Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Method for synthesizing diethylhydroxylamine

A technology of diethylhydroxylamine and triethylamine, applied in chemical instruments and methods, organic compound/hydride/coordination complex catalysts, organic chemistry, etc., can solve the problem of low total yield, many reaction steps, and large amounts of ethylene etc. to achieve the effect of high yield, high selectivity and high activity

Active Publication Date: 2018-12-28
NANJING UNIV OF TECH
View PDF3 Cites 4 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, most manufacturers at home and abroad mainly use the oxidative cracking method of triethylamine to produce N,N-diethylhydroxylamine, but the method of preparing N,N-diethylhydroxylamine through oxidation, dehydration and cracking of triethylamine and hydrogen peroxide obviously exists There are many reaction steps, complex production process, low overall yield, low product purity and difficulty in completely removing the moisture contained in the product. There are certain security risks

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) Catalyst preparation of Amberlyst-15 immobilized phosphotungstic acid:

[0028] Firstly, Amberlyst-15 was submerged in ethanol solution, stirred at room temperature for 3 hours, and then dried at 40°C until it was ready for use. Phosphotungstic acid (H 3 PW 12 o 40 ·XH 2 O) Add the aqueous solution to 50.0g of treated Amberlyst-15, stir at room temperature for 6h, wash with water to neutral after stirring, and dry at 40°C to constant weight to obtain 58.4g of Amberlyst-15 immobilized phosphotungstic acid catalyst (immobilized amount 14.25%).

[0029] (2) preparation of diethylhydroxylamine:

[0030] Take 9.5g Amberlyst-15 immobilized phosphotungstic acid catalyst and load it into a fixed bed reactor, and keep the catalyst bed at 60°C. 101.2g (1.00mol) of triethylamine (DEA) and 200g (11.11mol) of water, 60.06g (1.00mol) of glacial acetic acid (HOAc) and 113.36g (1.00mol) of 30% hydrogen peroxide mixture were injected into the reaction at a constant rate After...

Embodiment 2

[0032] (1) Catalyst preparation of Amberlyst-15 immobilized phosphotungstic acid:

[0033] Firstly, Amberlyst-15 was submerged in ethanol solution, stirred at room temperature for 4 hours, and then dried at 40°C until it was ready for use. Phosphotungstic acid (H 3 PW 12 o 40 ·XH 2 O) Add the aqueous solution to 50.0g of treated Amberlyst-15, stir at room temperature for 4h, wash with water to neutral after stirring, and dry at 40°C to constant weight to obtain 61.41g of Amberlyst-15 immobilized phosphotungstic acid catalyst (immobilized amount 18.57%).

[0034] (2) preparation of diethylhydroxylamine:

[0035] Take 49g of Amberlyst-15 immobilized phosphotungstic acid catalyst and load it into a fixed bed reactor, and keep the catalyst bed at 50°C. A mixture of 101.2g (1.00mol) triethylamine (DEA) and 200g (11.11mol) of water, 66.06g (1.1mol) of glacial acetic acid (HOAc) and 124.7g (1.1mol) of 30% hydrogen peroxide was injected at a constant speed After staying in the ...

Embodiment 3

[0037] (1) Catalyst preparation of Amberlyst-15 immobilized phosphotungstic acid:

[0038] Firstly, Amberlyst-15 was submerged in ethanol solution, stirred at room temperature for 4 hours, and then dried at 40°C until it was ready for use. Phosphotungstic acid (H 3 PW 12 o 40 ·XH 2 O) Add the aqueous solution to 50.0g of treated Amberlyst-15, stir at room temperature for 4h, wash with water to neutrality after stirring, and dry at 40°C to constant weight to obtain 64.57g of Amberlyst-15 immobilized phosphotungstic acid catalyst (immobilized amount 22.57%).

[0039] (2) preparation of diethylhydroxylamine:

[0040] Take 20g of Amberlyst-15 immobilized phosphotungstic acid catalyst and load it into a fixed bed reactor, and keep the catalyst bed at 40°C. 101.2g (1.00mol) of triethylamine (DEA) and 100g (11.11mol) of water, 90.08g (1.5mol) of glacial acetic acid (HOAc) and 113.36g (1.0mol) of 30% hydrogen peroxide mixture were injected into the reaction at a constant rate A...

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
boiling pointaaaaaaaaaa
flash pointaaaaaaaaaa
refractive indexaaaaaaaaaa
Login to View More

Abstract

The invention discloses a method for synthesizing diethylhydroxylamine. The method comprises steps as follows: (1), a solid acid catalyst supported with heteropoly acid is added to a fixed bed reactor, and the temperature of the fixed bed reactor is controlled to be 40-60 DEG C; (2), a mixed aqueous solution of triethylamine, acetic acid and hydrogen peroxide is injected into the fixed bed reactor, and the mixed aqueous solution stays in the fixed bed reactor for 2-24 h; (3), a product obtained from an outlet of the fixed bed reactor enters a cracking reaction kettle and is cracked, and diethylhydroxylamine is obtained; the temperature of the cracking reaction kettle is 100-120 DEG C, and the pressure is 600-700 mmHg. With the adoption of the method, potential safety hazard in a productionprocess can be reduced, and product purity is higher; the method is one new method which is capable of meeting the industrial demand of diethylhydroxylamine and quite high in practicability.

Description

technical field [0001] The invention belongs to the field of chemical industry and relates to a production process for preparing diethylhydroxylamine. Background technique [0002] The pure product of N,N-diethylhydroxylamine (DEHA) is a colorless transparent liquid, and the industrial product is a light yellow transparent liquid. The relative density is 1.867 (0-20°C), the melting point is -25°C, the boiling point is 125-130°C, the flash point is 45°C, and the refractive index is 1.4195 (20°C). DEHA is a new type of high-efficiency polymerization inhibitor. It has high polymerization inhibition efficiency and is not affected by temperature changes. It not only has high polymerization inhibition efficiency in the liquid phase of the monomer, but also in the gas phase. It has good polymerization inhibition performance; moreover, DEHA itself is non-toxic, has no pollution to the product, has high solubility in the monomer, and is easy to remove from the monomer, so it is conv...

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 Applications(China)
IPC IPC(8): C07C239/10B01J31/10B01J27/188
CPCC07C239/10B01J27/188B01J31/10
Inventor 余定华王文娟
Owner NANJING UNIV OF TECH
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com