CN107226781B - Method for continuously producing N-methyl isopropanolamine - Google Patents
Method for continuously producing N-methyl isopropanolamine Download PDFInfo
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- CN107226781B CN107226781B CN201710363686.4A CN201710363686A CN107226781B CN 107226781 B CN107226781 B CN 107226781B CN 201710363686 A CN201710363686 A CN 201710363686A CN 107226781 B CN107226781 B CN 107226781B
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- 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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Abstract
The invention relates to the technical field of petrochemical products, in particular to a method for continuously producing N-methyl isopropanolamine, which comprises the steps of respectively metering monomethylamine and propylene oxide, uniformly mixing the monomethylamine and the propylene oxide in a mixer, reacting the monomethylamine and the propylene oxide in the reactor, and separating and purifying an obtained crude product containing the N-methyl isopropanolamine sequentially through an amine distillation tower, a light component tower and a reduced pressure rectifying tower to obtain a refined product N-methyl isopropanolamine.
Description
Technical Field
The invention relates to the technical field of petrochemical products, in particular to a method for continuously producing N-methyl isopropanolamine.
Background
The N-methyl isopropanolamine is colorless transparent liquid with ammonia smell, and is soluble in water, methanol and ethanol, and slightly soluble in toluene, acetone, petroleum ether and other organic solvent, and has specific gravity of 0.896g/cm at normal temperature and pressure3The boiling point was 146 ℃, the flash point was 51 ℃, the viscosity was 2.1CP, and the refractive index was 1.438. In the actual production, the N-methyl isopropanolamine is widely applied to removing hydrogen sulfide from natural gas and oil refinery dry gas, and removing carbon dioxide from large-scale synthetic ammonia, so that the N-methyl isopropanolamine is a novel selective desulfurization and decarburization solvent with excellent performance, and has the advantages of high selectivity, low solvent consumption, remarkable energy-saving effect, difficulty in degradation and the like. In addition, N-methyl isopropanolamine may be also used in fiber assistant, fabric softener, tanning agent, pesticide, cutting oil, etc. and is one of the widely used emulsifier. Therefore, the N-methyl isopropanolamine has strong applicability and is a solvent which is greatly required in industrial production, so that the N-methyl isopropanolamine needs to be produced in large quantities. However, no industrial process for efficiently producing N-methyl isopropanolamine is available in the industry, so that the requirement of industrial production on N-methyl isopropanolamine cannot be met.
Disclosure of Invention
In view of the above technical problems in the prior art, the present invention aims to provide a method for continuously producing N-methyl isopropanolamine, which can continuously and stably produce N-methyl isopropanolamine in batches, and has the advantages of saving labor and energy, and stable product quality.
In order to achieve the purpose, the invention provides the following technical scheme:
provides a method for continuously producing N-methyl isopropanolamine, which is characterized by comprising the following steps: the method comprises the following steps:
step one, feeding: respectively metering propylene oxide and monomethylamine, and continuously feeding into a mixer;
wherein the molar ratio of the propylene oxide to the monomethylamine is 1: 1.1 to 1.3;
step two, mixing: regulating the temperature and the pressure of the mixer, and mixing monomethylamine and propylene oxide in the mixer to obtain a uniformly mixed mixture;
step three, reaction: continuously feeding the mixture obtained in the step two into a reactor, regulating the temperature and pressure of the reactor, and reacting the mixture in the reactor to obtain a first crude product containing N-methyl isopropanolamine;
step four, removing monomethylamine: continuously feeding the first crude product obtained in the step three into the middle part of an amine distilling tower, and then adjusting the pressure of the amine distilling tower, the tower top temperature of the amine distilling tower and the tower bottom temperature to distill off the unreacted monomethylamine from the tower top, wherein the tower bottom is a second crude product for removing the monomethylamine;
step five, removing an intermediate: continuously feeding the second crude product obtained in the step three into the middle of a light component tower, and regulating and controlling the pressure of the light component tower, the tower top temperature of the light component tower and the tower kettle temperature, so that an intermediate of the second crude product is distilled out of the top of the light component tower, and the tower kettle is a third crude product from which the intermediate is removed;
and step six, rectifying an N-methyl isopropanolamine product: and D, continuously feeding the third crude product obtained in the fifth step into the middle part of a reduced pressure rectifying tower, and then adjusting the pressure of the reduced pressure rectifying tower, the tower top temperature and the tower kettle temperature of the reduced pressure rectifying tower to distill the N-methyl isopropanolamine from the top of the reduced pressure rectifying tower to obtain an N-methyl isopropanolamine refined product, wherein the tower kettle liquid is a byproduct.
