CN114105802A - Method for controlling metal ions and chromaticity in preparation process of N-ethylformamide - Google Patents
Method for controlling metal ions and chromaticity in preparation process of N-ethylformamide Download PDFInfo
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- CN114105802A CN114105802A CN202111340089.2A CN202111340089A CN114105802A CN 114105802 A CN114105802 A CN 114105802A CN 202111340089 A CN202111340089 A CN 202111340089A CN 114105802 A CN114105802 A CN 114105802A
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- ethylformamide
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C231/00—Preparation of carboxylic acid amides
- C07C231/02—Preparation of carboxylic acid amides from carboxylic acids or from esters, anhydrides, or halides thereof by reaction with ammonia or amines
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C231/00—Preparation of carboxylic acid amides
- C07C231/22—Separation; Purification; Stabilisation; Use of additives
- C07C231/24—Separation; Purification
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Abstract
The invention discloses a method for controlling metal ions and chromaticity in the preparation process of N-ethylformamide, which comprises the steps of carrying out heat preservation treatment on reaction liquid obtained by reacting monoethylamine with methyl formate, carrying out rectification operation through rectification tower liquid after the reaction is completed, controlling the metal ions and chromaticity by controlling alkalinity in the reaction process of reacting monoethylamine with methyl formate and in the subsequent rectification process, and specifically, after rectification, ensuring that the alkalinity in a product is 0.002-0.01 percent calculated by monoethylamine, and the pH of the product is 9.9-10.6. The method disclosed by the invention is simple to operate, is accurate to control, can effectively reduce metal ions in the N-ethylformamide, improves the grade of the N-ethylformamide, and improves the economic benefit of enterprises.
Description
Technical Field
The invention relates to the field of production processes of N-ethylformamide, in particular to a method for controlling metal ions and chromaticity in the preparation process of N-ethylformamide.
Background
N-ethylformamide is a novel raw material for producing high-end displays, and is gradually produced in batches at present through years of experiments and trial trials of customers.
The N-ethylformamide is one of chemical products produced by enterprises, and the production process takes monoethylamine and methyl formate as raw materials to prepare a product with the purity of more than 99.7 percent through the processes of synthesis, rough distillation, dehydration, rectification and the like.
The detailed reaction formula is as follows: C2H7N + CH3 COOH =C3H7NO+CH3OH+Q。
The N-ethylformamide prepared through the reaction is a crude product, and the crude product N-ethylformamide needs to be refined in the actual production process, so that a product with higher purity is obtained. The refining needs a certain alkalinity in the operation process, and N-ethylformamide can cause metal ions and overproof chromaticity when the alkalinity can not reach;
the metal ions and color produced during the refining operation have a serious impact on product quality and yield. Therefore, a method for reducing the generation of metal ions and chromaticity can be found in the production process, and the economic benefit of enterprise production is directly influenced by the method for improving the product quality and yield of the N-ethylformamide.
Disclosure of Invention
In order to solve the problems, the invention discloses a method for controlling metal ions and chromaticity in the preparation process of N-ethylformamide, which is simple to operate and accurate to control, and can effectively reduce the metal ions in the N-ethylformamide, improve the grade of the N-ethylformamide and improve the economic benefit of enterprises.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a method for controlling metal ions and chromaticity in the preparation process of N-ethylformamide comprises the steps of carrying out heat preservation treatment on reaction liquid obtained by reacting monoethylamine with methyl formate, carrying out rectification operation through rectification tower liquid after the reaction is completed, controlling the metal ions and chromaticity by controlling alkalinity in the reaction process of reacting monoethylamine with methyl formate and in the subsequent rectification process, and specifically, after rectification, enabling the alkalinity in the product to reach 0.002% -0.01% by weight of monoethylamine, and enabling the pH of the product to be 9.9-10.6.
