CN115215757A - Preparation process of light-color lauroyl dimethyl propane diamine - Google Patents
Preparation process of light-color lauroyl dimethyl propane diamine Download PDFInfo
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- CN115215757A CN115215757A CN202210995650.9A CN202210995650A CN115215757A CN 115215757 A CN115215757 A CN 115215757A CN 202210995650 A CN202210995650 A CN 202210995650A CN 115215757 A CN115215757 A CN 115215757A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C231/00—Preparation of carboxylic acid amides
- C07C231/02—Preparation of carboxylic acid amides from carboxylic acids or from esters, anhydrides, or halides thereof by reaction with ammonia or amines
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C231/00—Preparation of carboxylic acid amides
- C07C231/22—Separation; Purification; Stabilisation; Use of additives
- C07C231/24—Separation; Purification
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a preparation process of light-colored lauroyl dimethyl propane diamine, which comprises the following steps of S1, adding lauric acid into a reaction kettle; s2, heating the reaction kettle to 60-80 ℃, and heating to dissolve lauric acid in the temperature range; s3, after dissolving for a set time, vacuumizing the reaction kettle; s4, filling inert gas into the reaction kettle; s5, adding dimethyl propane diamine into the reaction liquid in which the lauric acid is dissolved; carrying out secondary heating on the reaction kettle, and carrying out dehydration reaction under the high-temperature condition; s6, after the reaction is finished, vacuumizing the reaction kettle again to remove redundant amine; s7, cooling the reaction kettle to maintain the temperature of an inner cavity of the reaction kettle between 60 and 70 ℃, and filling inert gas into the reaction kettle to break the vacuum state; s8, carrying out secondary cooling treatment on the reaction kettle to obtain light-color lauroyl dimethyl propane diamine.
Description
Technical Field
The invention belongs to the technical field of compound preparation, and particularly relates to a preparation process of light-colored lauroyl dimethyl propane diamine.
Background
Lauric acid (also known as dodecanoic acid), a saturated fatty acid, has a molecular formula of C12H24O2. Although named as lauric acid, the lauric oil accounts for only 1 to 3 percent of the content of the lauric oil.
Dimethyl propylene diamine is a chemical substance, 2-Dimethyl-1,3-propane, and has a molecular formula of C5H14N2 and a molecular weight of 102.18.
Experimental observation shows that under the heating condition, the lauroyl dimethyl propane diamine is prepared from lauric acid and dimethyl propane diamine, the final product mostly presents a darker color, and if the lauroyl dimethyl propane diamine with the darker color is adopted to produce subsequent products, the subsequent products are also darker in color and cannot meet the requirement of the appearance color of the subsequent products, so that the preparation process of the light-color lauroyl dimethyl propane diamine is provided.
Disclosure of Invention
In view of the problems raised by the above background art, the present invention is directed to: aims at providing a preparation process of light-colored lauroyl dimethyl propane diamine.
In order to achieve the technical purpose, the technical scheme adopted by the invention is as follows:
a process for preparing light-colored lauroyl dimethyl propane diamine comprises the following steps,
s1, adding lauric acid into a reaction kettle;
s2, heating the reaction kettle to 60-80 ℃, and heating to dissolve lauric acid in the temperature range;
s3, after dissolving for a set time, vacuumizing the reaction kettle;
s4, filling inert gas into the reaction kettle;
s5, adding dimethyl propane diamine into the reaction liquid in which the lauric acid is dissolved; carrying out secondary heating on the reaction kettle, and carrying out dehydration reaction under the high-temperature condition;
s6, after the reaction is finished, vacuumizing the reaction kettle again to remove redundant amine;
s7, cooling the reaction kettle to maintain the temperature of the inner cavity of the reaction kettle between 60 and 70 ℃, and filling inert gas into the reaction kettle to break the vacuum state;
s8, carrying out secondary cooling treatment on the reaction kettle to obtain light-color lauroyl dimethyl propane diamine.