In the above technical scheme, the propylene oxide and monomethylamine continuously enter the mixer through metering pumps respectively.
In the above technical scheme, in the second step, the temperature of the mixer is 10-30 ℃, and the pressure is 3.5-5.0 MPa.
In the technical scheme, in the third step, the temperature of the reactor is 110-130 ℃, and the pressure is 3.5-5.0 MPa.
In the technical scheme, in the third step, the reaction time of the mixture in the reactor is 2-5 min.
In the technical scheme, in the fourth step, the pressure of the amine steaming tower is 0.05-0.4 MPa, the tower top temperature of the amine steaming tower is 80-110 ℃, and the tower kettle temperature of the amine steaming tower is 130-160 ℃.
In the above technical scheme, in the fifth step, the vacuum degree of the light component tower is-0.05 to-0.09 MPa, the tower top temperature of the light component tower is 50 to 90 ℃, and the tower kettle temperature of the light component tower is 90 to 130 ℃.
In the technical scheme, in the sixth step, the vacuum degree of the reduced pressure rectifying tower is-0.085-0.099 MPa, the tower top temperature of the reduced pressure rectifying tower is 85-110 ℃, and the tower kettle temperature of the reduced pressure rectifying tower is 105-135 ℃.
In the above technical solution, in the fourth step, the monomethylamine is returned to the metering tank of monomethylamine.
In the above technical scheme, in the fifth step, the intermediate directly and continuously enters the mixer.
The invention has the beneficial effects that:
(1) the invention respectively measures monomethylamine and propylene oxide, inputs the monomethylamine and the propylene oxide into a mixer, uniformly mixes the monomethylamine and the propylene oxide, then the monomethylamine and the propylene oxide enter a reactor for reaction, and then the obtained crude product containing the N-methyl isopropanolamine is separated and refined through an amine steaming tower, a light component tower and a reduced pressure rectification tower in sequence, thereby obtaining a refined product N-methyl isopropanolamine. The method adopts a continuous mode to separate and refine the N-methyl isopropanolamine, and fills the blank of high-efficiency batch production of the N-methyl isopropanolamine in the industry; in addition, the continuous production mode can continuously produce target products only by setting the parameters of each tower kettle, the parameters of the rectifying tower do not need to be continuously regulated and controlled manually, so that the manpower is saved, the stability during the production of equipment is improved, the quality and the yield of the products are improved, in addition, the reflux ratio of the tower is not required to be increased, the production energy consumption is greatly saved, and the reduction of the production cost is facilitated.
(2) The method for continuously producing the N-methyl isopropanolamine has the characteristics of simple operation method, low production cost and suitability for large-scale production.
Drawings
FIG. 1 is a flow diagram of a process for the continuous production of N-methyl isopropanolamine in accordance with the present invention.
Detailed Description
Example 1.
