CN113105345B - Production process of diethyl aminoethyl hexanoate citrate - Google Patents
Production process of diethyl aminoethyl hexanoate citrate Download PDFInfo
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- CN113105345B CN113105345B CN202110419843.5A CN202110419843A CN113105345B CN 113105345 B CN113105345 B CN 113105345B CN 202110419843 A CN202110419843 A CN 202110419843A CN 113105345 B CN113105345 B CN 113105345B
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- aminoethyl hexanoate
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/41—Preparation of salts of carboxylic acids
- C07C51/412—Preparation of salts of carboxylic acids by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C213/00—Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton
- C07C213/08—Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton by reactions not involving the formation of amino groups, hydroxy groups or etherified or esterified hydroxy groups
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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Abstract
The production process of the diethyl aminoethyl hexanoate citrate comprises the following steps: step one: adding diethyl aminoethyl hexanoate crude oil into a diethyl aminoethyl hexanoate preheating kettle; step two: adding powdery citric acid into a curing reaction kettle with a stirrer, starting stirring, introducing the preheated diethyl aminoethyl hexanoate crude oil in the first step into the curing reaction kettle from a feeding pipeline of the curing reaction kettle, and adding an organic auxiliary agent into the curing reaction kettle through an auxiliary agent feeding port in the curing reaction kettle; step three: continuously introducing an organic auxiliary agent, and introducing cooling water into the curing reaction kettle jacket for cooling until the temperature in the kettle is reduced to 30-40 ℃; step four: and opening a discharging hole at the bottom of the curing reaction kettle for discharging. The invention provides a process for producing diethyl aminoethyl hexanoate citrate, which adopts a one-pot process, can obtain powdery diethyl aminoethyl hexanoate citrate finished product by one-time reaction, does not need filtration and crushing operation, and has the advantages of low raw material consumption, low production energy consumption and short production period.
Description
Technical Field
The invention relates to a production process of diethyl aminoethyl hexanoate citrate, and belongs to the technical field of pesticide production.
Background
The diethyl aminoethyl hexanoate is a substitute product of plant growth regulator gibberellins, auxins, naphthalene rings, adenine and the like. The diethyl aminoethyl hexanoate is not phytohormone, but after the diethyl aminoethyl hexanoate is absorbed by plants, the activity and reasonable proportion balance of auxin, cytokinin, gibberellin, abscisic acid, ethylene and the like in the plants can be regulated, so that the plants develop towards the hope of us. In agricultural practice, it is generally desirable to make the diethyl aminoethyl hexanoate in the form of a solid citrate salt to facilitate application. At present, the production process of the diethyl aminoethyl hexanoate citrate generally comprises the steps of adding citric acid into diethyl aminoethyl hexanoate crude oil, reacting in an ethanol solvent, standing for solidification, filtering, and crushing a filter cake to obtain the diethyl aminoethyl hexanoate citrate. The process has more reaction steps, and the finished product can be obtained through three steps of crystallization, filtration and crushing, wherein the crystallization reaction takes more than 24 hours, the consumption of ethanol is 5-8 times of that of the diethyl aminoethyl hexanoate essential oil, and the whole production process has complex equipment, high energy consumption, high raw material consumption and high labor cost.
Disclosure of Invention
The invention aims at: the method for producing the diethyl aminoethyl hexanoate citrate has the advantages that a one-pot boiling process is adopted, a powdery diethyl aminoethyl hexanoate citrate finished product can be obtained through one-time reaction, filtering and crushing operations are not needed, raw material consumption is low, production energy consumption is low, and production period is short.
In order to achieve the above purpose, the invention adopts the following technical scheme: the production process of the diethyl aminoethyl hexanoate citrate comprises the following steps:
step one: adding the diethyl aminoethyl hexanoate crude oil into a diethyl aminoethyl hexanoate preheating kettle, starting a preheating kettle heating device, and heating the diethyl aminoethyl hexanoate crude oil in the preheating kettle to 60-80 ℃;
step two: adding powdery citric acid into a curing reaction kettle with a stirrer, starting stirring, introducing the preheated diethyl aminoethyl hexanoate crude oil in the step one into the curing reaction kettle from a feeding pipeline of the curing reaction kettle, and adding an organic auxiliary agent into the curing reaction kettle through an auxiliary agent feeding port in the curing reaction kettle while introducing the diethyl aminoethyl hexanoate crude oil, and continuously stirring until the temperature in the kettle is 60-90 ℃;
step three: after the temperature in the kettle reaches 60-90 ℃, continuing to introduce an organic auxiliary agent, introducing cooling water into a jacket of the curing reaction kettle for cooling, and controlling the cooling gradient in the kettle to be 2-5 ℃ per minute until the temperature in the kettle is cooled to 30-40 ℃, wherein the materials in the kettle are in fluffy powder;
step four: starting a discharging hole at the bottom of the curing reaction kettle for discharging;
further, in the second step, the mass ratio of the powdery citric acid to the pre-heated diethyl aminoethyl hexanoate crude oil in the first step is 0.7-1.2:1, the feeding speed of the diethyl aminoethyl hexanoate crude oil into a curing reaction kettle is 10-20 liters/min;
further, in the second step, the organic auxiliary agent and the diethyl aminoethyl hexanoate crude oil are added through the auxiliary agent feed inlet at the same time of introducing the diethyl aminoethyl hexanoate crude oil, and the mass ratio of the organic auxiliary agent to the diethyl aminoethyl hexanoate crude oil is 1:10-16, continuously stirring for 20-60 minutes until the temperature in the kettle is 60-90 ℃;
further, in the third step, the adding speed of the organic additive is 0.2-0.8 liter/min until the temperature in the kettle is reduced to 30-40 ℃; further, the organic auxiliary agent is any one or a mixture of a plurality of liquid organic alcohols.
