CN112939792A - Preparation method of high-purity trialkanolamine - Google Patents
Preparation method of high-purity trialkanolamine Download PDFInfo
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- CN112939792A CN112939792A CN202011624825.2A CN202011624825A CN112939792A CN 112939792 A CN112939792 A CN 112939792A CN 202011624825 A CN202011624825 A CN 202011624825A CN 112939792 A CN112939792 A CN 112939792A
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- tubular reactor
- ethylene oxide
- product mixture
- monoethanolamine
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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
- C07C213/04—Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton by reaction of ammonia or amines with olefin oxides or halohydrins
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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
- C07C213/10—Separation; Purification; Stabilisation; Use of additives
Abstract
The invention discloses a preparation method of high-purity trialkanolamine, belonging to the technical field of trialkanolamine production, comprising the following steps: step 1: adding ethylene oxide and liquid ammonia into a first tubular reactor, and reacting in the presence of a catalyst to obtain a first product mixture of monoethanolamine, diethanolamine and triethanolamine; step 2: separating out the monoethanolamine and the diethanolamine in the first tubular reactor in the step 1 independently, storing the monoethanolamine and the diethanolamine into a second tubular reactor and a third tubular reactor respectively, adding ethylene oxide into the second tubular reactor, and reacting the ethylene oxide with the monoethanolamine in the presence of a catalyst to obtain a second product mixture; the method can effectively improve the purity of the trialkanolamine through the processing procedure of multiple mixing reactions, and simultaneously adopts the reduced pressure rectification to ensure that the pressure bottom and the pressure drop of the system are small, and the temperature is controlled, thereby ensuring the color and the quality.
Description
Technical Field
The invention relates to the technical field of trialkanolamine production, in particular to a preparation method of high-purity trialkanolamine.
Background
A commercial method for producing ethanolamine by reacting ethylene oxide with ammonia, a method of reacting ethylene oxide with aqueous ammonia (aqueous ammonia method) is prevalent. The process results in three products, monoethanolamine, diethanolamine and triethanolamine. Therefore, in order to obtain triethanolamine, monoethanolamine, diethanolamine, unreacted ammonia and contained water must be separated by vacuum distillation. Since the crude triethanolamine thus obtained contains 4 to 8% of diethanolamine and 0.1 to 1% of high boiling substances, it is subjected to vacuum distillation. In the recovered distillate, the initial fraction contains diethanolamine at a high concentration, and the final or after-fraction contains high-boiling compounds at a high concentration, so that this vacuum distillation can produce high-purity trialkanolamine only at a low yield.
Disclosure of Invention
The object of the present invention is to provide a process for producing a high-purity trialkanolamine, which solves the problem of producing a high-purity trialkanolamine at a low yield as set forth in the above-mentioned background art.
In order to achieve the purpose, the invention provides the following technical scheme: a process for producing a high-purity trialkanolamine, comprising the steps of:
step 1: adding ethylene oxide and liquid ammonia into a first tubular reactor, and reacting in the presence of a catalyst to obtain a first product mixture of monoethanolamine, diethanolamine and triethanolamine;
step 2: separating out the monoethanolamine and the diethanolamine in the first tubular reactor in the step 1 independently, storing the monoethanolamine and the diethanolamine into a second tubular reactor and a third tubular reactor respectively, adding ethylene oxide into the second tubular reactor, and reacting the ethylene oxide with the monoethanolamine in the presence of a catalyst to obtain a second product mixture;
and step 3: adding the product mixture II obtained in the step 2 into a tubular reactor II, and adding ethylene oxide into the tubular reactor II to enable the product mixture II, the ethylene oxide and diethanol amine to react in the tubular reactor II to obtain a product mixture III;
and 4, step 4: and (3) adding the product mixture III obtained in the step (3) into a tubular reactor III, and reacting the product mixture III with triethanolamine to obtain the high-purity trialkanolamine.
