than that of the pure product of ethyl lactate. In the invention, the crude ethyl lactate is dissolved in the dehydrating agent, so that the moisture content of the obtained pure ethyl lactate is less than that of the crude ethyl lactate, and the moisture content of the ethyl lactate is further reduced.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The invention provides a method for removing water in ethyl lactate, wherein the water content of the ethyl lactate prepared by a common purification method in the prior art is as high as 0.04% or more and can not meet the requirements of the electronic industry, so that the ethyl lactate can not be applied to the electronic industry, and related devices in the electronic industry can be caused to lose efficacy even if the ethyl lactate is applied to the electronic industry, and the performance of the related devices is further influenced.
The embodiment of the invention provides a method for removing water in ethyl lactate, which comprises the following steps: providing a crude product of ethyl lactate and a dehydrating agent, adding the dehydrating agent into the crude product of ethyl lactate to form a precursor solution, then carrying out first heat treatment and first stirring treatment on the precursor solution to form a first intermediate product, then carrying out suction filtration treatment on the first intermediate product to form a second intermediate product, and then carrying out second stirring treatment on the second intermediate product to form a pure product of ethyl lactate, wherein the moisture content of the crude product of ethyl lactate is greater than that of the pure product of ethyl lactate. In the invention, the water content of the obtained pure ethyl lactate product is less than that of the crude ethyl lactate product by dissolving the crude ethyl lactate product in the dehydrating agent, so that the water content of the ethyl lactate product is reduced.
The specific description is as follows:
example one
In a glove box, providing a crude product of ethyl lactate with the purity of 99.0 percent or less and the moisture content of 0.04 percent or more, and providing a dehydrating agent with the purity of more than 99.99999 percent, wherein the dehydrating agent is trimethyl gallium; adding 100g of crude ethyl lactate into a three-neck flask A with lower discharging liquid, wherein the lower discharging liquid means that a discharging valve is arranged below the three-neck flask A; then, adding 5g of trimethyl gallium into the three-neck flask A to form a precursor solution; then, carrying out first heat treatment and first stirring treatment on the precursor liquid to form a first intermediate product, setting the temperature of the first heat treatment to be 5 ℃, setting the stirring speed of the first stirring treatment to be 60r/min, and setting the stirring time of the first stirring treatment to be 1 hour; then, adding the first intermediate product into a receiving bottle B with a vacuumizing funnel, performing suction filtration for 1 hour to form a second intermediate product after the suction filtration is finished; and then, introducing the second intermediate product back into the three-neck flask A, carrying out second stirring treatment on the second intermediate product, wherein the second stirring time is 1 hour, and then carrying out second heat treatment on the second intermediate product to recover the trimethylgallium, wherein the temperature of the second heat treatment is 70 ℃. And then, detecting the residual pure ethyl lactate, wherein the moisture content in the ethyl lactate is less than 0.0005 percent and less through a moisture detector, namely the moisture content of the crude ethyl lactate is greater than that of the pure ethyl lactate, the purity is 99.6 percent and more through HPLC (high performance liquid chromatography), and the mass of the pure ethyl lactate is 98.5g, namely the yield of the pure ethyl lactate reaches 98.5 percent and more.
The glove box is also called as a vacuum glove box, an inert gas protection box, a dry box and the like, and is laboratory equipment which fills high-purity inert gas into a box body and filters active substances in the box body in a circulating mode.
In the invention, the operation is carried out in the glove box, so that the problems that the experiment cannot be carried out or the experiment effect is poor and the like caused by the flammability of trimethyl gallium in the air are avoided, the cost is reduced and the yield is improved.
The moisture detector is used for detecting moisture content in various organic and inorganic solid, liquid and gas samples.
Hplc (high Performance Liquid chromatography) is a high Performance Liquid chromatography, which is also called high pressure Liquid chromatography, high Performance Liquid chromatography, high resolution Liquid chromatography, modern column chromatography, and the like. The high performance liquid phase chromatography uses liquid as mobile phase, adopts high pressure transfusion system, pumps the mobile phase of single solvent with different polarity or mixed solvent, buffer solution and the like with different proportions into a chromatographic column filled with stationary phase, and after each component in the chromatographic column is separated, the components enter a detector for detection, thereby realizing the analysis of the sample.
In the invention, the pure ethyl lactate with the moisture content of less than 0.0005 percent and less can be obtained by adding trimethyl gallium into the crude ethyl lactate, so that the moisture content in the ethyl lactate is reduced, and the ethyl lactate is applied to the electronic industry, so that the performance of an electronic device can be improved; the method for removing the water in the ethyl lactate is adopted to purify the crude ethyl lactate, the yield of the ethyl lactate is as high as 98.5% or more, namely, the yield is high, and the cost is further reduced.
