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Synthesis of 1, 4-oxygen nitrogen heterocyclic hexane catalyst by ammonification of diethylene glycol and process thereof

A technology for oxazepine and diethylene glycol ammonia, which is applied in the field of diethylene glycol amination preparation, can solve the problems of high cost, complicated preparation process and the like, and achieves a technology with low production cost, good selectivity and high activity. Effect

Inactive Publication Date: 2005-01-26
CNPC JILIN CHEM GROUP CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to overcome the existing diethylene glycol ammoniation morpholine catalyst, which has high cost and complicated preparation process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 1. Carrier pre-baking:

[0024] Weigh 70g clover-type φ1.5mmγ-Al 2 o 3 , pre-calcined at 800° C. for 4 hours, and naturally cooled to room temperature to obtain a pre-calcined carrier.

[0025] 2. Impregnated active components:

[0026] Weigh 110g of copper nitrate trihydrate, 78g of nickel nitrate hexahydrate, 1.6g of cobalt nitrate hexahydrate, and add them to 120ml of water to dissolve, and circulate the prepared solution to impregnate the pre-calcined carrier obtained in 1. The solution is pumped into the dipping kettle, soaked at 40°C for 10 minutes, and released, then pumped into the dipping kettle, and soaked in circulation for 24 hours. After filtration, it was dried at 60°C for 2 hours, then dried at 120°C for 8 hours, and finally calcined at 450°C for 4 hours, and cooled to room temperature naturally to obtain the required catalyst. The chemical composition of the catalyst was analyzed in Table 1.

[0027] 3. Catalyst evaluation and application:

[0028] ...

Embodiment 2

[0030] 1. Carrier pre-baking:

[0031] Weigh 70g clover-type φ1.5mmγ-Al 2 o 3 , pre-calcined at 800° C. for 4 hours, and naturally cooled to room temperature to obtain a pre-calcined carrier.

[0032] 2. Impregnated active components:

[0033] Weigh 100g of copper nitrate trihydrate, 110g of nickel nitrate hexahydrate, 34.0g of cobalt nitrate hexahydrate, and add them to 90ml of water to dissolve them, and use the prepared solution to circulate and impregnate the pre-calcined carrier obtained from 1 at 50°C for 12 hours , the dipping process is the same as in Example 1. After filtering, dry at 60°C for 2 hours, then dry at 120°C for 4 hours, and finally bake at 500°C for 4 hours, and cool down to room temperature naturally to obtain the required catalyst. The chemical composition of the catalyst is shown in Table 1.

[0034] 3. Catalyst evaluation and application:

[0035] Take the required amount of the catalyst prepared as above, put it into a 100ml fixed-bed reactor, p...

Embodiment 3

[0037] 1. Carrier pre-baking:

[0038] Weigh 70g clover-type φ1.5mmγ-Al 2 o 3 , pre-calcined at 700° C. for 4 hours, and naturally cooled to room temperature to obtain a pre-calcined carrier.

[0039] 2. Impregnated active components:

[0040] Weigh 170g copper nitrate trihydrate and 220g nickel nitrate hexahydrate, dissolve them in 90ml water, and use the prepared solution to cyclically impregnate the pre-calcined carrier obtained in 1 at 60°C for 12 hours. The impregnation process is the same as in Example 1. After filtering, dry at 60°C for 2 hours, then dry at 120°C for 8 hours, and finally bake at 550°C for 4 hours, and cool down to room temperature naturally to obtain the required catalyst.

[0041] 3. Catalyst evaluation and application:

[0042] Take the required amount of catalyst prepared as above, put it into a 100ml fixed-bed reactor, pass through the hydrogen gas at 600ml / min after passing the nitrogen replacement, and reduce it under the hydrogen flow at 280-...

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PUM

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Abstract

The invention relates to diethylene glycol ammoniated morpholine catalyst and the process. Its character lies in: it uses gamma-Al2O3 or (gamma + theta)-Al2O3 as carrier, carrying at least two active components in Cu, Ni, CO. The manufacturing method is: the above mentioned carrier is baked under temperature of 700-800deg.C for 4-10 hours, acquires the preheated carrier, immersing at least two nitrite salt liquid with Cu, Ni, CO under 40-70deg.C, then they are dried after being filtered, baked under 400-600deg.C for 4 hours, then it is cooled to room temperature naturally. The DEG converting rate is 98.1-99.8mol%; the morpholine selectivity is 90.71-94.44mol%. The process is simple and the cost is low.

Description

technical field [0001] The invention relates to an ammoniation catalyst, in particular to a catalyst for producing 1,4-oxazepine through the ammoniation of diethylene glycol, and a preparation method and application of the catalyst. Background technique [0002] 1,4-Oxazepine, commonly known as morpholine, is an important fine chemical, mainly used in rubber accelerators, vulcanizing agents, corrosion inhibitors, anti-scaling agents, pharmaceutical surfactants and textile printing and dyeing auxiliaries raw materials. The synthetic methods of morpholine mainly fall into two categories, one is diethanolamine strong acid dehydration method, and the other is diethylene glycol ammoniation method. Because the raw materials of the former are more expensive and the three wastes are serious, the use of the former is basically stopped at present. Generally, diethylene glycol, a by-product of petrochemical industry, is used as raw material to synthesize morp...

Claims

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Application Information

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IPC IPC(8): B01J23/70B01J37/02C07D295/02
Inventor 王硕侯淑兰王勋章李立军
Owner CNPC JILIN CHEM GROUP CORP
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