Preferably, the catalyst comprises one or more of a zeolite catalyst and water.
Preferably, the reaction temperature in the step 1 is 160-180 ℃, and the reaction pressure in the step 1 is 133-266 pa.
Preferably, the reaction temperature in the step 2 is 100-150 ℃, and the reaction pressure in the step 2 is 133-266 pa.
Preferably, the reaction temperature in the step 3 is 70-100 ℃, and the reaction pressure in the step 3 is 133-266 pa.
Preferably, the reaction temperature in the step 4 is 160-180 ℃, and the reaction pressure in the step 4 is 133-266 pa.
Preferably, the reaction time in the step 1 is 10-20min, the reaction time in the steps 2 and 3 is 10-30min, and the reaction time in the step 4 is 30 min.
Preferably, the amounts of ethylene oxide added in the steps 1, 2 and 3 are the same, and the amount of ethylene oxide added in the step 4 is 2 times the amount of ethylene oxide added in the steps 1, 2 and 3.
Compared with the prior art, the invention has the beneficial effects that:
the method can effectively improve the purity of the trialkanolamine through the processing procedure of multiple mixing reactions, and simultaneously adopts the reduced pressure rectification to ensure that the pressure bottom and the pressure drop of the system are small, and the temperature is controlled, thereby ensuring the color and the quality.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all 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.
In the description of the present invention, it is to be understood that the terms "upper", "lower", "front", "rear", "left", "right", "top", "bottom", "inner", "outer", and the like, indicate orientations and positional relationships only for convenience in describing the present invention and simplifying the description, but do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be construed as limiting the present invention.
The invention provides a technical scheme that:
example 1:
a process for producing a high-purity trialkanolamine, comprising the steps of:
step 1: adding ethylene oxide and liquid ammonia into a first tubular reactor, and reacting in the presence of a catalyst to obtain a first product mixture of monoethanolamine, diethanolamine and triethanolamine, wherein the reaction temperature is 180 ℃, the reaction pressure is 220pa, and the reaction time is 10 min;
step 2: the monoethanolamine and the diethanolamine in the first tubular reactor in the step 1 are separated separately and stored in a second tubular reactor and a third tubular reactor respectively, ethylene oxide is added into the second tubular reactor and reacts with the monoethanolamine in the presence of a catalyst to obtain a second product mixture, the reaction temperature is 150 ℃, the reaction pressure is 200pa, and the reaction time is 30 min;
and step 3: adding the product mixture II obtained in the step 2 into a tubular reactor II, adding ethylene oxide into the tubular reactor II, and reacting the product mixture II, the ethylene oxide and diethanol amine in the tubular reactor II to obtain a product mixture III, wherein the reaction temperature is 100 ℃, the reaction pressure is 200pa, and the reaction time is 30 min;
and 4, step 4: and (3) adding the product mixture III obtained in the step (3) into a tubular reactor III, and reacting the product mixture III with triethanolamine to obtain the high-purity trialkanolamine, wherein the reaction temperature is 180 ℃, the reaction pressure is 250pa, and the reaction time is 30 min.
The catalyst comprises a zeolite catalyst and water.
The ethylene oxide amount in the step 1, the step 2 and the step 3 is the same, and the ethylene oxide amount in the step 4 is 2 times of the ethylene oxide amount in the step 1, the step 2 and the step 3.