In this embodiment, a method for continuously producing N-methyl isopropanolamine is shown in fig. 1, and includes the following steps:
step one, feeding: respectively feeding propylene oxide and monomethylamine into a mixer through a metering pump, wherein the molar ratio of the propylene oxide to the monomethylamine is 1: 1.1;
step two, mixing: regulating the temperature of the mixer to be 10 ℃ and the pressure to be 3.5MPa, and mixing monomethylamine and propylene oxide in the mixer to obtain a uniformly mixed mixture;
step three, reaction: pumping the mixture obtained in the step two into a reactor, regulating the temperature of the reactor to be 110 ℃ and the pressure to be 3.5MPa, and enabling the mixture to fully react in the reactor for 5min to obtain a first crude product containing N-methyl isopropanolamine; wherein the reaction formula of the propylene oxide and the monomethylamine is as follows:
step four, removing monomethylamine: continuously feeding the first crude product obtained in the step three into the middle of an amine distilling tower, and then adjusting the pressure of the amine distilling tower to be 0.05-0.1 MPa, the tower top temperature of the amine distilling tower to be 80-90 ℃ and the tower kettle temperature to be 130-140 ℃, so that the monomethylamine which does not participate in the reaction is distilled out of the tower top, and a second crude product without the monomethylamine is obtained; wherein the monomethylamine is returned to a metering tank for monomethylamine;
step five, removing an intermediate: continuously feeding the second crude product obtained in the third step into the middle of a light component tower, regulating and controlling the vacuum degree of the light component tower to be-0.05 to-0.06 MPa, and regulating and controlling the tower top temperature of the light component tower to be 80 to 90 ℃ and the tower kettle temperature to be 120 to 130 ℃, so that the intermediate of the second crude product is distilled out of the top of the light component tower, and a third crude product without the intermediate is obtained;
and sixthly, distilling off the N-methyl isopropanolamine: continuously feeding the third crude product obtained in the fifth step into the middle of a vacuum rectification tower, then adjusting the vacuum degree of the vacuum rectification tower to be-0.085-0.09 MPa, adjusting the tower top temperature of the vacuum rectification tower to be 100-110 ℃ and the tower kettle temperature to be 125-135 ℃, and distilling N-methyl isopropanolamine from the top of the vacuum rectification tower to obtain a refined product N-methyl isopropanolamine; wherein the intermediate is passed directly into a mixer.
Example 2.
In this embodiment, a method for continuously producing N-methyl isopropanolamine is shown in fig. 1, and includes the following steps:
step one, feeding: respectively feeding propylene oxide and monomethylamine into a mixer by a metering pump, wherein the molar ratio of the propylene oxide to the monomethylamine is 1: 1.3;
step two, mixing: regulating the temperature of the mixer to be 30 ℃ and the pressure to be 5.0MPa, and mixing monomethylamine and propylene oxide in the mixer to obtain a uniformly mixed mixture;
step three, reaction: continuously feeding the mixture obtained in the step two into a reactor, regulating the temperature of the reactor to be 130 ℃ and the pressure to be 5.0MPa, and fully reacting the mixture in the reactor for 2min to obtain a first crude product containing N-methyl isopropanolamine; wherein the reaction formula of the propylene oxide and the monomethylamine is as follows:
step four, removing monomethylamine: continuously feeding the first crude product obtained in the step three into the middle of an amine distilling tower, and then adjusting the pressure of the amine distilling tower to be 0.07-0.4 MPa, the tower top temperature of the amine distilling tower to be 90-110 ℃ and the tower kettle temperature to be 148-160 ℃, so that the monomethylamine which does not participate in the reaction is distilled out of the tower top, and a second crude product without the monomethylamine is obtained; wherein, the monomethylamine returns to the metering tank of the monomethylamine;
step five, removing an intermediate: continuously feeding the second crude product obtained in the third step into the middle of a light component tower, regulating the vacuum degree of the light component tower to be-0.07 to-0.09 MPa, and regulating the tower top temperature of the light component tower to be 50-70 ℃ and the tower kettle temperature to be 90-110 ℃, so that the intermediate of the second crude product is distilled out of the top of the light component tower, and the tower kettle is a third crude product without the intermediate;
and sixthly, distilling off the N-methyl isopropanolamine: continuously feeding the third crude product obtained in the fifth step into the middle of a vacuum rectification tower, then adjusting the vacuum degree of the vacuum rectification tower to be-0.096-0.099 MPa, adjusting the tower top temperature of the vacuum rectification tower to be 85-100 ℃ and the tower kettle temperature to be 105-120 ℃, and distilling N-methyl isopropanolamine from the top of the vacuum rectification tower to obtain a refined product N-methyl isopropanolamine; wherein the intermediate is fed directly and continuously into the mixer.
Example 3.
In this embodiment, a method for continuously producing N-methyl isopropanolamine is shown in fig. 1, and includes the following steps:
step one, feeding: respectively feeding propylene oxide and monomethylamine into a mixer by a metering pump, wherein the molar ratio of the propylene oxide to the monomethylamine is 1: 1.2;
step two, mixing: regulating the temperature of the mixer to be 15 ℃ and the pressure to be 4.0MPa, and mixing monomethylamine and propylene oxide in the mixer to obtain a uniformly mixed mixture;
step three, reaction: continuously feeding the mixture obtained in the step two into a reactor, regulating the temperature of the reactor to be 120 ℃, and controlling the pressure to be 4.0MPa, and fully reacting the mixture in the reactor for 3.5min to obtain a first crude product containing N-methyl isopropanolamine; wherein the reaction formula of the propylene oxide and the monomethylamine is as follows:
step four, removing monomethylamine: continuously feeding the first crude product obtained in the step three into the middle of an amine distilling tower, and then adjusting the vacuum degree of the amine distilling tower to be 0.08-0.2 MPa, the tower top temperature of the amine distilling tower to be 80-110 ℃ and the tower kettle temperature to be 135-150 ℃, so that the monomethylamine which does not participate in the reaction is distilled out of the tower top, and a second crude product with the monomethylamine removed is obtained; wherein, the monomethylamine returns to the metering tank of the monomethylamine;
step five, removing an intermediate: continuously feeding the second crude product obtained in the third step into the middle of a light component tower, regulating and controlling the pressure of the light component tower to be-0.05 to-0.08 MPa, and regulating the tower top temperature of the light component tower to be 70 to 80 ℃ and the tower kettle temperature to be 110 to 120 ℃, so that the intermediate of the second crude product is distilled out of the top of the light component tower, and the tower kettle is a third crude product without the intermediate;
and sixthly, distilling off the N-methyl isopropanolamine: continuously feeding the third crude product obtained in the fifth step into the middle of a vacuum rectification tower, then adjusting the vacuum degree of the vacuum rectification tower to be-0.09-0.095 MPa, adjusting the tower top temperature of the vacuum rectification tower to be 95-105 ℃ and the tower kettle temperature to be 120-130 ℃, and distilling N-methyl isopropanolamine from the top of the vacuum rectification tower to obtain a refined product N-methyl isopropanolamine; wherein the intermediate is fed directly and continuously into the mixer.