Example two
In a glove box, providing a crude product of ethyl lactate with the purity of 99.0 percent or less and the moisture content of 0.04 percent or more, and providing a dehydrating agent with the purity of more than 99.99999 percent, wherein the dehydrating agent is trimethyl boron; adding 100g of crude ethyl lactate into a three-neck flask A with lower discharging liquid, wherein the lower discharging liquid means that a discharging valve is arranged below the three-neck flask A; then, adding 10g of trimethylboron into the three-neck flask A to form a precursor solution; then, carrying out first heat treatment and first stirring treatment on the precursor liquid to form a first intermediate product, setting the temperature of the first heat treatment to be 10 ℃, setting the stirring speed of the first stirring treatment to be 80r/min, and setting the stirring time of the first stirring treatment to be 2 h; then, adding the first intermediate product into a receiving bottle B with a vacuumizing funnel, performing suction filtration for 2 hours to form a second intermediate product after the suction filtration is finished; then, the second intermediate product is led back to the three-neck flask A, the second stirring treatment is carried out on the second intermediate product, the stirring time of the second stirring treatment is 2 hours, then, the second intermediate product is subjected to second heat treatment, the trimethyl boron is recovered, and the temperature of the second heat treatment is 75 ℃. And then, detecting the residual pure ethyl lactate, wherein the moisture content in the ethyl lactate is less than 0.0005 percent and less through a moisture detector, namely the moisture content of the crude ethyl lactate is greater than that of the pure ethyl lactate, the purity is 99.5 percent and more through HPLC (high performance liquid chromatography), and the mass of the pure ethyl lactate is 98.5g, namely the yield of the pure ethyl lactate reaches 98.5 percent and more.
In the invention, the operation is carried out in the glove box, so that the problems that the experiment cannot be carried out or the experiment effect is poor and the like caused by the flammability of the trimethylboron in the air are avoided, the cost is reduced and the yield is improved.
In the invention, the pure ethyl lactate with the water content of less than 0.0005 percent and less can be obtained by adding the crude ethyl lactate into the crude ethyl lactate for hours, so that the water content in the ethyl lactate is reduced, and the ethyl lactate is applied to the electronic industry, so that the performance of an electronic device can be improved; the method for removing the water in the ethyl lactate is adopted to purify the crude ethyl lactate, the yield of the ethyl lactate is as high as 98.5% or more, namely, the yield is high, and the cost is further reduced.
EXAMPLE III
In a glove box, providing a crude product of ethyl lactate with the purity of 99.0 percent or less and the moisture content of 0.04 percent or more, and providing a dehydrating agent with the purity of more than 99.99999 percent, wherein the dehydrating agent is trimethyl indium; adding 100g of crude ethyl lactate into a three-neck flask A with lower discharging liquid, wherein the lower discharging liquid means that a discharging valve is arranged below the three-neck flask A; then, adding 10g of trimethylindium into the three-neck flask A to form a precursor solution; then, carrying out first heat treatment and first stirring treatment on the precursor liquid to form a first intermediate product, setting the temperature of the first heat treatment to be 13 ℃, setting the stirring speed of the first stirring treatment to be 99r/min, and setting the stirring time of the first stirring treatment to be 1 h; then, adding the first intermediate product into a receiving bottle B with a vacuumizing funnel, performing suction filtration for 1.5 hours to form a second intermediate product after the suction filtration is finished; then, the second intermediate product is returned to the three-neck flask A, the second intermediate product is subjected to second stirring treatment, the stirring time of the second stirring treatment is 1.5 hours, then, the second intermediate product is subjected to second heat treatment, trimethyl indium is recovered, and the temperature of the second heat treatment is 65 ℃. And then, detecting the residual pure ethyl lactate, wherein the moisture content in the ethyl lactate is less than 0.0005 percent and less through a moisture detector, namely the moisture content of the crude ethyl lactate is greater than that of the pure ethyl lactate, the purity is 99.5 percent and more through HPLC (high performance liquid chromatography), and the mass of the pure ethyl lactate is 98.5g, namely the yield of the pure ethyl lactate reaches 98.5 percent and more.
In the invention, the operation is carried out in the glove box, so that the problems that the experiment cannot be carried out or the experiment effect is poor and the like caused by the flammability of the trimethyl indium in the air are avoided, the cost is reduced and the yield is improved.
In the invention, the pure ethyl lactate with the moisture content of less than 0.0005 percent and less can be obtained by adding trimethyl indium into the crude ethyl lactate, so that the moisture content in the ethyl lactate is reduced, and the performance of an electronic device can be improved when the ethyl lactate is applied to the electronic industry; the method for removing the water in the ethyl lactate is adopted to purify the crude ethyl lactate, the yield of the ethyl lactate is as high as 98.5% or more, namely, the yield is high, and the cost is further reduced.