Example 2:
a process for producing a high-purity trialkanolamine, comprising the steps of:
step 1: adding ethylene oxide and liquid ammonia into a first tubular reactor, and reacting in the presence of a catalyst to obtain a first product mixture of monoethanolamine, diethanolamine and triethanolamine, wherein the reaction temperature is 170 ℃, the reaction pressure is 220pa, and the reaction time is 10 min;
step 2: the monoethanolamine and the diethanolamine in the first tubular reactor in the step 1 are separated separately and stored in a second tubular reactor and a third tubular reactor respectively, ethylene oxide is added into the second tubular reactor and reacts with the monoethanolamine in the presence of a catalyst to obtain a second product mixture, the reaction temperature is 120 ℃, the reaction pressure is 200pa, and the reaction time is 30 min;
and step 3: adding the product mixture II obtained in the step 2 into a tubular reactor II, adding ethylene oxide into the tubular reactor II, and reacting the product mixture II, the ethylene oxide and diethanol amine in the tubular reactor II to obtain a product mixture III, wherein the reaction temperature is 80 ℃, the reaction pressure is 200pa, and the reaction time is 30 min;
and 4, step 4: and (3) adding the product mixture III obtained in the step (3) into a tubular reactor III, and reacting the product mixture III with triethanolamine to obtain the high-purity trialkanolamine, wherein the reaction temperature is 170 ℃, the reaction pressure is 250pa, and the reaction time is 30 min.
The catalyst comprises a zeolite catalyst and water.
The ethylene oxide amount in the step 1, the step 2 and the step 3 is the same, and the ethylene oxide amount in the step 4 is 2 times of the ethylene oxide amount in the step 1, the step 2 and the step 3.
Example 3:
a process for producing a high-purity trialkanolamine, comprising the steps of:
step 1: adding ethylene oxide and liquid ammonia into a first tubular reactor, and reacting in the presence of a catalyst to obtain a first product mixture of monoethanolamine, diethanolamine and triethanolamine, wherein the reaction temperature is 160 ℃, the reaction pressure is 250pa, and the reaction time is 20 min;
step 2: the monoethanolamine and the diethanolamine in the first tubular reactor in the step 1 are separated independently and stored in a second tubular reactor and a third tubular reactor respectively, ethylene oxide is added into the second tubular reactor and reacts with the monoethanolamine in the presence of a catalyst to obtain a second product mixture, the reaction temperature is 100 ℃, the reaction pressure is 220pa, and the reaction time is 30 min;
and step 3: adding the product mixture II obtained in the step 2 into a tubular reactor II, adding ethylene oxide into the tubular reactor II, and reacting the product mixture II, the ethylene oxide and diethanol amine in the tubular reactor II to obtain a product mixture III, wherein the reaction temperature is 70 ℃, the reaction pressure is 220pa, and the reaction time is 30 min;
and 4, step 4: and (3) adding the product mixture III obtained in the step (3) into a tubular reactor III, and reacting the product mixture III with triethanolamine to obtain the high-purity trialkanolamine, wherein the reaction temperature is 180 ℃, the reaction pressure is 250pa, and the reaction time is 30 min.
The catalyst comprises a zeolite catalyst and water.
The ethylene oxide amount in the step 1, the step 2 and the step 3 is the same, and the ethylene oxide amount in the step 4 is 2 times of the ethylene oxide amount in the step 1, the step 2 and the step 3.
While there have been shown and described the fundamental principles and essential features of the invention and advantages thereof, it will be apparent to those skilled in the art that the invention is not limited to the details of the foregoing exemplary embodiments, but is capable of other specific forms without departing from the spirit or essential characteristics thereof; the present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
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 (8)
1. A process for producing a high-purity trialkanolamine, characterized by: the method comprises the following steps:
step 1: adding ethylene oxide and liquid ammonia into a first tubular reactor, and reacting in the presence of a catalyst to obtain a first product mixture of monoethanolamine, diethanolamine and triethanolamine;
step 2: separating out the monoethanolamine and the diethanolamine in the first tubular reactor in the step 1 independently, storing the monoethanolamine and the diethanolamine into a second tubular reactor and a third tubular reactor respectively, adding ethylene oxide into the second tubular reactor, and reacting the ethylene oxide with the monoethanolamine in the presence of a catalyst to obtain a second product mixture;
and step 3: adding the product mixture II obtained in the step 2 into a tubular reactor II, and adding ethylene oxide into the tubular reactor II to enable the product mixture II, the ethylene oxide and diethanol amine to react in the tubular reactor II to obtain a product mixture III;
and 4, step 4: and (3) adding the product mixture III obtained in the step (3) into a tubular reactor III, and reacting the product mixture III with triethanolamine to obtain the high-purity trialkanolamine.