Further, in the S2, the specific heating dissolution temperature of the lauric acid is 70 ℃.
Further, in the S3 and the S6, the reaction kettle is pumped to a vacuum state at a negative pressure value of-0.1 MPa.
In a further limitation, in S4 and S7, the inert gas filled is nitrogen.
Further, in the step S5, the achievement of the high temperature condition is based on a steam backflow phenomenon.
Further, in the S5, the reaction time of the dehydration reaction is 5 to 8 hours.
In step S7, the temperature of the reaction kettle is decreased to 65 ℃.
Further limiting, in S3, the reaction kettle is vacuumized through the one-way valve, and due to the design, external air backflow is avoided and the external air enters the reaction kettle, particularly, air backflow caused by power failure or vacuum system pressure fluctuation and other factors is prevented, so that the product oxidation phenomenon can be reduced, and the product chromaticity is reduced.
Further limiting, in the S5, in the dehydration reaction process, the reaction kettle needs to be communicated with the outside air through a safety valve and an emptying pipe, the emptying pipe and the safety valve have the same caliber, and the pressure of the safety valve is set to be 0.01MPa.
The invention has the beneficial effects that:
1. through to the reation kettle evacuation, fill nitrogen gas again, got rid of the oxygen that originally exists in the reation kettle inner chamber, avoided oxygen and amine reaction, produce coloured material to after getting rid of unnecessary, unreacted amine, cool down and handle, acquire lauroyl dimethyl propylene diamine again, the lauroyl dimethyl propylene diamine who prepares the gained with this technology is the light color, has avoided follow-up product color to deepen, has satisfied the outward appearance colour requirement of follow-up product.
Detailed Description
In order that those skilled in the art can better understand the present invention, the following embodiments are provided to further illustrate the present invention.
Example I (while introducing nitrogen gas for protection, using gas to prevent backflow and convection structure), the preparation process of light-colored lauroyl dimethyl propane diamine comprises the following steps,
s1, adding lauric acid into a reaction kettle;
s2, heating the reaction kettle to 60-80 ℃, and heating to dissolve lauric acid in the temperature range;
s3, after dissolving for a set time, adopting a one-way valve to vacuumize the reaction kettle at a negative pressure value of-0.1 MPa;
s4, filling inert gas into the reaction kettle, wherein the filled inert gas is nitrogen;
s5, adding dimethyl propane diamine into the reaction liquid in which the lauric acid is dissolved; carrying out secondary heating on the reaction kettle until the steam backflow phenomenon is generated, carrying out dehydration reaction, wherein the reaction time is 5-8 hours, in the dehydration reaction process, the reaction kettle is communicated with the outside air through a safety valve and an emptying pipe, the diameter of the emptying pipe is the same as that of the safety valve, and the pressure of the safety valve is 0.01MPa;
s6, after the reaction is finished, vacuumizing the reaction kettle again at a negative pressure value of-0.1 MPa, and removing redundant amine in the reaction kettle;
s7, cooling the reaction kettle to maintain the temperature of the inner cavity of the reaction kettle between 60 and 70 ℃, and filling inert gas into the reaction kettle to break the vacuum state;
s8, carrying out secondary cooling treatment on the reaction kettle to obtain light-colored lauroyl dimethyl propane diamine;