Further, the method specifically comprises the following steps:
(1) introducing methyl formate and monoethylamine with mass excess of 0.5-1% into an N-ethylformamide reactor, and reacting at 38-45 ℃ under normal pressure;
(2) feeding the mixed reaction liquid obtained in the step (1) into a coarse distillation tower through a coarse distillation tower feeding pump to perform coarse distillation operation, wherein methanol and monoethylamine are obtained at the top of the coarse distillation tower, and N-ethylformamide crude liquid is obtained at the bottom of the coarse distillation tower;
(3) detecting the N-ethylformamide crude liquid in the tower kettle of the crude distillation tower, when the mass fraction of the N-ethylformamide is more than or equal to 95%, feeding the N-ethylformamide into a dehydrating tower through a dehydrating tower feeding pump, rectifying the dehydrating tower under a vacuum condition to remove water and methanol, and obtaining dehydrating tower kettle liquid at the tower kettle;
(4) and (3) detecting the residue of the dehydration tower, when the mass fraction of the N-ethylformamide is more than or equal to 98.5%, feeding the N-ethylformamide into a rectifying tower through a feeding pump of the rectifying tower, rectifying under vacuum, and collecting the product N-ethylformamide from the top of the rectifying tower.
Further, the temperature of the bottom of the crude distillation tower in the step (2) is reduced to 120 ℃, the temperature of the top of the crude distillation tower is reduced to 60 ℃, and the methanol obtained from the top of the crude distillation tower is sent to a methanol recovery tank for recycling.
Further, the temperature of the tower kettle of the dehydration tower in the step (3) is reduced to 115 ℃, the temperature of the tower top is less than or equal to 40 ℃, and the vacuum degree of the tower top is 0.08-0.10 Mpa.
Further, the temperature of the kettle of the rectifying tower in the step (4) is reduced to 115-120 ℃, and the temperature of the top of the rectifying tower is reduced to 100-110 ℃.
Further, the temperature of a condenser at the top of the tower in the operation processes of the steps (2), (3) and (4) is 30-35 ℃, and under the condition, after the rectification of the product N-ethylformamide rectified in the step (4), a certain amount of monoethylamine solution is added into a metering tank, so that the alkalinity of the product is 0.002-0.01 percent calculated by monoethylamine, and the pH value of the product is 9.9-10.6.
Further, the monoethylamine in the step (1) is subjected to decompression treatment to obtain monoethylamine gas, and the pressure of the monoethylamine gas is 0.1-0.2 MPa.
The invention has the beneficial effects that:
the invention mainly aims to improve the processes of crude distillation, dehydration and distillation of N-ethylformamide, and control the alkalinity of N-ethylformamide products in the processes of crude distillation, dehydration and distillation so as to ensure that metal ions and chromaticity in the products meet the high requirement of electronic grade when the purity of the products is reached. The specific effects of the present invention are shown in the comparison of comparative examples with examples.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments.
Comparative example 1:
a method for preparing N-ethylformamide is characterized in that the detailed operation method of the production process in the prior art comprises the following steps:
1) introducing methyl formate and monoethylamine into an N-ethylformamide reactor, reacting at 38-45 ℃ under normal pressure, and reacting to obtain a mixed reaction solution of N-ethylformamide and methanol;
2) feeding the mixed reaction liquid obtained in the step 1) into a coarse distillation tower through a feeding pump of the coarse distillation tower for coarse distillation operation, wherein methanol is obtained at the top of the coarse distillation tower, and N-ethylformamide is obtained at the bottom of the coarse distillation tower;
3) detecting the N-ethylformamide crude liquid in the tower kettle of the crude distillation tower, when the mass fraction of the N-ethylformamide is more than or equal to 95%, feeding the N-ethylformamide into a dehydrating tower through a dehydrating tower feeding pump, rectifying the dehydrating tower under a vacuum condition to remove water and methanol, and obtaining dehydrating tower kettle liquid at the tower kettle;
4) detecting the residue in the dehydration tower, when the mass fraction of N-ethylformamide is more than or equal to 98.5%, feeding into a rectification tower through a rectification tower feeding pump, rectifying under vacuum, collecting the product N-ethylformamide from the top of the tower,
the monoethylamine in the step 1) is subjected to decompression treatment to obtain ethylamine gas, and the pressure is 0.1-0.2 Mpa; because the reaction is a normal-pressure reaction, the raw material monoethylamine needs to be subjected to decompression treatment after quantification, and the decompressed monoethylamine is directly introduced into the N-ethylformamide reactor, so that the influence of pressure on the reaction process is avoided.
