阅读说明：本技术 一种n-十二烷基-2-吡咯烷酮的生产工艺 (Production process of N-dodecyl-2-pyrrolidone ) 是由 何永矩 王春友 于 2020-03-31 设计创作，主要内容包括：本发明公开了一种N-十二烷基-2-吡咯烷酮生产工艺,步骤如下：S01:原料Y-丁内酯和十二烷基伯胺通过预热器先预热50-80℃；S02:将原料经计量泵按原料摩尔比例1.0～1.4：1泵入管道反应器内连续反应；S03:通过调节加热介质的温度控制管道反应器内物料温度230-270℃；S04:通过管道反应器出口调节阀自动调节压力4.0-7.0MPA；S05:调节阀出来的合成液直接进入闪蒸塔去除轻组分和大部分水；S06:塔底粗品经过减压蒸馏的方式,降低蒸馏温度,提高效率,最终能得到含量99.5％以上的纯度。本发明设备投资和安全要求低,节省操作时间和能耗,可实现自动控制,避免副反应发生,产量高质量稳定。(The invention discloses a production process of N-dodecyl-2-pyrrolidone, which comprises the following steps: s01, preheating raw materials of Y-butyrolactone and dodecyl primary amine by a preheater to 50-80 ℃; s02, the raw materials are mixed by a metering pump according to the raw material molar ratio of 1.0-1.4: 1 pumping into a pipeline reactor for continuous reaction; s03, controlling the material temperature in the pipeline reactor 230-270 ℃ by adjusting the temperature of the heating medium; s04, automatically adjusting the pressure to 4.0-7.0MPA through an outlet adjusting valve of the pipeline reactor; s05, directly feeding the synthetic liquid from the regulating valve into a flash tower to remove light components and most of water; s06, the crude product at the bottom of the tower is subjected to reduced pressure distillation to reduce the distillation temperature and improve the efficiency, and the purity of the crude product with the content of more than 99.5 percent can be finally obtained. The invention has low equipment investment and safety requirements, saves operation time and energy consumption, can realize automatic control, avoids side reaction and has high yield and stable quality.)

1. a production process of N-dodecyl-2-pyrrolidone is characterized in that: which comprises the following steps:

s01, preheating raw materials of dodecyl primary amine and Y-butyrolactone by a preheater to 50-80 ℃;

s02, the raw materials are mixed by a metering pump according to the raw material molar ratio of 1.0-1.4: 1 pumping into a pipeline reactor for continuous reaction;

s03, controlling the material temperature in the pipeline reactor at 230-275 ℃ by adjusting the temperature of the heating medium;

s04, automatically adjusting the pressure to 4.0-7.0MPA through an outlet adjusting valve of the pipeline reactor;

s05, directly feeding the synthetic liquid from the regulating valve into a flash tower to remove light components and most of water;

s06, the crude product at the bottom of the tower is subjected to reduced pressure distillation to reduce the distillation temperature and improve the efficiency, and the purity of the crude product with the content of more than 99.5 percent can be finally obtained.

2. The process according to claim 1 for the production of N-dodecyl-2-pyrrolidone, wherein: in step S01, the raw material is preheated to 60 +/-2 ℃.

3. The process according to claim 1 for the production of N-dodecyl-2-pyrrolidone, wherein: the molar ratio of the raw materials in the step S02 is 1.1 +/-0.1: 1.

4. the process according to claim 1 for the production of N-dodecyl-2-pyrrolidone, wherein: the residence time of the material in step S02 in the tubular reactor is 2-4 hours.

5. The process according to claim 1 for the production of N-dodecyl-2-pyrrolidone, wherein: the temperature of the materials in the pipeline reactor in the step S03 is 250-270 ℃.

6. The process according to claim 1 for the production of N-dodecyl-2-pyrrolidone, wherein: in step S04, the pressure of the pipeline reactor is regulated by a pipeline reactor outlet regulating valve to 5.0-6.5MPA, so as to ensure the full reaction of the materials.

7. The process according to claim 1 for the production of N-dodecyl-2-pyrrolidone, wherein: the temperature of the top of the flash tower in the step S05 is controlled between 90 ℃ and 98 ℃.

8. The process according to claim 1 for the production of N-dodecyl-2-pyrrolidone, wherein: the operating pressure of the distillation column in the step S06 is-0.09 to-0.1 MPA.

9. The process according to claim 1 for the production of N-dodecyl-2-pyrrolidone, wherein: the column top operating temperature of the distillation column in step S06 was 180-220 ℃.

Technical Field

The invention belongs to the field of fine chemicals and preparation methods thereof, and particularly relates to a production process of N-dodecyl-2-pyrrolidone.

Background

The N-dodecyl-2-pyrrolidone is an environment-friendly thickening and emulsifying agent, and is widely applied to the fields of industrial chemicals, raw materials for chemical synthesis, electronics, agricultural chemicals, daily chemical products and the like.

