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Preparation method of catalyst for ammoxidation of caprolactam

A caprolactam and catalyst technology, applied in the direction of catalyst activation/preparation, preparation of organic compounds, physical/chemical process catalysts, etc., can solve the problems of low conversion rate, low reaction temperature, low selectivity, etc., and achieve low cost and simple preparation , Preparation and easy-to-obtain effect

Active Publication Date: 2019-11-05
CHINA CATALYST HLDG CO LTD
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  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the preparation of 6-aminocapronitrile is mainly obtained by partial hydrogenation of 1,6-adiponitrile. The preparation of 6-aminocapronitrile by caprolactam has a gas phase method and a liquid phase method. The liquid phase method mainly uses phosphate as a catalyst, and the reaction temperature Low, but the conversion rate is relatively low
The gas-phase method uses one or more of alkaline earth metal oxides, transition metal oxides, silicon oxide or alumina as a catalyst. Compared with the liquid-phase method, the conversion rate is higher, but the selectivity is low, and the catalyst is not used for a long time.

Method used

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  • Preparation method of catalyst for ammoxidation of caprolactam
  • Preparation method of catalyst for ammoxidation of caprolactam
  • Preparation method of catalyst for ammoxidation of caprolactam

Examples

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Effect test

Embodiment 1

[0024] Weigh 5g of magnesium nitrate, 5g of aluminum nitrate, 1g of nickel nitrate and 150g of water to prepare a mixed solution, weigh 100g of aluminum phosphorus molecular sieve, add the aqueous solution of the active component to the aluminum phosphorus molecular sieve; After 4 hours, the water was dried under reduced pressure; the filter cake was dried at 120°C, shaped, and calcined at 550°C for 6 hours to obtain a catalyst (see Figure 1-3 ). Take 4g of the calcined catalyst and fill it in a fixed bed, heat up to 420°C, dissolve the caprolactam with acetonitrile and feed it at a space velocity of 0.5h-1, cool and collect the reaction solution, take a sample and control it, the conversion rate of the raw material caprolactam is 81%, and the product The selectivity of 6-aminocapronitrile is greater than 99.0%.

Embodiment 2

[0026] Weigh 7g of magnesium nitrate, 7g of aluminum nitrate, 1g of nickel nitrate and 170g of water to prepare a mixed solution, weigh 100g of aluminum phosphorus molecular sieve, and add the aqueous solution of the active component to the aluminum phosphorus molecular sieve; After 4 hours, the water was dried under reduced pressure; the filter cake was dried at 120° C., shaped, and calcined at 550° C. for 5 hours to obtain the catalyst. Take 4g of the calcined catalyst and fill it in a fixed bed, raise the temperature to 450°C, dissolve the caprolactam in acetonitrile and feed it at a space velocity of 0.5h-1, cool and collect the reaction solution, take a sample and control it, the conversion rate of the raw material is 82.2%, the selectivity Greater than 99.0%.

Embodiment 3

[0028] Weigh 9g of magnesium nitrate, 9g of aluminum nitrate, 2g of nickel nitrate and 200g of water to prepare a mixed solution, weigh 100g of aluminum phosphorus molecular sieve, add the aqueous solution of the active component to the aluminum phosphorus molecular sieve; After 4 hours, the water was dried under reduced pressure; the filter cake was dried at 120°C, shaped, and calcined at 550°C for 6 hours to obtain the catalyst. Take 4g of the calcined catalyst and fill it in a fixed bed, raise the temperature to 420°C, dissolve the caprolactam in acetonitrile and feed it at a space velocity of 0.5h-1, cool and collect the reaction liquid, take a sample and control it, the conversion rate of the raw material is 82.2%, the selectivity Greater than 99.0%.

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Abstract

The invention discloses a preparation method of a catalyst for ammoxidation of caprolactam. According to the method, a phosphorus-aluminum molecular sieve is taken as a carrier, a certain amount of active components of magnesium nitrate, aluminum nitrate and nickel nitrate are carried through a dipping method at a certain temperature, an ammoniation dehydration catalyst is obtained after drying, forming and roasting, the catalyst is packed in a fixed bed, and the caprolactam and ammonia gas are subjected to a reaction at 420-500 DEG C under 0-1 mpa. The preparation method of the obtained catalyst is simple, the conversion rate of the caprolactam is greater than 80%, and the selectivity of 6-aminocapronitrile is greater than 99%.

Description

technical field [0001] The invention belongs to a method for synthesizing organic compounds, and relates to a method for preparing a catalyst for caprolactam ammonification. Background technique [0002] 6-Aminocapronitrile is an important chemical intermediate and an important raw material for the preparation of hexamethylenediamine, which can be used to produce the polymer nylon 66. At present, the preparation of 6-aminocapronitrile is mainly obtained by partial hydrogenation of 1,6-adiponitrile. There are gas phase method and liquid phase method for preparing 6-aminocapronitrile by caprolactam. The liquid phase method mainly uses phosphate as a catalyst, and the reaction temperature low, but the conversion rate is relatively low. The gas phase method uses one or more of alkaline earth metal oxides, transition metal oxides, silicon oxide or alumina as a catalyst. Compared with the liquid phase method, the conversion rate is higher, but the selectivity is low, and the cata...

Claims

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Application Information

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IPC IPC(8): B01J29/83B01J37/02C07C253/00C07C255/24
CPCB01J29/83B01J37/0201C07C253/00C07C255/24
Inventor 王庆吉王蕊李小龙王炳春王贤彬李进
Owner CHINA CATALYST HLDG CO LTD
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