In the step 2), the temperature of the tower kettle of the crude distillation tower is 135 ℃, the temperature of the tower top is 65 ℃, and the methanol obtained from the tower top of the crude distillation tower is sent into a methanol recovery tank for recycling; methanol in the production process is separated through the crude distillation tower, N-ethyl formamide is not discharged, the separated high-purity methanol can be put into the synthesis of methyl formate, and the cyclic utilization of resources is ensured.
The temperature of a tower kettle of the dehydration tower in the step 3) is 125 ℃, the temperature of the top of the tower is less than or equal to 40 ℃, and the vacuum degree of the top of the tower is 0.08-0.10 Mpa; the dehydration tower is mainly used for discharging excessive water and a small amount of methanol in the N-ethylformamide product, and has good dehydration and separation effects and improves the purity of the final product by the principle of vacuum suction.
In the step 4), the temperature of the kettle of the rectifying tower is 200-210 ℃, and the temperature of the top of the rectifying tower is 100-110 ℃; the rectifying tower is mainly used for the final refining operation of the N-ethylformamide product, and meanwhile, the N-ethylformamide product at the tower top can be conveniently collected through high temperature and vacuum suction.
The crude N-ethylformamide produced by the process is analyzed to obtain several groups of data:
| serial number | Purity (%) | Metal ion (ppm) | Chroma (platinum cobalt) | PH | Alkalinity (%) |
| 1 | 96.62 | 49 | 35 | 10.33 | 0.005 |
| 2 | 97.51 | 88 | 40 | 10.27 | 0.004 |
| 3 | 96.22 | 42 | 30 | 10.30 | 0.005 |
| 4 | 94.92 | 35 | 25 | 10.50 | 0.012 |
The N-ethylformamide finished product produced by the process is analyzed to obtain several groups of data:
| serial number | Purity (%) | Metal ion (ppm) | Chroma (platinum cobalt) | PH | Alkalinity (%) |
| 1 | 99.87 | 35 | 25 | 7.89 | 0.001 |
| 2 | 99.84 | 24 | 35 | 8.20 | 0.001 |
| 3 | 99.88 | 35 | 15 | 8.12 | 0.001 |
| 4 | 99.81 | 23 | 10 | 8.01 | 0.001 |
| 5 | 99.80 | 19 | 10 | 8.15 | 0.001 |
The N-ethylformamide produced by the process is insufficient in alkalinity control and cannot meet ideal requirements on indexes of metal ions and chromaticity.
Comparative example 2: a process for controlling metal ions and chromaticity in the preparation process of N-ethylformamide is different from the process of example 1 in that the temperature of a bottom kettle of a crude distillation tower and the temperature of a bottom kettle of a dehydration tower are reduced, and the temperature of a top of the crude distillation tower and the temperature of the dehydration tower are reduced, and the detailed operation method is as follows:
1) introducing methyl formate and monoethylamine (the excess of the monoethylamine is controlled to be 0.5-1% through the cooperation of a precision flowmeter and analysis) into an N-ethylformamide reactor, and reacting at 38-45 ℃ under normal pressure to obtain a mixed reaction solution of N-ethylformamide and methanol;
2) feeding the mixed reaction liquid obtained in the step 1) into a coarse distillation tower through a feeding pump of the coarse distillation tower for coarse distillation operation, wherein methanol and a small amount of monoethylamine are obtained at the top of the coarse distillation tower, and a crude N-ethylformamide liquid is obtained at the bottom of the coarse distillation tower; the temperature of the bottom of the crude distillation tower is reduced to 120 ℃, the temperature of the top of the crude distillation tower is reduced to 60 ℃, and the methanol obtained at the top of the crude distillation tower is sent to a methanol recovery tank for recycling.
3) Detecting the N-ethylformamide crude liquid in the tower kettle of the crude distillation tower, when the mass fraction of the N-ethylformamide is more than or equal to 95%, feeding the N-ethylformamide into a dehydrating tower through a dehydrating tower feeding pump, rectifying the dehydrating tower under a vacuum condition to remove water and methanol, and obtaining dehydrating tower kettle liquid at the tower kettle; the temperature of the tower kettle of the dehydration tower is reduced to 115 ℃, the temperature of the tower top is less than or equal to 40 ℃, and the vacuum degree of the tower top is 0.08-0.10 Mpa.
4) Detecting the residue of the dehydration tower, when the mass fraction of the N-ethylformamide is more than or equal to 98.5%, sending the N-ethylformamide into a rectifying tower through a rectifying tower feed pump, rectifying under vacuum, collecting the product N-ethylformamide from the top of the rectifying tower, reducing the temperature of the bottom of the rectifying tower to 115-120 ℃, and reducing the temperature of the top of the rectifying tower to 100-110 ℃.
The temperature of the condenser at the top of the tower in the operation process of the steps 2, 3 and 4) is further reduced to 30-35 ℃ on the basis of the original 50 ℃.
The crude N-ethylformamide produced by the process is analyzed to obtain several groups of data:
| serial number | Purity (%) | Metal ion (ppm) | Chroma (platinum cobalt) | PH | Alkalinity (%) |
| 1 | 95.38 | 32 | 20 | 10.58 | 0.015 |
| 2 | 94.52 | 24 | 30 | 10.51 | 0.012 |
| 3 | 94.97 | 29 | 25 | 10.52 | 0.012 |
| 4 | 95.56 | 25 | 35 | 10.50 | 0.010 |
| 5 | 94.28 | 27 | 25 | 10.59 | 0.017 |
The N-ethylformamide finished product produced by the process is analyzed to obtain several groups of data:
| serial number | Purity (%) | Metal ion (ppm) | Chroma (platinum cobalt) | PH | Alkalinity (%) |
| 1 | 99.89 | 12 | 5 | 8.87 | 0.001 |
| 2 | 99.90 | 11 | 5 | 8.67 | 0.001 |
| 3 | 99.90 | 4 | 5 | 8.92 | 0.001 |
| 4 | 99.89 | 2 | 5 | 8.94 | 0.001 |
| 5 | 99.86 | 3 | 5 | 8.95 | 0.001 |
Although the N-ethylformamide produced by the process meets better requirements on metal ions and color intensity, according to sample tracking of one month, the N-ethylformamide sample with the pH value less than 9.0 is unstable in property, and the color intensity is higher than the original color intensity in the later period, namely the color intensity is increased after a period of time, so that the quality of the N-ethylformamide is unstable.
The N-ethylformamide finished product produced by the process is tracked at the later stage (more than 30 days) and analyzed to obtain a plurality of groups of data:
| serial number | Purity (%) | Metal ion (ppm) | Chroma (platinum cobalt) | PH | Alkalinity (%) |
| 1 | 99.89 | 24 | 15 | 8.22 | 0.001 |
| 2 | 99.90 | 25 | 15 | 8.58 | 0.001 |
| 3 | 99.90 | 18 | 10 | 8.35 | 0.001 |
| 4 | 99.89 | 15 | 10 | 8.56 | 0.001 |
| 5 | 99.86 | 12 | 10 | 8.82 | 0.001 |
Based on the above information, the PH of the product was further increased to 9.5 or more without affecting the product quality, and this was shown in example 3.