The process route of the N-dodecyl-2-pyrrolidone generally adopts batch reaction, which causes the defects of long reaction time, high equipment investment and safety requirements, high energy consumption, low yield and the like.

Therefore, it is necessary to provide a novel and efficient process for synthesizing N-dodecyl-2-pyrrolidone.

Disclosure of Invention

The invention aims to solve the problems in the prior art and provide a production process of N-dodecyl-2-pyrrolidone.

The purpose of the invention can be realized by the following technical scheme: a continuous reaction production process of N-dodecyl-2-pyrrolidone is characterized by comprising the following steps:

s01, preheating raw materials of dodecyl primary amine and Y-butyrolactone by a preheater to 50-80 ℃;

s02, pumping the raw materials into a pipeline reactor through a metering pump according to the molar ratio of the raw materials for continuous reaction;

s03, controlling the material temperature in the pipeline reactor 230-270 ℃ by adjusting the temperature of the heating medium;

s04, automatically adjusting the pressure to 4.0-7.0MPA through an outlet adjusting valve of the pipeline reactor;

s05, directly feeding the synthetic liquid from the regulating valve into a flash tower to remove light components and most of water;

s06, the crude product at the bottom of the tower is subjected to reduced pressure distillation to reduce the distillation temperature and improve the efficiency, and the purity of the crude product with the content of more than 99.5 percent can be finally obtained.

Preferably, the material in step S01 is preheated to 60 ± 2 ℃.

Preferably, the molar ratio of the raw materials in the step S02 is 1.1 +/-0.1: 1.

preferably, the material residence time in step S02 is 2-4 hours.

Preferably, the material temperature in step S03 is 250-270 ℃.

Preferably, the regulator valve in step S04 regulates the pressure in the range of 5.0-6.5 MPA.

Preferably, the flash column top temperature in step S05 is controlled between 90-98 ℃.

Preferably, the operating pressure of the distillation column in step S06 is-0.096 to-0.1 MPA.

Preferably, the column top operating temperature of the distillation column in step S06 is 185-215 ℃.

The working raw materials of the invention are as follows: the chemical reaction formula of the invention is as follows,

。

compared with the prior art, the invention has the following advantages:

the invention has the advantages of simple equipment, small reactor capacity, simple and convenient operation, and avoids the defects of high investment, large occupied area, high safety requirement and the like of an intermittent reactor.

The pipeline reactor adopted by the invention can continuously feed and discharge materials, and avoids the auxiliary operation time of feeding materials, adjusting the temperature and pressure of operation, discharging materials, preparing the next batch of feeding materials and the like in intermittent operation.

The invention can realize automatic control, and the metering pump, the pipeline reactor, the outlet regulating valve and the instrument can realize automatic control of continuous feeding and discharging, ensure relatively stable temperature and pressure, ensure stable yield and quality, and avoid the defects of difficult and expensive automatic control of intermittent operation, and the like.

The pipeline reactor adopted by the invention depends on the circulation of the materials as a heat transfer agent, the reaction heat can be timely led out, the concentration of reactants is relatively reduced, and the defect that the intermittent reaction heat can not be transferred so as to increase the probability of side reaction is avoided.

The yield is high and the quality is stable, the primary yield of the finished product of the N-dodecyl-2-pyrrolidone purified by a rectifying tower for producing a crude product by a pipeline reactor adopted by the invention can reach 80 percent, the purity is 99.5 percent, the primary yield of the finished product of the batch reaction is only 65 percent, and the purity is 98 percent.

Drawings

FIG. 1 is a diagram showing a purity chart of an N-dodecyl-2-pyrrolidone product obtained in example 1 of the present invention.

Detailed Description

The following are specific examples of the present invention and further describe the technical solutions of the present invention, but the present invention is not limited to these examples.

Example 1

Raw materials: raw materials of 1920KG dodecyl primary amine and 940KG Y-butyrolactone;

firstly, preheating the raw materials to 60 ℃;

the metering pump pumps the feed into the pipeline reactor at 150L/H (volume 330L);

adjusting a heating medium and an outlet adjusting valve of the pipeline reactor to ensure that the pressure in the pipeline is 5.4MPA and the temperature is 255 ℃;

maintaining the temperature at the top of the flash tower to be 95 ℃;

maintaining the operation pressure of the distillation tower to be 0.098MPA and the operation temperature force of the tower top to be 200 ℃;

the obtained product 2100KG of N-dodecyl-2-pyrrolidone has the purity of 99.6 percent.

The specific embodiments described herein are merely illustrative of the spirit of the invention. Various modifications or additions may be made to the described embodiments or alternatives may be employed by those skilled in the art without departing from the spirit or scope of the invention as defined in the appended claims.

The report obtained by combining example 1 and FIG. 1 is as follows: