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Method for synthesizing diethylhydroxylamine from peracetic acid

A technology of diethylhydroxylamine and peracetic acid, applied in chemical instruments and methods, chemical/physical processes, physical/chemical process catalysts, etc., can solve the problems of high production cost, low product purity, and low product purity, etc. High activity and high selectivity

Active Publication Date: 2018-12-28
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Oxidation of diethylamine to prepare diethylhydroxylamine is complicated, the product purity is not high and the production cost is high
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 Disadvantages of low product purity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Catalyst preparation of Amberlyst-15 immobilized phosphotungstic acid:

[0031] 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 6.0g of treated Amberlyst-15, stir at room temperature for 4h, wash with water until neutral after stirring, steam the water under negative pressure, dry at 40°C to constant weight, and obtain Amberlyst-15 immobilized phosphotungstic acid catalyst 7.43g (solid loading 19.25%).

[0032] Preparation of triethylamine oxide:

[0033] 50.6g (0.50mol) triethylamine (DEA) and 100g aqueous solution are mixed in there-necked flask, add 30.03g (0.50mol) glacial acetic acid (HOAc) and the catalyst of 0.1gAmberlyst-15 immobilized heteropoly acid after processing, Keep the temperature in the water bath to 50°C, add 56.68g (0.50mol) of 30% hydrogen peroxide dropwise within 90 minu...

Embodiment 2

[0036] Catalyst preparation of Amberlyst-15 immobilized phosphotungstic acid:

[0037] 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 6.0g of treated Amberlyst-15, stir at room temperature for 4h, wash with water until neutral after stirring, steam the water under negative pressure, dry at 40°C to constant weight, and obtain Amberlyst-15 immobilized phosphotungstic acid catalyst 7.85g (solid loading 23.57%).

[0038] Preparation of triethylamine oxide:

[0039] 50.6g (0.50mol) triethylamine (DEA) and 100g aqueous solution are mixed in there-necked flask, add 33.03g (0.55mol) glacial acetic acid (HOAc) and the catalyst of 0.51gAmberlyst-15 immobilized heteropoly acid after processing, Constant temperature in water bath to 50°C, add 62.35g (0.55mol) 30% hydrogen peroxide dropwise within 90 minutes, a...

Embodiment 3

[0042] Catalyst preparation of Amberlyst-15 immobilized phosphotungstic acid:

[0043] 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 6.0g of treated Amberlyst-15, stir at room temperature for 4h, wash with water until neutral after stirring, steam the water under negative pressure, dry at 40°C to constant weight, and obtain Amberlyst-15 immobilized phosphotungstic acid catalyst 8.64g (solid loading 30.56%).

[0044] Preparation of triethylamine oxide:

[0045] 50.6g (0.50mol) triethylamine (DEA) and 100g aqueous solution are stirred and mixed in the there-necked flask, add 45.04g (0.75mol) glacial acetic acid (HOAc) and the catalyzer of the 0.4gAmberlyst-15 immobilized heteropolyacid after processing, Keep the temperature in the water bath to 50°C, add 56.68g (0.50mol) of 30% hydrogen peroxide dro...

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Abstract

The invention discloses a method for synthesizing diethylhydroxylamine from peracetic acid. The method comprises the following steps: (1) a mixed aqueous solution containing a heteropolyacid supportedsolid acid catalyst, triethylamine, acetic acid and hydrogen peroxide is subjected to a reaction at 35-70 DEG C for 3-16 h, then hydrogen peroxide and peracetic acid which are not reacted completelyare removed, and oxidized triethylamine is obtained by distillation; (2) oxidized triethylamine is subjected to reduced-pressure distillation at 50-80 DEG C under inert gas protection, temperature isincreased to 80-150 DEG C for pyrolysis when distillate is obviously reduced, and diethylhydroxylamine is obtained. Compared with a traditional hydrogen peroxide oxidizing agent, peracetic acid is taken as an oxidizing agent, selectivity of the product diethylhydroxylamine is high, and the heteropolyacid supported catalyst is high in activity and selectivity and recyclable.

Description

technical field [0001] The invention belongs to the field of chemical industry and relates to a method for synthesizing diethylhydroxylamine with peracetic acid. Background technique [0002] N,N-diethylhydroxylamine (DEHA), molecular formula (C 2 h 5 ) 2 NOH, the pure product is a colorless transparent liquid, 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 itself is non-toxic, non-polluting to products, has high solubility in monomers, and is easy to remove from monomers, which makes it easy to use. DEHA is a medium-strength organic reducing agent, belonging to disubstituted hydroxylamine compounds, because of its high efficiency, low toxicity, no corrosion, easy separation, etc., and has high polymerization inhibition performance in both gas and liquid phases, and The polymerization ...

Claims

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Application Information

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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
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