Example 1: a process for controlling metal ions and chromaticity in the preparation process of N-ethylformamide comprises the following detailed operation method:
the operation steps of the reaction step, the dehydration step and the rectification step in the embodiment are the same as those in the comparative example 2, and the difference is that on the basis of the comparative example 2, the rectified product N-ethylformamide is further controlled, after rectification, a certain amount of monoethylamine solution is added into a metering tank through a vacuum sample injector, so that the alkalinity of the product reaches 0.002% -0.01% (calculated by monoethylamine), and the pH of the product is 9.9-10.6.
The crude N-ethylformamide produced by the process is analyzed to obtain several groups of data:
| serial number | Purity (%) | Metal ion (ppm) | Chroma (platinum cobalt) | PH | Alkalinity (%) |
| 1 | 95.38 | 32 | 20 | 10.58 | 0.015 |
| 2 | 94.52 | 24 | 30 | 10.51 | 0.012 |
| 3 | 94.97 | 29 | 25 | 10.52 | 0.012 |
| 4 | 95.56 | 25 | 35 | 10.50 | 0.010 |
| 5 | 94.28 | 27 | 25 | 10.59 | 0.017 |
The N-ethylformamide finished product produced by the process is analyzed to obtain several groups of data:
| serial number | Purity (%) | Metal ion (ppm) | Chroma (platinum cobalt) | PH | Alkalinity (%) |
| 1 | 99.89 | 12 | 5 | 10.58 | 0.004 |
| 2 | 99.90 | 11 | 5 | 10.55 | 0.005 |
| 3 | 99.90 | 4 | 5 | 10.62 | 0.004 |
| 4 | 99.89 | 2 | 5 | 10.58 | 0.005 |
| 5 | 99.86 | 3 | 5 | 10.56 | 0.005 |
Although the N-ethylformamide produced by the process meets good requirements on metal ions and chromaticity, the sample tracking analysis shows that the metal ions have slight change, the chromaticity is not changed, and the chromaticity (platinum cobalt) is still 5.
The finished N-ethylformamide (after 30 days) produced by the above process is subjected to sample tracking analysis to obtain several groups of data:
| serial number | Purity (%) | Metal ion (ppm) | Chroma (platinum cobalt) | PH | Alkalinity (%) |
| 1 | 99.89 | 14 | 5 | 10.62 | 0.004 |
| 2 | 99.90 | 10 | 5 | 10.83 | 0.005 |
| 3 | 99.90 | 5 | 5 | 10.68 | 0.004 |
| 4 | 99.89 | 2 | 5 | 10.88 | 0.005 |
| 5 | 99.86 | 3 | 5 | 10.66 | 0.005 |
Claims (7)
1. A method for controlling metal ions and chromaticity in the preparation process of N-ethylformamide is characterized in that heat preservation treatment is carried out on reaction liquid obtained by reacting monoethylamine with methyl formate, rectification operation is carried out through rectification tower liquid after the reaction is completed, the metal ions and chromaticity are controlled by controlling alkalinity in the reaction process of reacting monoethylamine with methyl formate and in the subsequent rectification process, specifically, after rectification, the alkalinity in the product is 0.002% -0.01% counted by monoethylamine, and the PH of the product is 9.9-10.6.
