CN112409189A - Continuous process for recycling triethylamine - Google Patents
Continuous process for recycling triethylamine Download PDFInfo
- Publication number
- CN112409189A CN112409189A CN202011356564.0A CN202011356564A CN112409189A CN 112409189 A CN112409189 A CN 112409189A CN 202011356564 A CN202011356564 A CN 202011356564A CN 112409189 A CN112409189 A CN 112409189A
- Authority
- CN
- China
- Prior art keywords
- liquid
- water separator
- triethylamine
- water
- continuous process
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 title claims abstract description 84
- 238000010924 continuous production Methods 0.000 title claims abstract description 12
- 238000004064 recycling Methods 0.000 title claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 46
- 239000007788 liquid Substances 0.000 claims abstract description 38
- 238000000034 method Methods 0.000 claims abstract description 14
- 230000008569 process Effects 0.000 claims abstract description 11
- 230000003068 static effect Effects 0.000 claims abstract description 11
- 239000002351 wastewater Substances 0.000 claims abstract description 9
- ILWRPSCZWQJDMK-UHFFFAOYSA-N triethylazanium;chloride Chemical compound Cl.CCN(CC)CC ILWRPSCZWQJDMK-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000003513 alkali Substances 0.000 claims abstract description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 2
- 238000011084 recovery Methods 0.000 abstract description 7
- 239000002274 desiccant Substances 0.000 abstract description 3
- 239000005562 Glyphosate Substances 0.000 description 4
- XDDAORKBJWWYJS-UHFFFAOYSA-N glyphosate Chemical compound OC(=O)CNCP(O)(O)=O XDDAORKBJWWYJS-UHFFFAOYSA-N 0.000 description 4
- 229940097068 glyphosate Drugs 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- JEUXZUSUYIHGNL-UHFFFAOYSA-N n,n-diethylethanamine;hydrate Chemical compound O.CCN(CC)CC JEUXZUSUYIHGNL-UHFFFAOYSA-N 0.000 description 3
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000006184 cosolvent Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000002363 herbicidal effect Effects 0.000 description 2
- 239000004009 herbicide Substances 0.000 description 2
- 239000004471 Glycine Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000012824 chemical production Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Images
Classifications
-
- 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
- C07C209/84—Purification
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a continuous process for recycling triethylamine, which comprises the following steps of S1, adding process wastewater containing triethylamine hydrochloride into a static mixer, S2, simultaneously adding liquid alkali into the static mixer, adjusting the pH value of liquid at the outlet of the static mixer, S3, adding mixed liquid with the adjusted pH value into a first water separator, ensuring the temperature in the first water separator to be 60-70 ℃, S4, continuously separating the mixed liquid through the first water separator, separating upper-layer liquid (triethylamine) of the mixed liquid, feeding the upper-layer liquid into a cooler, feeding lower-layer solution into a second water separator, keeping the temperature in the second water separator to be 60-70 ℃, and S5, continuously separating the solution in the second water separator, feeding the upper-layer liquid into the cooler, wherein the lower-layer solution is wastewater. In the implementation process of the invention, the use of steam and drying agent can be reduced, and the recovery rate of triethylamine can be improved.
Description
Technical Field
The invention belongs to the technical field of triethylamine recovery, and particularly relates to a continuous process for recovering triethylamine.
Background
Triethylamine is an acid-binding agent and a cosolvent which are widely used in the chemical production process, and the triethylamine is recovered and recycled in the production process, so that the triethylamine is an important link for reducing consumption, saving cost and protecting environment
For example: a large amount of triethylamine is used as a cosolvent in the glycine method production process of herbicide glyphosate. Triethylamine in some fine chemical products is also widely used as an acid-binding agent, and finally triethylamine hydrochloride is generated and dissolved in a water phase.
The current recovery process is as follows:
the triethylamine hydrochloride in the water phase is dissociated out by neutralizing the triethylamine hydrochloride with liquid alkali, and then the triethylamine is rectified and recycled in a rectifying tower.
Because triethylamine-water can form binary azeotrope (the azeotropic composition is triethylamine: water: 90: 10 azeotropic temperature is 75 ℃), the final product is mostly triethylamine water solution with about 90 percent although a high-efficiency rectifying tower is used in the rectifying process.
When the catalyst is recycled, if the reaction system is forbidden to use water, a drying agent is used for further dehydration, and the catalyst can be reused.
Not only a large amount of energy (steam) and a large amount of drying agent are consumed in the recovery process, but also the loss of triethylamine is greatly increased in the recovery process.
The invention content is as follows:
aiming at the situation, in order to overcome the defects of the prior art, the invention provides a continuous process for recovering triethylamine, which effectively solves the problems in the background art.
