CN112125808A - Triethylamine drying and purifying method - Google Patents
Triethylamine drying and purifying method Download PDFInfo
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- CN112125808A CN112125808A CN202011027296.8A CN202011027296A CN112125808A CN 112125808 A CN112125808 A CN 112125808A CN 202011027296 A CN202011027296 A CN 202011027296A CN 112125808 A CN112125808 A CN 112125808A
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- triethylamine
- drying
- crude product
- sodium hydroxide
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
- C07C209/82—Purification; Separation; Stabilisation; Use of additives
- C07C209/86—Separation
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- Organic Chemistry (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The invention relates to a method for drying and purifying triethylamine, which comprises the following steps: pumping a triethylamine crude product with the water content of 1-3% into a sodium hydroxide drying tower for primary drying, wherein the water of the triethylamine crude product and sodium hydroxide form an aqueous solution and gather at the bottom of the sodium hydroxide drying tower, pumping the triethylamine crude product after the primary drying into a potassium hydroxide drying tower for secondary drying, and the triethylamine crude product after the secondary drying is colorless and transparent and has the water content of 0.1-0.15%; and (3) carrying out drying on the triethylamine crude product after the secondary drying by using a 4A molecular sieve according to the speed of 3 m/h to obtain refined triethylamine, wherein the moisture content is below 0.1%. And pumping the sodium hydroxide aqueous solution subjected to primary drying to a triethylamine tail gas absorption tower for purifying triethylamine tail gas. The invention has the advantages that: the production cost is reduced, the environmental pollution is reduced, the production efficiency is improved, and the labor intensity is reduced.
Description
The technical field is as follows:
the invention relates to a method for drying and purifying triethylamine.
Background art:
triethylamine is an important raw and auxiliary material for producing acesulfame potassium, and is used as a catalyst in a large amount, and the triethylamine has the physicochemical property of being slightly soluble in water, so that solid potassium hydroxide is required to be used in the recovery process of the triethylamine to reduce the water content of the triethylamine. The price of potassium hydroxide is 9000 yuan per ton, while sodium hydroxide only needs 3700 yuan per ton. Therefore, the cost of potassium hydroxide used in the existing triethylamine recovery is too high.
The invention content is as follows:
the invention aims to overcome the defects of high process cost and low drying recovery rate in the prior art, and provides a triethylamine drying and purifying method.
The invention adopts the following technical scheme:
a triethylamine drying and purifying method is characterized by comprising the following steps:
1) pumping the triethylamine crude product with the water content of 1-3% in the triethylamine receiving groove into a sodium hydroxide drying tower through a circulating pump at the speed of 30 m/h, performing primary drying through the circulating pump, wherein water contained in the triethylamine crude product and sodium hydroxide in the drying tower form an aqueous solution, the sodium hydroxide solution is gathered at the bottom of the sodium hydroxide drying tower, and the triethylamine crude product with the water content of 0.3-0.5% after the primary drying is refluxed to the triethylamine receiving groove from the top of the drying tower;
2) pumping the triethylamine crude product after the first-stage drying into a potassium hydroxide drying tower through a circulating pump at the speed of 10 m/h for second-stage drying, wherein the triethylamine crude product after the second-stage drying is colorless and transparent, and the water content is 0.1-0.15%;
3) and (3) carrying out drying on the triethylamine crude product after the secondary drying by using a 4A molecular sieve according to the speed of 3 m/h to obtain refined triethylamine, wherein the moisture content is below 0.1%.
On the basis of the technical scheme, the following further technical scheme is provided:
and pumping the sodium hydroxide aqueous solution subjected to primary drying to a triethylamine tail gas absorption tower for purifying triethylamine tail gas.
The potassium hydroxide aqueous solution after the secondary drying is used in the neutralization section of the production of the acesulfame potassium.
The invention relates to an original alkaline washing tower in a production enterprise, which uses solid sodium hydroxide as a raw material to neutralize acid gas generated by acesulfame.