2. The process for producing a high-purity trialkanolamine according to claim 1, characterized in that: the catalyst comprises one or more of a zeolite catalyst and water.
3. The process for producing a high-purity trialkanolamine according to claim 1, characterized in that: the reaction temperature in the step 1 is 160-180 ℃, and the reaction pressure in the step 1 is 133-266 pa.
4. The process for producing a high-purity trialkanolamine according to claim 1, characterized in that: the reaction temperature in the step 2 is 100-150 ℃, and the reaction pressure in the step 2 is 133-266 pa.
5. The process for producing a high-purity trialkanolamine according to claim 1, characterized in that: the reaction temperature in the step 3 is 70-100 ℃, and the reaction pressure in the step 3 is 133-266 pa.
6. The process for producing a high-purity trialkanolamine according to claim 1, characterized in that: the reaction temperature in the step 4 is 160-180 ℃, and the reaction pressure in the step 4 is 133-266 pa.
7. The process for producing a high-purity trialkanolamine according to claim 1, characterized in that: the reaction time in the step 1 is 10-20min, the reaction time in the steps 2 and 3 is 10-30min, and the reaction time in the step 4 is 30 min.
8. The process for producing a high-purity trialkanolamine according to claim 1, characterized in that: the ethylene oxide amount in the step 1, the step 2 and the step 3 is the same, and the ethylene oxide amount in the step 4 is 2 times of the ethylene oxide amount in the step 1, the step 2 and the step 3.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116082171A (en) * | 2023-04-11 | 2023-05-09 | 山东友泉新材料有限公司 | Application of water absorbing sieve in preparation of isopropanolamine and preparation method of isopropanolamine |
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| CN1519225A (en) * | 2003-02-03 | 2004-08-11 | ��ʽ�����ձ���ý | Process for prepn. of high pureness trialkanolamine |
| CN101033194A (en) * | 2003-02-03 | 2007-09-12 | 株式会社日本触媒 | Process for producing high purity trialkanolamine |
| CN106478430A (en) * | 2016-09-30 | 2017-03-08 | 大连微凯化学有限公司 | A kind of triethanolamine continuous production device and technique |
| CN106608832A (en) * | 2015-10-22 | 2017-05-03 | 中国石油化工股份有限公司 | Technological method for cooperatively producing ethanolamine through liquid ammonia method and ammonium hydroxide method |
| CN108698979A (en) * | 2016-03-18 | 2018-10-23 | 株式会社日本触媒 | The manufacturing method of ethyl alcohol amine |
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2020
- 2020-12-31 CN CN202011624825.2A patent/CN112939792A/en active Pending
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| CN1519225A (en) * | 2003-02-03 | 2004-08-11 | ��ʽ�����ձ���ý | Process for prepn. of high pureness trialkanolamine |
| CN101033194A (en) * | 2003-02-03 | 2007-09-12 | 株式会社日本触媒 | Process for producing high purity trialkanolamine |
| CN106608832A (en) * | 2015-10-22 | 2017-05-03 | 中国石油化工股份有限公司 | Technological method for cooperatively producing ethanolamine through liquid ammonia method and ammonium hydroxide method |
| CN108698979A (en) * | 2016-03-18 | 2018-10-23 | 株式会社日本触媒 | The manufacturing method of ethyl alcohol amine |
| CN106478430A (en) * | 2016-09-30 | 2017-03-08 | 大连微凯化学有限公司 | A kind of triethanolamine continuous production device and technique |
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| CN116082171A (en) * | 2023-04-11 | 2023-05-09 | 山东友泉新材料有限公司 | Application of water absorbing sieve in preparation of isopropanolamine and preparation method of isopropanolamine |
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