2. The method for controlling metal ions and chromaticity in the preparation process of N-ethylformamide according to claim 1, wherein the method specifically comprises the following steps:
(1) introducing methyl formate and monoethylamine with mass excess of 0.5-1% into an N-ethylformamide reactor, and reacting at 38-45 ℃ under normal pressure;
(2) feeding the mixed reaction liquid obtained in the step (1) into a coarse distillation tower through a coarse distillation tower feeding pump to perform coarse distillation operation, wherein methanol and monoethylamine are obtained at the top of the coarse distillation tower, and N-ethylformamide crude liquid is obtained at the bottom of the coarse distillation tower;
(3) detecting the N-ethylformamide crude liquid in the tower kettle of the crude distillation tower, when the mass fraction of the N-ethylformamide is more than or equal to 95%, feeding the N-ethylformamide into a dehydrating tower through a dehydrating tower feeding pump, rectifying the dehydrating tower under a vacuum condition to remove water and methanol, and obtaining dehydrating tower kettle liquid at the tower kettle;
(4) and (3) detecting the residue of the dehydration tower, when the mass fraction of the N-ethylformamide is more than or equal to 98.5%, feeding the N-ethylformamide into a rectifying tower through a feeding pump of the rectifying tower, rectifying under vacuum, and collecting the product N-ethylformamide from the top of the rectifying tower.
3. The method for controlling metal ions and chromaticity in the preparation process of N-ethylformamide as claimed in claim 2, wherein the temperature of the bottom of the crude distillation tower in the step (2) is reduced to 120 ℃, the temperature of the top of the crude distillation tower is reduced to 60 ℃, and the methanol obtained from the top of the crude distillation tower is sent to a methanol recovery tank for recycling.
4. The method for controlling metal ions and chromaticity in the preparation process of N-ethylformamide as claimed in claim 2, wherein the temperature of the bottom of the dehydration tower in the step (3) is reduced to 115 ℃, the temperature of the top of the tower is less than or equal to 40 ℃, and the vacuum degree of the top of the tower is 0.08-0.10 MPa.
5. The method for controlling metal ions and chromaticity in the preparation process of N-ethylformamide as claimed in claim 2, wherein the temperature of the bottom of the rectifying tower in the step (4) is reduced to 115-120 ℃, and the temperature of the top of the rectifying tower is reduced to 100-110 ℃.
6. The method for controlling metal ions and chromaticity in the preparation process of N-ethylformamide according to claim 2, wherein the temperature of the overhead condenser in the operation processes of the steps (2), (3) and (4) is 30-35 ℃, and under the condition, after the rectification of the product N-ethylformamide rectified in the step (4), a certain amount of monoethylamine solution is added into a metering tank, so that the alkalinity in the product is 0.002-0.01% calculated by monoethylamine, and the pH of the product is 9.9-10.6.
7. The method for controlling metal ions and chromaticity in the preparation process of N-ethylformamide according to claim 2, wherein the monoethylamine in the step (1) is decompressed and then is in the form of ethylamine gas, and the pressure is 0.1-0.2 MPa.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114591143A (en) * | 2022-03-16 | 2022-06-07 | 齐翔华利新材料有限公司 | Preparation method of sodium methyl allyl alcohol |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5075486A (en) * | 1987-09-15 | 1991-12-24 | Sanofi | Process for preparing di-n-propylacetonitrile |
| CN101062901A (en) * | 2006-04-30 | 2007-10-31 | 海南盛科生命科学研究院 | Preparation method of methyl ethylamine |
| CN105330559A (en) * | 2015-10-14 | 2016-02-17 | 宿迁新亚科技有限公司 | Electronic-grade formamide compound preparation method |
-
2021
- 2021-11-12 CN CN202111340089.2A patent/CN114105802A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5075486A (en) * | 1987-09-15 | 1991-12-24 | Sanofi | Process for preparing di-n-propylacetonitrile |
| CN101062901A (en) * | 2006-04-30 | 2007-10-31 | 海南盛科生命科学研究院 | Preparation method of methyl ethylamine |
| CN105330559A (en) * | 2015-10-14 | 2016-02-17 | 宿迁新亚科技有限公司 | Electronic-grade formamide compound preparation method |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114591143A (en) * | 2022-03-16 | 2022-06-07 | 齐翔华利新材料有限公司 | Preparation method of sodium methyl allyl alcohol |
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