in the reaction process, the deepening of the color of the lauroyl dimethyl propane diamine is mainly inhibited in three aspects, 1. The reaction kettle is vacuumized and filled with nitrogen, so that the air originally existing in the inner cavity of the reaction kettle is eliminated, and the air contains oxygen which can oxidize the amine in the preparation process to generate a colored substance, so that the color of the final product lauroyl dimethyl propane diamine is deepened; 2. after the dehydration reaction is finished, discharging redundant amine which does not participate in the reaction by vacuumizing, and avoiding the reaction of the amine and oxygen which is accidentally remained in the reaction kettle, or the reaction of the amine and oxygen which flows into the reaction kettle from the external environment after a subsequent reaction kettle is opened; 3. after removing redundant amine, carrying out certain cooling treatment, recharging nitrogen to maintain the pressure of the internal environment and the external environment to be consistent, and obtaining light-colored lauroyl dimethyl propane diamine after secondary cooling, wherein the oxidation of oxygen to amine is intensified due to the rise of temperature, if the vacuum environment is broken by using nitrogen, oxygen is accidentally mixed in, the amine is not exhausted, and the amine can be oxidized under the condition of no cooling, so that after secondary cooling, even if the vacuum is broken by using nitrogen, oxygen is accidentally mixed in, the amine is not exhausted, the condition of reaction between the amine and the oxygen is also lacked, and the color of the lauroyl dimethyl propane diamine is not deepened;
in the technology, the production of light-colored lauroyl dimethyl propane diamine is realized, the vacuumizing is very critical, when the reaction kettle is vacuumized through the evacuation pipe, the air backflow can be avoided by adopting the one-way valve, the safety valve with the safety pressure of 0.01MPa can be added on the evacuation pipe, and the phenomenon that the external air enters the reaction kettle in a convection mode in the reaction process is reduced;
the light-colored lauroyl dimethyl propane diamine I is prepared by the process, and the chromaticity detection is carried out on the light-colored lauroyl dimethyl propane diamine I, wherein the chromaticity detection value of platinum and cobalt is 8.
Example II (no gas backflow prevention, convection prevention structure, only nitrogen protection), the preparation process of light-colored lauroyl dimethyl propane diamine comprises the following steps,
s1, adding lauric acid into a reaction kettle;
s2, heating the reaction kettle to 60-80 ℃, and heating to dissolve lauric acid in the temperature range;
s3, directly vacuumizing the reaction kettle to vacuum at a negative pressure value of-0.1 MPa after dissolving for a set time;
s4, filling inert gas into the reaction kettle, wherein the filled inert gas is nitrogen;
s5, adding dimethyl propane diamine into the reaction liquid in which the lauric acid is dissolved; carrying out secondary heating on the reaction kettle until the steam reflux phenomenon is generated, and carrying out dehydration reaction for 5-8 hours;
s6, after the reaction is finished, vacuumizing the reaction kettle again at a negative pressure value of-0.1 MPa, and removing redundant amine in the reaction kettle;
s7, cooling the reaction kettle to maintain the temperature of the inner cavity of the reaction kettle between 60 and 70 ℃, and filling inert gas into the reaction kettle to break the vacuum state;
s8, carrying out secondary cooling treatment on the reaction kettle to obtain light-colored lauroyl dimethyl propane diamine;
the light-colored lauroyl dimethyl propane diamine II is prepared by the process, and the chromaticity detection is carried out on the light-colored lauroyl dimethyl propane diamine II, wherein the chromaticity detection value of platinum and cobalt is 18.
In comparative example I, on the basis of example II, the nitrogen protection process is further removed, light-colored lauroyl dimethyl propylene diamine III is prepared, and the chromaticity detection is carried out on the light-colored lauroyl dimethyl propylene diamine III, wherein the chromaticity detection value of platinum and cobalt is 105.
The platinum-cobalt color test values of the products of examples I, II and I are shown in Table 1:
TABLE 1 chromaticity detection Table
According to detection data, when nitrogen is introduced for protection, a gas backflow prevention and convection prevention structure (such as a one-way valve and a safety valve) is matched for use, so that the chromaticity of the lauroyl dimethyl propane diamine is obviously reduced, the deepening of the product color is avoided, and the requirement on the appearance color of subsequent products is met.