According to the technical scheme, sodium hydroxide is used as the early-stage drying agent of triethylamine, the formed liquid sodium hydroxide is distilled and then is specially used for the alkaline tower, on one hand, the consumption of potassium hydroxide can be saved, and on the other hand, the requirement of the alkaline tower on treatment of acid gas in the production of acesulfame is met.
The invention has the advantages that:
1. the process technology adopted by the project is mature and reliable: simple steps, low production cost and less environmental pollution.
2. Compared with the original traditional production process, the production steps are reduced, the drying efficiency is improved, and the environmental pollution is reduced; 1. after the original triethylamine tail gas is forcibly and circularly washed by a sodium hydroxide solution in an alkaline tower, the residual gas is discharged outdoors, but in the production process, the observation shows that in the actual operation, about 0.3 ton of sodium hydroxide is consumed every day, 1 to 3 bags of sodium hydroxide are dissolved on site by each worker, the labor capacity of the workers is increased, and the safety risk exists. After the transformation, the sodium hydroxide solution obtained by primary predrying is used for neutralizing the alkaline tower, and only the sodium hydroxide solution is directly pumped to a liquid caustic soda stock preparation tank of a third floor by a pump, so that the working strength of staff is greatly reduced; 2. after the transformation is integrated, the unit consumption of the potassium hydroxide is reduced to 13KG from the annual scheme target of 25KG, the price of each ton is 9000 yuan according to the calculation of 10762 tons of acesulfame honey yield in 2018, and the cost of the potassium hydroxide for saving raw materials is nearly 116 ten thousand.
Description of the drawings:
FIG. 1 is a process flow diagram of the present invention.
The specific implementation mode is as follows:
as shown in figure 1, the invention provides a triethylamine drying and purifying method, which comprises the following steps:
1. throwing a triethylamine crude product (with the water content of 1-3 percent and partial opalescent turbid liquid) in a triethylamine receiving groove into a sodium hydroxide drying tower at the speed of 30 m/h through a pump, wherein solid sodium hydroxide in the tower accounts for about 1/3 of the volume of the tower, the triethylamine crude product is pumped in from the lower part of the drying tower, and primary drying is carried out through continuous forced circulation of a circulating pump, a small amount of water contained in the triethylamine crude product can form an aqueous solution with sodium hydroxide, the solubility of triethylamine becomes smaller due to the sodium hydroxide solution, the density of triethylamine is 0.73, the sodium hydroxide solution is gathered at the lower part of the drying tower and is fully circulated and mixed, a small amount of water in the triethylamine crude product is separated, and the triethylamine crude product with the water content of 0.3-0.5 percent after primary drying reflows to the triethylamine.
2. Pumping the triethylamine crude product subjected to primary drying in the triethylamine receiving groove into a potassium hydroxide drying tower for secondary circulating drying at the speed of 10 m/h through a circulating pump, wherein solid potassium hydroxide in the tower accounts for about 1/5 of the volume of the tower, and performing secondary circulating drying to obtain the triethylamine crude product which is colorless and transparent and has the water content of 0.1-0.15%;
3. carrying out dry distillation on the triethylamine crude product after the secondary drying through a 4A molecular sieve according to the speed of 3 m/h to obtain refined triethylamine, wherein the moisture content of the refined triethylamine is below 0.1%;
4. pumping the sodium hydroxide aqueous solution after primary drying into a tail gas absorption tower for purifying triethylamine tail gas;
5. the potassium hydroxide aqueous solution after the secondary drying is used in the neutralization section of the production of the acesulfame potassium.
Claims (3)
1. A triethylamine drying and purifying method is characterized by comprising the following steps:
1) pumping the triethylamine crude product with the water content of 1-3% in the triethylamine receiving groove into a sodium hydroxide drying tower through a circulating pump at the speed of 30 m/h, performing primary drying through the circulating pump, wherein water contained in the triethylamine crude product and sodium hydroxide in the drying tower form an aqueous solution, the sodium hydroxide solution is gathered at the bottom of the sodium hydroxide drying tower, and the triethylamine crude product with the water content of 0.3-0.5% after the primary drying is refluxed to the triethylamine receiving groove from the top of the drying tower;
2) pumping the triethylamine crude product after the first-stage drying into a potassium hydroxide drying tower through a circulating pump at the speed of 10 m/h for second-stage drying, wherein the triethylamine crude product after the second-stage drying is colorless and transparent, and the water content is 0.1-0.15%;
3) and (3) carrying out drying on the triethylamine crude product after the secondary drying by using a 4A molecular sieve according to the speed of 3 m/h to obtain refined triethylamine, wherein the moisture content is below 0.1%.
2. The method for drying and purifying triethylamine according to claim 1, wherein:
and pumping the sodium hydroxide aqueous solution subjected to primary drying to a triethylamine tail gas absorption tower for purifying triethylamine tail gas.
3. The method for drying and purifying triethylamine according to claim 1, wherein:
the potassium hydroxide aqueous solution after the secondary drying is used in the neutralization section of the production of the acesulfame potassium.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011027296.8A CN112125808A (en) | 2020-09-26 | 2020-09-26 | Triethylamine drying and purifying method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011027296.8A CN112125808A (en) | 2020-09-26 | 2020-09-26 | Triethylamine drying and purifying method |
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| CN112125808A true CN112125808A (en) | 2020-12-25 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202011027296.8A Pending CN112125808A (en) | 2020-09-26 | 2020-09-26 | Triethylamine drying and purifying method |
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| CN (1) | CN112125808A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114166009A (en) * | 2021-11-26 | 2022-03-11 | 安徽金禾实业股份有限公司 | Drying device and method for triethylamine in acesulfame potassium production |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101085739A (en) * | 2007-07-04 | 2007-12-12 | 四川省乐山市福华农科投资集团有限责任公司 | Dehydration treatment method for triethylamine |
| CN101875612A (en) * | 2009-04-28 | 2010-11-03 | 苏州佳辉化工有限公司 | Method for continuously drying triethylamine in glyphosate production |
| CN103708993A (en) * | 2013-12-30 | 2014-04-09 | 江苏梅兰化工有限公司 | Alkali washing and dehydrating process for crude cracked gas in vinylidene fluoride production |
| CN104193625A (en) * | 2014-09-27 | 2014-12-10 | 安徽金禾实业股份有限公司 | Recovery method of catalyst triethylamine in acesulfame potassium production |
| CN208104264U (en) * | 2018-03-06 | 2018-11-16 | 湖北泰盛化工有限公司 | Triethylamine dried recovered device in a kind of glyphosate production process |
-
2020
- 2020-09-26 CN CN202011027296.8A patent/CN112125808A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101085739A (en) * | 2007-07-04 | 2007-12-12 | 四川省乐山市福华农科投资集团有限责任公司 | Dehydration treatment method for triethylamine |
| CN101875612A (en) * | 2009-04-28 | 2010-11-03 | 苏州佳辉化工有限公司 | Method for continuously drying triethylamine in glyphosate production |
| CN103708993A (en) * | 2013-12-30 | 2014-04-09 | 江苏梅兰化工有限公司 | Alkali washing and dehydrating process for crude cracked gas in vinylidene fluoride production |
| CN104193625A (en) * | 2014-09-27 | 2014-12-10 | 安徽金禾实业股份有限公司 | Recovery method of catalyst triethylamine in acesulfame potassium production |
| CN208104264U (en) * | 2018-03-06 | 2018-11-16 | 湖北泰盛化工有限公司 | Triethylamine dried recovered device in a kind of glyphosate production process |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114166009A (en) * | 2021-11-26 | 2022-03-11 | 安徽金禾实业股份有限公司 | Drying device and method for triethylamine in acesulfame potassium production |
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Application publication date: 20201225 |