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Catalyst required for coproducing N-methyl morpholine and morpholine

A technology of methyl morpholine and catalyst, applied in the field of catalyst, can solve the problems of single product and inflexible production scheme, and achieve the effects of simplifying the separation process, long service life and high catalytic activity

Active Publication Date: 2009-10-14
BC P INC CHINA NAT PETROLEUM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These two processes have the disadvantages of single product and inflexible production plan.

Method used

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  • Catalyst required for coproducing N-methyl morpholine and morpholine
  • Catalyst required for coproducing N-methyl morpholine and morpholine
  • Catalyst required for coproducing N-methyl morpholine and morpholine

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0014] Example 1 (preparation of catalyst)

[0015] Φ3.2 clover-shaped γ-Al 2 o 3 The carrier was impregnated with 4% magnesium nitrate aqueous solution at 70°C for 3-4 hours, then drained and dried at 120°C for 16 hours. Then high-temperature calcination was carried out, and the temperature was raised to 850° C. at a rate of 50° C. / 30 min and kept for 4 hours. Add 50 grams of the calcined carrier into the beaker and put it in a water bath at 85°C; prepare a mixed solution of copper nitrate and nickel nitrate with a content of 118 grams of copper nitrate / L and 142 grams of nickel nitrate / L, and place it at 85°C in the water bath. After the temperature of the two is constant, add the above-mentioned mixed solution into the beaker containing the carrier, it is advisable that the liquid has just covered the carrier. Immerse for 4 hours, during which time the beaker is shaken constantly. Then the impregnated catalyst was taken out and drained, dried at 120°C for 16 hours, the...

example 2～9

[0016] Example 2~9 (application of catalyst)

[0017] Ni-Cu / (δ+θ)-Al 2 o 3 - The MgO catalyst was crushed into 24-32 mesh particles, weighed 10ml (about 8 grams) and filled into the reactor, and reduced with hydrogen at 300°C for 8 hours, and the flow rate of hydrogen was controlled at 50ml / min. Diethylene glycol, methylamine and liquid ammonia are added to the batching tank at a ratio of 1:2:8 for preparation. Then use the advection pump to continuously add the above-prepared raw materials to the mixer on the upper part of the vaporizer, mix with the hydrogen from the hydrogen cylinder, and then enter the vaporizer bone on the upper part of the reactor together for gasification, and the gas phase material passes through the microreactor continuously The catalyst bed layer, the reaction product is condensed by the condenser and then enters the gas-liquid separator to collect the crude product in the liquid phase, and the gas phase is absorbed by the back pressure valve and t...

example 10～15

[0026] Ni-Cu / (δ+θ)-Al 2 o 3 - The MgO catalyst is crushed into 24-32 mesh particles, weighed 10ml (about 8 grams) and packed into the reactor, and heated at 300°C 4 Reduction with hydrogen under conditions for 8 hours, the flow of hydrogen was controlled at 50ml / min. The reaction pressure is 1.8Mpa, the reaction temperature is 220°C, and the DEG space velocity is 0.14h -1 , the molar ratio of hydrogen to diethylene glycol is 50:1, and the molar ratio of liquid ammonia to diethylene glycol is 8:1. All the other operations are the same as examples 2-9. The processing condition and reaction result of example 10~15 are shown in Table 2.

[0027] The process condition and reaction result of table 2 example 10~15

[0028] Reality

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Abstract

The present invention relates to a kind of catalyst that takes diethylene glycol, liquefied ammonia and monomethylamine as raw materials to co-produce N-methylmorpholine and morpholine, which is based on (δ+θ)Al2O3 and MgO, CaO and BaO Any one is a carrier, on which Ni and Cu are supported as two active components to form; in percent by weight, the catalyst is 100 parts, and the carrier is 78%, wherein (δ+θ) Al O375%, MgO, CaO or BaO is 3%; the active component is 22%, of which Ni is 12% and Cu is 10%. The preparation method of the catalyst is as follows: the clover-shaped γ-Al2O3 carrier is impregnated with magnesium, calcium or barium nitrate aqueous solution, dried and calcined to obtain the above carrier, and then impregnated with copper and nickel nitrate mixed solution, dried and calcined. The above catalyst was obtained.

Description

technical field [0001] The invention relates to a catalyst required for the joint production of N-methylmorpholine and morpholine. Background technique [0002] The patents CN87105893 and CN87105833 of China Petroleum & Chemical Corporation Research Institute of Petroleum and Chemical Industry disclose the Ni-Cu-Cr-Re / Al 2 o 3 In the presence of a catalyst, using diethylene glycol (GDE) and liquid ammonia as raw materials, adopting a liquid-phase fixed-bed reaction process to prepare morpholine, the yield is 80 to 93%; taking diethylene glycol, methanol and liquid ammonia as raw materials, Co-production of N-methylmorpholine and morpholine, the yield of N-methylmorpholine is 66%, and the yield of morpholine is 23%. Due to the adoption of the liquid phase method, the reaction system has a large amount of water and liquid ammonia, and the Cu in the catalyst is easily corroded to generate a copper ammonia complex and loses. The service life of the catalyst is short, so its po...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/755C07D295/02
Inventor 田振生张吉波宋岩张钰崔中文张启忠刘辉
Owner BC P INC CHINA NAT PETROLEUM CORP
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