Unlock instant, AI-driven research and patent intelligence for your innovation.

A kind of method utilizing 1,4-butanediol to prepare n-methylpyrrolidone

A technology of methylpyrrolidone and butanediol, which is applied in the direction of chemical instruments and methods, physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, etc., can solve the problem of long reaction time, low selectivity, conversion Low efficiency and other problems, to achieve good synergy, increase the active site, improve the effect of selectivity

Active Publication Date: 2022-03-25
安徽晟捷新能源科技股份有限公司
View PDF6 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, the catalyzer adopted in the 1,4-butanediol dehydrogenation-amination method still has problems such as low selectivity and low conversion rate, as reported by Chinese patent CN102029156B, which adopts an oxide catalyst containing Cu, Zr and Ce In the presence of 1,4-butanediol reaction to obtain gamma-butyrolactone, there are long reaction time in this method, low selectivity of gamma-butyrolactone, low yield and other problems
As used in CN11077317A, the catalyst has the following general formula: M1aM2bM3cOx, wherein M1 is Cu, M2 is at least one element selected from Al and Si, and M3 is at least one element selected from Na, Mg, Ce, Cr, Mn and Zn An element, but it has problems such as low conversion rate of 1,4-butanediol, low selectivity of γ-butyrolactone, low yield, etc., and it also needs to be prepared under high pressure, which requires high equipment requirements
[0005] Therefore, there are still relatively large defects in solid catalysts at present. Solid catalysts still have the problems of low conversion rate of raw material 1,4-butanediol and low selectivity of product γ-butyrolactone, and the requirements for equipment are relatively high under high pressure. high

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • A kind of method utilizing 1,4-butanediol to prepare n-methylpyrrolidone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Embodiment 1: a kind of method utilizing 1,4-butanediol to prepare N-methylpyrrolidone, concrete steps are as follows:

[0029] Step 1, preparation of Sm, Yb co-doped porous three-dimensional flower-shaped CuO catalyst: take 0.1mol copper acetate, 4mmol samarium nitrate, 3mmol ytterbium nitrate and add glycerol, methanol and water mixed solvent 2L (glycerol, methanol and water The volume ratio of 1:1:2), add 0.4mol urea, carry out magnetic stirring for 10min, then add 0.4mol of sodium dodecylbenzenesulfonate, continue magnetic stirring for 10min, and then transfer to the lined with polytetrafluoroethylene Carry out solvothermal reaction in a high-pressure reactor, seal it, control the pressure of the reactor to 1.5MPa, keep it at 200°C for 8 hours, take it out after cooling to room temperature, filter, wash, and dry to obtain Sm, Yb co-doped porous three-dimensional flower shape CuO catalyst. The doping ratio of Sm in the obtained Sm, Yb co-doped porous three-dimension...

Embodiment 2

[0033] Embodiment 2: a kind of method utilizing 1,4-butanediol to prepare N-methylpyrrolidone, concrete steps are as follows:

[0034] Step 1, preparation of Sm, Yb co-doped porous three-dimensional flower-shaped CuO catalyst: Take 0.1mol copper acetate, 3mmol samarium nitrate, 4mmol ytterbium nitrate and add glycerol, methanol and water mixed solvent 2L (glycerol, methanol and water The volume ratio is 1:1:2), add 0.5mol urea, carry out magnetic stirring for 20min, then add 0.5mol sodium dodecylbenzenesulfonate, continue magnetic stirring for 5min, and then transfer to the lined with polytetrafluoroethylene Carry out solvothermal reaction in a high-pressure reactor, seal it, control the pressure of the reactor to 1.3MPa, keep it at 180°C for 10 hours, take it out after cooling to room temperature, filter, wash, and dry to obtain Sm, Yb co-doped porous three-dimensional flower shape CuO catalyst. The doping ratio of Sm in the obtained Sm, Yb co-doped porous three-dimensional ...

Embodiment 3

[0038] Embodiment 3: a kind of method utilizing 1,4-butanediol to prepare N-methylpyrrolidone, concrete steps are as follows:

[0039] Step 1, preparation of Sm, Yb co-doped porous three-dimensional flower-shaped CuO catalyst: take 0.1mol copper acetate, 5mmol samarium nitrate, 2mmol ytterbium nitrate and add glycerol, methanol and water mixed solvent 2L (glycerol, methanol and water The volume ratio is 1:1:2), add 0.6mol urea, carry out magnetic stirring for 15min, then add 0.5mol sodium dodecylbenzenesulfonate, continue magnetic stirring for 8min, and then transfer to the lined with polytetrafluoroethylene Carry out solvothermal reaction in a high-pressure reactor, seal it, control the pressure of the reactor to 1.8MPa, keep it at 220°C for 5 hours, take it out after cooling to room temperature, filter, wash and dry to obtain Sm, Yb co-doped porous three-dimensional flower shape CuO catalyst. The doping ratio of Sm in the obtained Sm, Yb co-doped porous three-dimensional fl...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
particle sizeaaaaaaaaaa
specific surface areaaaaaaaaaaa
specific surface areaaaaaaaaaaa
Login to View More

Abstract

The invention relates to a method for preparing N-methylpyrrolidone, in particular to a method for preparing N-methylpyrrolidone by using 1,4-butanediol. The present invention first prepares Sm, Yb co-doped porous three-dimensional flower-shaped CuO catalyst, due to the special structure of the catalyst and the synergistic effect of Sm, Yb co-doping, it is guaranteed that the catalyst can be used to prepare γ- from 1,4-butanediol When using butyrolactone, in a short time under normal pressure, 1,4-butanediol has a higher conversion rate and γ-butyrolactone has a higher selectivity, thereby ensuring the production of γ-butyrolactone When using γ-butyrolactone, only simple rectification can be used for the preparation of N-methylpyrrolidone. When γ-butyrolactone is used to prepare N-methylpyrrolidone, due to ultrasonic cavitation and mediation Porous silica supported Zn / Mn / Cu composite catalyst works together to ensure the conversion rate of γ-butyrolactone and the selectivity of N-methylpyrrolidone, and then prepare N-methylpyrrolidone with high purity and high yield.

Description

technical field [0001] The invention relates to a synthesis method of N-methylpyrrolidone, in particular to a method for directly preparing high-purity N-methylpyrrolidone by dehydrogenating 1,4-butanediol to generate intermediate product γ-butyrolactone without purification . Background technique [0002] N-Methylpyrrolidone (NMP for short), belongs to nitrogen heterocyclic compound, molecular formula is C5H9NO, boiling point is 204°C, flash point is 95°C, it is a liquid with slight ammonia odor, miscible with water in any proportion, almost compatible with all solvents ( Alcohol, acetaldehyde, ketone, aromatic hydrocarbon, etc.) mixed completely. NMP is a polar aprotic solvent with high boiling point, strong polarity, low viscosity, strong solvency, no corrosion, low toxicity, strong biodegradability, low volatility, excellent chemical stability and thermal stability. It is mainly used in many industries such as petrochemical industry, plastic industry, pharmaceuticals, ...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): C07D207/267B01J23/83B01J23/889B01J35/10
CPCC07D207/267B01J23/83B01J23/002B01J35/0013B01J35/1019B01J23/8892B01J35/1061B01J2523/00B01J2523/17B01J2523/3737B01J2523/3787B01J2523/27B01J2523/41B01J2523/72
Inventor 王亚赵建勇刘龙波
Owner 安徽晟捷新能源科技股份有限公司