The invention has the positive and beneficial technical effects that: the invention has the positive and beneficial technical effects that: according to the invention, the curing reaction kettle is arranged, the organic auxiliary agent enters the curing reaction kettle in a continuous feeding mode, the final dosage of the organic auxiliary agent is only 6-10% of the raw oil quantity of the diethyl aminoethyl hexanoate, and in the traditional process, the dosage of ethanol is 5-8 times of the raw oil quantity of the diethyl aminoethyl hexanoate, and the dosage of the organic auxiliary agent is reduced by more than 50-130 times, so that the raw material dosage in the reaction is reduced, and the production cost is reduced. The method for continuously adding the organic auxiliary agent changes the mode of the organic auxiliary agent to participate in the reaction, so that the process can adopt various organic auxiliary agents such as liquid organic alcohol and the like, the process conditions are widened, stirring is carried out in the material curing reaction stage, the curing reaction process is accelerated, the reactant is homogenized, and the product yield is improved to about 99% from about 94% of the original process; the production period of the product is shortened to about 5 hours from one day, the product is stirred and crushed while being solidified, the reaction and the solidification are carried out in a solidification reaction kettle, and the finished product is obtained after the reaction kettle is used for solidification, so that the production links of filtration and crushing are omitted, the production equipment is reduced, and the production cost and the labor cost are reduced.
Drawings
FIG. 1 is a schematic process flow diagram of one embodiment of the present invention.
Detailed Description
In order to more fully explain the practice of the invention, examples of the practice of the invention are provided below, which are merely illustrative of the invention and do not limit the scope of the invention.
The invention will be explained in further detail with reference to the accompanying drawings, in which: 1. an diethyl aminoethyl hexanoate preheating kettle; 2. curing reaction kettle; 3. stirring blades; 4. an organic auxiliary agent storage tank; 5. an organic additive feed pump; 6. and (3) cooling the pipeline.
Example 1: firstly, adding 500kg of diethyl aminoether crude oil into a diethyl aminoether preheating kettle 1, starting a preheating kettle heating device, and heating the diethyl aminoether crude oil in the preheating kettle to 70 ℃; 400kg of powdery citric acid is added into the curing reaction kettle 3, the stirring blade 3 is started to stir, and meanwhile, the diethyl aminoethyl hexanoate crude oil in the preheating kettle is input into the curing reaction kettle from a feed inlet, and the feeding speed of the diethyl aminoethyl hexanoate crude oil is controlled at 15 liters/min; the adding amount of the methanol in the organic aid storage tank is 60 liters, and the methanol in the organic aid storage tank is introduced into a curing reaction kettle while the diethyl aminoethyl hexanoate crude oil is introduced, and the methanol is continuously stirred for 30 minutes until the temperature in the kettle is 70 ℃; continuously introducing methanol, controlling the methanol adding speed to be 0.5-1 liter/min, introducing cooling water into the curing reaction kettle jacket through a cooling pipeline 6 for cooling, and controlling the cooling gradient in the kettle to be 2-5 ℃/min until the temperature in the kettle is cooled to 30 ℃, wherein the materials in the kettle are fluffy powder;
step four: and opening a discharge hole at the bottom of the curing reaction kettle to discharge, thus obtaining 900kg of diethyl aminoethyl hexanoate citrate with the yield of 98.8%.
Example 2: firstly, adding 500kg of diethyl aminoether crude oil into a diethyl aminoether preheating kettle 1, starting a preheating kettle heating device, and heating the diethyl aminoether crude oil in the preheating kettle to 70 ℃; 400kg of powdery citric acid is added into the curing reaction kettle 3, the stirring blade 3 is started to stir, and meanwhile, the diethyl aminoethyl hexanoate crude oil in the preheating kettle is input into the curing reaction kettle from a feed inlet, and the feeding speed of the diethyl aminoethyl hexanoate crude oil is controlled at 20 liters/min; adding 90 liters of ethanol into an organic aid storage tank, and introducing the ethanol in the organic aid storage tank into a curing reaction kettle while introducing the diethyl aminoethyl hexanoate crude oil, wherein the ethanol is continuously stirred for 25 minutes until the temperature in the kettle is 60 ℃; continuously introducing ethanol, controlling the adding speed of the ethanol to be 0.5-1 liter/min, introducing cooling water into the jacket of the curing reaction kettle through a cooling pipeline 6 for cooling, and controlling the cooling gradient in the kettle to be 2-5 ℃/min until the temperature in the kettle is cooled to 35 ℃, wherein the materials in the kettle are fluffy powder;
step four: and opening a discharge hole at the bottom of the curing reaction kettle to discharge, thus obtaining 900kg of diethyl aminoethyl hexanoate citrate with the yield of 99.2%.
Having described embodiments of the present invention in detail, it will be apparent to those skilled in the art that various changes and modifications can be made therein without departing from the scope and spirit of the invention as defined in the appended claims, and any simple, equivalent changes and modifications to the above examples are intended to be within the scope of the present invention and the invention is not limited to the embodiments as set forth in the specification.
Claims (3)
1. A production process of diethyl aminoethyl hexanoate citrate is characterized in that: the method comprises the following steps: step one: adding the diethyl aminoethyl hexanoate crude oil into a diethyl aminoethyl hexanoate preheating kettle, starting a preheating kettle heating device, and heating the diethyl aminoethyl hexanoate crude oil in the preheating kettle to 60-80 ℃; step two: adding powdery citric acid into a curing reaction kettle with a stirrer, starting stirring, introducing the preheated diethyl aminoethyl hexanoate crude oil in the step one into the curing reaction kettle from a feeding pipeline of the curing reaction kettle, and adding an organic auxiliary agent into the curing reaction kettle through an auxiliary agent feeding port in the curing reaction kettle while introducing the diethyl aminoethyl hexanoate crude oil, and continuously stirring until the temperature in the kettle is 60-90 ℃; step three: after the temperature in the kettle reaches 60-90 ℃, continuing to introduce an organic auxiliary agent, introducing cooling water into a jacket of the curing reaction kettle for cooling, and controlling the cooling gradient in the kettle to be 2-5 ℃ per minute until the temperature in the kettle is cooled to 30-40 ℃, wherein the materials in the kettle are fluffy powder; the adding speed of the organic auxiliary agent is 0.2-0.8 liter/min until the temperature in the kettle is reduced to 30-40 ℃;
step four: starting a discharging hole at the bottom of the curing reaction kettle for discharging; in the second step, the organic auxiliary agent and the diethyl aminoethyl hexanoate crude oil are added through the auxiliary agent feed inlet at the same time of introducing the diethyl aminoethyl hexanoate crude oil, wherein the mass ratio of the organic auxiliary agent to the diethyl aminoethyl hexanoate crude oil is 1:10-16, and continuously stirring for 20-60 minutes until the temperature in the kettle is 60-90 ℃.
2. The process for producing diethyl aminoethyl hexanoate citrate according to claim 1, wherein the process comprises the steps of: in the second step, the mass ratio of the powdery citric acid to the pre-heated diethyl aminoethyl hexanoate crude oil in the first step is 0.7-1.2:1, the feeding speed of the diethyl aminoethyl hexanoate crude oil into the curing reaction kettle is 10-20 liters/min.
3. The process for producing diethyl aminoethyl hexanoate citrate according to claim 1, wherein the process comprises the steps of: the organic auxiliary agent is any one or a mixture of a plurality of liquid organic alcohols.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1280766A (en) * | 1999-07-16 | 2001-01-24 | 吴少宁 | Plant growth regulator and its preparing process |
| CN1666975A (en) * | 2005-03-11 | 2005-09-14 | 谢云漫 | Process for preparing dialkylamino ethanol carboxylate and its salts |
| CN101293845A (en) * | 2007-04-27 | 2008-10-29 | 中国科学院化学研究所 | Method for synthesizing hexanoic acid diethylaminoethanol ester citrate with one-step method |
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- 2021-04-19 CN CN202110419843.5A patent/CN113105345B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1280766A (en) * | 1999-07-16 | 2001-01-24 | 吴少宁 | Plant growth regulator and its preparing process |
| CN1666975A (en) * | 2005-03-11 | 2005-09-14 | 谢云漫 | Process for preparing dialkylamino ethanol carboxylate and its salts |
| CN101293845A (en) * | 2007-04-27 | 2008-10-29 | 中国科学院化学研究所 | Method for synthesizing hexanoic acid diethylaminoethanol ester citrate with one-step method |
Non-Patent Citations (1)
| Title |
|---|
| 一种胺鲜酯合成方法的研究;余永德;《四川化工》;20200815;第23卷(第4期);第6页4.2 * |
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