The product quality index of the N-methyl isopropanolamine obtained by the method is shown in the table 1:
TABLE 1
| Product index | Quality standard |
| Appearance of the product | Colorless transparent liquid |
| The content is more than or equal to wt percent | 99.2 |
| The water content is less than or equal to wt% | 0.3 |
| Primary amine and secondary amine, less than or equal to weight percent | 0.5 |
| Chroma (Hazen unit, platinum-cobalt color number less than or equal to | 30 |
As can be seen from Table 1, the content of N-methyl isopropanolamine in the product prepared by the method is as high as 99.2%, and the sum of impurities such as water, primary amine, tertiary amine and the like is less than 0.8%.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the protection scope of the present invention, although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (1)
1. A method for continuously producing N-methyl isopropanolamine is characterized by comprising the following steps: the method comprises the following steps:
step one, feeding: respectively metering propylene oxide and monomethylamine, and continuously feeding into a mixer;
wherein the molar ratio of the propylene oxide to the monomethylamine is 1: 1.1 to 1.3;
step two, mixing: regulating the temperature and the pressure of the mixer, and mixing monomethylamine and propylene oxide in the mixer to obtain a uniformly mixed mixture;
step three, reaction: continuously feeding the mixture obtained in the step two into a reactor, regulating the temperature and pressure of the reactor, and reacting the mixture in the reactor to obtain a first crude product containing N-methyl isopropanolamine;
step four, removing monomethylamine: continuously feeding the first crude product obtained in the step three into the middle part of an amine distilling tower, and then adjusting the pressure of the amine distilling tower, the tower top temperature of the amine distilling tower and the tower bottom temperature to distill off the unreacted monomethylamine from the tower top, wherein the tower bottom is a second crude product for removing the monomethylamine;
step five, removing an intermediate: continuously feeding the second crude product obtained in the step three into the middle of a light component tower, and regulating and controlling the pressure of the light component tower, the tower top temperature of the light component tower and the tower kettle temperature, so that an intermediate of the second crude product is distilled out of the top of the light component tower, and the tower kettle is a third crude product from which the intermediate is removed;
and step six, rectifying an N-methyl isopropanolamine product: continuously feeding the third crude product obtained in the fifth step into the middle part of a reduced pressure rectifying tower, and then adjusting the pressure of the reduced pressure rectifying tower, the tower top temperature and the tower kettle temperature of the reduced pressure rectifying tower to distill the N-methyl isopropanolamine from the top part of the reduced pressure rectifying tower to obtain an N-methyl isopropanolamine refined product, wherein the tower kettle liquid is a byproduct;
in the second step, the temperature of the mixer is 10-30 ℃, and the pressure is 3.5-5.0 MPa;
in the third step, the temperature of the reactor is 110-130 ℃, and the pressure is 3.5-5.0 MPa;
in the third step, the reaction time of the mixture in the reactor is 2-5 min;
in the fourth step, the pressure of the amine steaming tower is 0.05-0.4 MPa, the tower top temperature of the amine steaming tower is 80-110 ℃, and the tower kettle temperature of the amine steaming tower is 130-160 ℃;
in the fifth step, the vacuum degree of the light component tower is-0.05 to-0.09 MPa, the tower top temperature of the light component tower is 50 to 90 ℃, and the tower kettle temperature of the light component tower is 90 to 130 ℃;
in the sixth step, the vacuum degree of the reduced pressure rectifying tower is-0.085-0.099 MPa, the tower top temperature of the reduced pressure rectifying tower is 85-110 ℃, and the tower kettle temperature of the reduced pressure rectifying tower is 105-135 ℃;
the propylene oxide and the monomethylamine continuously enter the mixer through a metering pump respectively;
in the fourth step, the monomethylamine returns to a metering tank of the monomethylamine;
in the fifth step, the intermediate directly and continuously enters a mixer.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101475494A (en) * | 2009-01-19 | 2009-07-08 | 抚顺佳化聚氨酯有限公司 | Production process of alkanolamine |
| CN101781219A (en) * | 2009-12-31 | 2010-07-21 | 茂名云龙工业发展有限公司 | Method for continuous production of N-methyldiethanolamine |
| CN101830812A (en) * | 2009-12-31 | 2010-09-15 | 茂名云龙工业发展有限公司 | Process for continuously producing N-monomethylethanolamine |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101475494A (en) * | 2009-01-19 | 2009-07-08 | 抚顺佳化聚氨酯有限公司 | Production process of alkanolamine |
| CN101781219A (en) * | 2009-12-31 | 2010-07-21 | 茂名云龙工业发展有限公司 | Method for continuous production of N-methyldiethanolamine |
| CN101830812A (en) * | 2009-12-31 | 2010-09-15 | 茂名云龙工业发展有限公司 | Process for continuously producing N-monomethylethanolamine |
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