In order to achieve the purpose, the invention provides the following technical scheme: a continuous process for recovering triethylamine comprises the following steps,
s1, adding the process wastewater containing triethylamine hydrochloride into a static mixer,
s2, simultaneously adding liquid caustic soda into the static mixer, adjusting the pH value of the outlet of the static mixer,
s3, adding the mixed liquid with the adjusted pH value into the first water separator, ensuring the temperature in the first water separator to be between 60 and 70 ℃,
s4, after the mixed liquid is continuously separated by the first water separator, separating the upper layer liquid and making the upper layer liquid flow into the cooler, making the lower layer liquid flow into the second water separator, keeping the temperature in the second water separator between 60 ℃ and 70 ℃,
and S5, continuously separating the solution in the second water separator, and allowing the upper-layer solution to flow into a cooler, wherein the lower-layer solution is wastewater.
Preferably, the residence time of the liquid flowing into the first water divider in the first water divider is not less than 2 hours, and the residence time of the liquid flowing into the second water divider in the second water divider is not less than 1 hour.
Preferably, the ratio of the diameter to the height of the first water separator is 1: 5-6.
Preferably, the diameter-to-height ratio of the second water separator is 1: 9-10.
Preferably, the concentration of the liquid alkali in the S2 is between 20% and 30%, and the pH value of the liquid after adjustment is between 12 and 13 in the S2.
The theoretical basis of the invention is as follows:
the triethylamine is dissolved in water, and the triethylamine-water is partially miscible at normal temperature and can be miscible at any proportion below 18.5 ℃. The triethylamine phase can reach more than 98 percent when the intersolubility degree is reduced to 70 ℃ along with the temperature rise and the triethylamine content in the water phase is less than 1 percent
Compared with the prior art, the beneficial effects of the invention are illustrated by the implementation effects:
the new process is used for the production of herbicide glyphosate, and the steam consumption of 100 percent glyphosate raw pesticide per ton is reduced by 600 kg/t. The consumption of 100 percent glyphosate technical triethylamine per ton is reduced from 60kg/t to 25kg/t, and obvious economic benefit is obtained.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:
FIG. 1 is a schematic flow diagram of a primary recovery process;
FIG. 2 is a schematic flow diagram of the recovery process of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments; 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.
As shown in the figure 1-2, the invention discloses a continuous process for recycling triethylamine, which comprises the steps of simultaneously adding process wastewater containing triethylamine hydrochloride and 20-30% alkali liquor into a static mixer, fully mixing the alkali liquor and the process wastewater containing triethylamine hydrochloride in the static mixer, ensuring the pH value of the mixed liquid to be between 12 and 13, feeding the fully mixed liquid into a first automatic water separator, ensuring the temperature in the first automatic water separator to be between 60 and 70 ℃, ensuring the time of the mixed liquid in the first automatic water separator to be not less than 2 hours, feeding the upper liquid into a cooler, feeding the lower liquid into a second automatic water separator, ensuring the temperature of the second automatic water separator to be between 60 and 70 ℃, ensuring the time of the fed liquid in the second automatic water separator to be not less than 1 hour, and then, the upper layer liquid in the second automatic water separator enters a cooler, the lower layer liquid in the second automatic water separator is discharged as waste water, the liquid in the cooler is cooled and then enters a storage tank, and the concentration of triethylamine in the liquid is more than 98%.
The diameter-height ratio of the first water separator is 1:5-6
The diameter-height ratio of the second water divider is 1:9-10
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (5)
1. A continuous process for recovering triethylamine is characterized in that: comprises the following steps of (a) carrying out,
s1, adding the process wastewater containing triethylamine hydrochloride into a static mixer,
s2, simultaneously adding liquid caustic soda into the static mixer, adjusting the pH value of the liquid at the outlet of the static mixer,
s3, adding the mixed liquid with the adjusted pH value into the first water separator, ensuring the temperature in the first water separator to be between 60 and 70 ℃,
s4, after the mixed liquid is continuously separated by the first water separator, the upper layer liquid is separated and flows into the cooler, the lower layer solution flows into the second water separator, the temperature in the second water separator is kept between 60 ℃ and 70 ℃,
and S5, after the solution in the second water separator is continuously separated, enabling the upper-layer solution to flow into the cooler and the lower-layer solution to be wastewater.
2. The continuous process for recycling triethylamine according to claim 1, wherein: the stay time of the liquid flowing into the first water divider in the first water divider is not less than 2 hours, and the stay time of the liquid flowing into the first water divider in the first water divider is not less than 1 hour.
3. The continuous process for recycling triethylamine according to claim 1, wherein:
the diameter-height ratio of the first water divider is 1: 5-6.
4. The continuous process for recycling triethylamine according to claim 1, wherein: the diameter-height ratio of the second water divider is 1: 9-10.
