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Method for synthesizing 4-cyclohexyl morpholine

A technology of cyclohexylmorpholine and a synthesis method, which is applied in the synthesis field of 4-cyclohexylmorpholine, can solve the problems of difficulty in realizing industrialized production, large equipment investment and high production cost, and achieves low price, high yield and utilization of raw materials. high rate effect

Active Publication Date: 2011-11-02
ZHEJIANG JIANYE CHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method requires the use of ozone as an oxidant, which requires large investment in equipment, high production costs, and many by-products, making it difficult to realize industrial production.

Method used

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  • Method for synthesizing 4-cyclohexyl morpholine
  • Method for synthesizing 4-cyclohexyl morpholine
  • Method for synthesizing 4-cyclohexyl morpholine

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preparation example Construction

[0029] (1) Preparation of copper-nickel catalyst

[0030] a), the commercially available γ-Al 2 o 3 Roast at 450°C for 3h and 750°C for 5h before use;

[0031] b) Dissolve 41.2g of copper nitrate and 34.2g of solid nickel nitrate (excluding crystal water) in 50ml of distilled water, and impregnate the alumina that has undergone high-temperature pretreatment at the ratio of 1.2ml of solution / 1g of alumina. In the solution, impregnate 36hr; Filter, obtain filtrate and catalyst;

[0032] c), drying the catalyst obtained by filtration at 60°C for 2h, then putting it into a muffle furnace and roasting at 80°C, 150°C, and 280°C for 3h respectively, and then cooling down naturally;

[0033] d), the catalyst obtained after the above-mentioned cooling is put into the filtrate obtained in step b) and soaked for 24h, and filtered;

[0034] e) Dry the catalyst obtained in step d) at 80°C for 2h, then put it into a muffle furnace and roast at 150°C for 2h, then at 450°C for 4h, then co...

Embodiment 1

[0041] Embodiment 1, a kind of production method of 4-cyclohexylmorpholine, carry out following steps successively:

[0042] 1), prepare copper-nickel catalyst.

[0043] 2) Load the prepared supported catalyst into a fixed-bed reactor, heat at 200°C, and activate by purging with hydrogen until the activation is complete, that is, no condensed water is produced in the lower part of the reactor.

[0044] 3) Mix 42.5g (0.4mol) of diethylene glycol with 73.8g (0.8mol) of cyclohexylamine and place it in a mixing tank. The mixed solution is vaporized by the top preheater of the fixed bed and enters the catalyst bed together with hydrogen Carry out the hydroamination reaction, the volume space velocity of the raw material solution is 0.2h -1, adjust the hydrogen pressure so that the reactor pressure is 0.8Mpa, the catalyst bed temperature is controlled at 220°C, the product after the reaction is collected in liquid form after condensation, and analyzed and separated after enough pro...

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Abstract

The invention discloses a method for synthesizing 4-cyclohexyl morpholine. The method comprises the following steps of: mixing diethylene glycol and cyclohexylamine in a mixing tank; allowing the mixture to pass through a fixed bed containing a supported catalyst; performing catalytic amination reaction under the hydrogen condition; condensing and collecting products; and rectifying to obtain the4-cyclohexyl morpholine, wherein the molar ratio of the diethylene glycol to the cyclohexylamine is 1:(2-10); the aminolysis reaction temperature is between 140 and 240 DEG C; the reaction pressure is 0.6 to 1.8 Mpa; and the volume space velocity of the mixed solution is 0.1 to 0.4 h<-1>. The method has the advantages that: (1) the method is implemented without a solvent, so the reaction is clean, pollution is low and pressure for separating and purifying the products is reduced; (2) the method is high in utilization ratio of raw materials, short in flow and easy to operate, and cost is greatly reduced compared with that of other processes; and (3) the method is wide in raw material sources, low in price, mild in reaction condition, high in yield, simple in aftertreatment and applicable to industrialized production.

Description

technical field [0001] The present invention relates to the synthetic method of organic compound, especially a kind of synthetic method of 4-cyclohexylmorpholine. Background technique [0002] 4-cyclohexylmorpholine (4-cyclohexylmorpholine), its molecular formula is C 10 h 19 NO, whose structural formula is shown in S-1, has a boiling point of 240.0-241.0°C and has a wide range of industrial applications. It is an important organic chemical intermediate and an excellent reagent, emulsifier, corrosion inhibitor and polyurethane foam. catalyst. [0003] [0004] Comprehensive literature report, according to the difference of raw material, the preparation of 4-cyclohexylmorpholine mainly adopts following method at present: [0005] 1. Journal of the American Chemical Society, 107(14), 4175-82(1985) reported that 4,5,6,7-tetrahydrobenzo[d][1,3]disulfide was used as solvent with acetic acid The reaction of heterocyclopentene-2-thione with mercuric acetate gave the product ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D295/033B01J23/755B01J23/745
Inventor 冯烈陈云斌强林萍钟九生
Owner ZHEJIANG JIANYE CHEM
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