The invention provides a method for removing water in ethyl lactate, which comprises the following steps: providing a crude product of ethyl lactate and a dehydrating agent, adding the dehydrating agent into the crude product of ethyl lactate to form a precursor solution, and then carrying out first heat treatment on the precursor solution to form a pure product of ethyl lactate, wherein the moisture content of the crude product of ethyl lactate is greater than that of the pure product of ethyl lactate. In the invention, the ethyl lactate crude product is dissolved in the dehydrating agent, so that the moisture content of the obtained ethyl lactate pure product is less than that of the ethyl lactate crude product, the moisture content of the ethyl lactate pure product is as low as 0.0004% or less, and the purity of the ethyl lactate pure product is as high as 99.5% or more, thereby reducing the moisture content of the ethyl lactate and the production cost.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (10)
1. A method for removing water in ethyl lactate is characterized by comprising the following steps:
providing a crude product of ethyl lactate and a dehydrating agent, and adding the dehydrating agent into the crude product of ethyl lactate to form a precursor solution;
and carrying out first heat treatment on the precursor solution to form a pure ethyl lactate product, wherein the moisture content of the crude ethyl lactate product is greater than that of the pure ethyl lactate product.
2. The method for removing moisture in ethyl lactate according to claim 1, wherein the temperature of the first heat treatment is 5-19 ℃.
3. The method for removing moisture in ethyl lactate according to claim 1, wherein the mass ratio of the dehydrating agent to the crude ethyl lactate is 1: 10-10000.
4. The method for removing moisture in ethyl lactate as claimed in claim 1, wherein the dehydrating agent comprises one or more of trimethyl boron, trimethyl aluminum, trimethyl gallium, trimethyl indium and trimethyl thallium.
5. The method for removing water in ethyl lactate according to claim 1, wherein the step of performing the first heat treatment on the precursor solution to form a pure product of ethyl lactate comprises:
and carrying out first stirring treatment and first heat treatment on the precursor liquid to form a first intermediate product.
6. The method for removing water from ethyl lactate according to claim 5, wherein the stirring time of the first stirring treatment is 1 hour to 5 hours.
7. The method for removing water from ethyl lactate according to claim 6, wherein after the steps of performing the first stirring treatment and the first heat treatment on the precursor liquid to form the first intermediate product, the method further comprises:
and carrying out suction filtration treatment on the first intermediate product to form a second intermediate product.
8. The method for removing water in ethyl lactate according to claim 7, wherein after the step of performing suction filtration treatment on the first intermediate product to form a second intermediate product, the method further comprises the following steps:
and carrying out second stirring treatment on the second intermediate product to form a pure ethyl lactate product.
9. The method for removing water from ethyl lactate according to claim 8, wherein the stirring time of the second stirring treatment is 1 hour to 3 hours.
10. The method for removing water in ethyl lactate according to claim 8, wherein the step of performing the second stirring treatment on the second intermediate product to form a pure ethyl lactate product comprises the following steps:
and carrying out second heat treatment on the second intermediate product, and recovering the dehydrating agent, wherein the temperature of the second heat treatment is 60-80 ℃.
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| CN202110082687.8A CN112898154A (en) | 2021-01-21 | 2021-01-21 | Method for removing water in ethyl lactate |
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| CN202110082687.8A CN112898154A (en) | 2021-01-21 | 2021-01-21 | Method for removing water in ethyl lactate |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102320969A (en) * | 2011-06-10 | 2012-01-18 | 天津大学 | System and method for rectifying and purifying food grade ethyl lactate into electronic grade ethyl lactate |
| CN103836885A (en) * | 2014-03-27 | 2014-06-04 | 张德龙 | Chemical drying water removal method |
| CN104241688A (en) * | 2013-06-24 | 2014-12-24 | 微宏动力系统（湖州）有限公司 | Lithium ion battery electrolyte and lithium ion battery |
| CN104610061A (en) * | 2015-02-06 | 2015-05-13 | 孝感市易生新材料有限公司 | Preparation method of electronic ethyl lactate |
-
2021
- 2021-01-21 CN CN202110082687.8A patent/CN112898154A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102320969A (en) * | 2011-06-10 | 2012-01-18 | 天津大学 | System and method for rectifying and purifying food grade ethyl lactate into electronic grade ethyl lactate |
| CN104241688A (en) * | 2013-06-24 | 2014-12-24 | 微宏动力系统（湖州）有限公司 | Lithium ion battery electrolyte and lithium ion battery |
| CN103836885A (en) * | 2014-03-27 | 2014-06-04 | 张德龙 | Chemical drying water removal method |
| CN104610061A (en) * | 2015-02-06 | 2015-05-13 | 孝感市易生新材料有限公司 | Preparation method of electronic ethyl lactate |
Non-Patent Citations (1)
| Title |
|---|
| 朱洪法等: "《催化剂手册》", 31 August 2008, 金盾出版社 * |
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Application publication date: 20210604 |