The foregoing embodiments are merely illustrative of the principles of the present invention and its efficacy, and are not to be construed as limiting the invention. Those skilled in the art can modify or change the above-described embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (9)
1. The preparation process of light-color lauroyl dimethyl propane diamine is characterized by comprising the following steps of: the preparation process comprises the following steps of,
s1, adding lauric acid into a reaction kettle;
s2, heating the reaction kettle to 60-80 ℃, and heating to dissolve lauric acid in the temperature range;
s3, after dissolving for a set time, vacuumizing the reaction kettle;
s4, filling inert gas into the reaction kettle;
s5, adding dimethyl propane diamine into the reaction liquid in which the lauric acid is dissolved; carrying out secondary heating on the reaction kettle, and carrying out dehydration reaction under the high-temperature condition;
s6, after the reaction is finished, vacuumizing the reaction kettle again to remove redundant amine;
s7, cooling the reaction kettle to maintain the temperature of the inner cavity of the reaction kettle between 60 and 70 ℃, and filling inert gas into the reaction kettle to break the vacuum state;
s8, carrying out secondary cooling treatment on the reaction kettle to obtain light-color lauroyl dimethyl propane diamine.
2. The process of claim 1 for preparing light-colored lauroyl dimethyl propane diamine, wherein: in the S2, the specific heating and dissolving temperature of the lauric acid is 70 ℃.
3. The process of claim 2, wherein the process comprises the steps of: in the S3 and the S6, the reaction kettle is pumped to a vacuum state at a negative pressure value of-0.1 MPa.
4. A process according to claim 3 for the preparation of light-colored lauroyl dimethyl propane diamine, wherein: and in the S4 and the S7, the inert gas is filled with nitrogen.
5. The process of claim 4, wherein the reaction is carried out in the presence of a catalyst selected from the group consisting of: and in the S5, the standard of reaching the high-temperature condition is the phenomenon of generating water vapor backflow.
6. The process of claim 5, wherein the process comprises the steps of: in the S5, the reaction time of the dehydration reaction is 5 to 8 hours.
7. The process of claim 6, wherein the reaction is carried out in the presence of a catalyst selected from the group consisting of: and in the S7, reducing the temperature to 65 ℃ by cooling treatment.
8. The process of claim 1 for the preparation of light-colored lauroyl dimethyl propane diamine, wherein: and in the S3, the reaction kettle is vacuumized through a one-way valve.
9. The process of claim 1 for the preparation of light-colored lauroyl dimethyl propane diamine, wherein: in the S5, in the dehydration reaction process, the reaction kettle is communicated with the outside air through a safety valve and an emptying pipe, the diameter of the emptying pipe is the same as that of the safety valve, and the pressure of the safety valve is 0.01MPa.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210995650.9A CN115215757A (en) | 2022-08-18 | 2022-08-18 | Preparation process of light-color lauroyl dimethyl propane diamine |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070060762A1 (en) * | 2003-10-06 | 2007-03-15 | Akiko Kawashima | Production process for carboxylic amide and derivatives thereof |
| JP2009155739A (en) * | 2007-12-25 | 2009-07-16 | Lion Corp | Liquid softener composition |
| CN103483215A (en) * | 2013-09-30 | 2014-01-01 | 南京威尔生物化学有限公司 | Green production technology of lauramidopropyl dimethylamine |
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- 2022-08-18 CN CN202210995650.9A patent/CN115215757A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070060762A1 (en) * | 2003-10-06 | 2007-03-15 | Akiko Kawashima | Production process for carboxylic amide and derivatives thereof |
| JP2009155739A (en) * | 2007-12-25 | 2009-07-16 | Lion Corp | Liquid softener composition |
| CN103483215A (en) * | 2013-09-30 | 2014-01-01 | 南京威尔生物化学有限公司 | Green production technology of lauramidopropyl dimethylamine |
Non-Patent Citations (1)
| Title |
|---|
| 方奕文等: "N，N-二甲基-N’-月桂酰基-1，3-丙二胺的合成", 精细化工, vol. 18, no. 8, pages 438 - 439 * |
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