5. The continuous process for recycling triethylamine according to claim 1, wherein: the concentration of the liquid alkali in the S2 is between 20% and 30%, and the pH value of the liquid after adjustment is between 12 and 13 in the S2.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011356564.0A CN112409189A (en) | 2020-11-26 | 2020-11-26 | Continuous process for recycling triethylamine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011356564.0A CN112409189A (en) | 2020-11-26 | 2020-11-26 | Continuous process for recycling triethylamine |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112409189A true CN112409189A (en) | 2021-02-26 |
Family
ID=74843087
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011356564.0A Pending CN112409189A (en) | 2020-11-26 | 2020-11-26 | Continuous process for recycling triethylamine |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112409189A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114181092A (en) * | 2021-12-02 | 2022-03-15 | 泰兴华盛精细化工有限公司 | Method for recycling triethylamine in vinylene carbonate production process |
| CN114213257A (en) * | 2021-12-09 | 2022-03-22 | 聊城鲁西聚碳酸酯有限公司 | System and method for recycling interface catalyst |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103304423A (en) * | 2013-06-18 | 2013-09-18 | 湖北泰盛化工有限公司 | Method for recovering triethylamine from glyphosate material |
| CN105111088A (en) * | 2015-09-02 | 2015-12-02 | 江苏瑞克医药科技有限公司 | Method for recycling triethylamine from wastewater containing triethylamine hydrochloride |
| CN106543009A (en) * | 2015-09-21 | 2017-03-29 | 江苏瑞科医药科技有限公司 | The recovery method of triethylamine in a kind of effective PSI-6206 intermediate synthesis |
| CN111978269A (en) * | 2020-09-23 | 2020-11-24 | 青岛科技大学 | Continuous production process and device for isatoic anhydride |
-
2020
- 2020-11-26 CN CN202011356564.0A patent/CN112409189A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103304423A (en) * | 2013-06-18 | 2013-09-18 | 湖北泰盛化工有限公司 | Method for recovering triethylamine from glyphosate material |
| CN105111088A (en) * | 2015-09-02 | 2015-12-02 | 江苏瑞克医药科技有限公司 | Method for recycling triethylamine from wastewater containing triethylamine hydrochloride |
| CN106543009A (en) * | 2015-09-21 | 2017-03-29 | 江苏瑞科医药科技有限公司 | The recovery method of triethylamine in a kind of effective PSI-6206 intermediate synthesis |
| CN111978269A (en) * | 2020-09-23 | 2020-11-24 | 青岛科技大学 | Continuous production process and device for isatoic anhydride |
Non-Patent Citations (1)
| Title |
|---|
| 任不凡,周海杨,胡跃华,陈晓祥: "烷基酯法草甘膦生产工艺中的三乙胺连续化回收", no. 06, pages 1 - 4 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114181092A (en) * | 2021-12-02 | 2022-03-15 | 泰兴华盛精细化工有限公司 | Method for recycling triethylamine in vinylene carbonate production process |
| CN114213257A (en) * | 2021-12-09 | 2022-03-22 | 聊城鲁西聚碳酸酯有限公司 | System and method for recycling interface catalyst |
| CN114213257B (en) * | 2021-12-09 | 2023-08-01 | 聊城鲁西聚碳酸酯有限公司 | System and method for recycling interface catalyst |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN112409189A (en) | Continuous process for recycling triethylamine | |
| CA1114132A (en) | Process for selective removal of sodium sulfate from an aqueous slurry | |
| CN105417823A (en) | Method of recycling ammonia from low-concentration ammonium chloride waste water | |
| CN102822138B (en) | Process for producing ammonium salts | |
| CN105236450A (en) | Total-circulation clean production process of baking soda through double decomposition reaction | |
| CN112552197B (en) | Kettle type continuous glycine production method | |
| CN106277005B (en) | A kind of method that ice crystal, calcium carbonate and sodium sulphate are reclaimed in the resource from calcium fluoride sludge | |
| CN110980782A (en) | Method for producing high-purity magnesium sulfate by using alkylation waste sulfuric acid and application thereof | |
| CN103011503B (en) | Method and device for wastewater treatment and salt extraction during hydrazine hydrate production by ketazine process | |
| CN108585335B (en) | Method for treating phenylhydrazine hydrochloride production waste liquid and recovering resources | |
| CN106591873A (en) | Treating and recycling method of sodium hypochlorite-containing waste liquid | |
| CN213446254U (en) | System for calcium sulfate is prepared and hydrochloric acid is retrieved to calcium chloride | |
| CN101906082A (en) | Method for synthesizing TBBS (Tertiarybutyl Benzothiazole Sulfenamide) by mechanically applying mother solution | |
| CN104844414A (en) | Equipment and process for recovering glyphosate solvent during production with glycine method | |
| CN105272839A (en) | Synthesis method of diphenyl ketone | |
| CN113599990B (en) | Anhydrous desulfurizing agent and application thereof | |
| CN109180605A (en) | The method of the direct synthetic rubber vulcanization accelerator TBBS of resin in waste water | |
| CN214915926U (en) | Device for continuously decyanating cyanoacetic acid aqueous solution | |
| CN114225880A (en) | System and method for continuously and efficiently synthesizing hexamethyldisilazane in multi-tower counter-flow manner | |
| CN219518808U (en) | Green chlorine hydrogen internal consumption absorption system in foaming agent production | |
| CN106748895A (en) | A kind of processing method of ADC foaming agent condensed mother liquors | |
| CN219502705U (en) | Biurea production ammonia recovery system | |
| CN218357408U (en) | Hydrazine hydrate refining desalination system | |
| CN110067005A (en) | A kind of potassium hydroxide ionic membrane method production system | |
| CN115627372B (en) | Rare earth precipitation method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210226 |
|
| RJ01 | Rejection of invention patent application after publication |