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Method for synthesizing N-methylmorpholine with granular solid superacid as catalyst

A technology of solid superacid and methylmorpholine, which is applied in the fields of chemical instruments and methods, physical/chemical process catalysts, organic chemistry, etc., and can solve the problems of increased cost of N-methylmorpholine, low reaction selectivity, and high raw material prices, etc. problems, to achieve the effect of excellent catalytic activity, high product yield and single raw material

Inactive Publication Date: 2010-02-03
曲阜市圣泉催化应用科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Wherein the morpholine method and the dichloroethyl ether method have higher raw material prices, which will increase the cost of producing N-methylmorpholine; the diethanolamine method and the diethylene glycol method, the reaction process will not only carry out the alkylation reaction, but also carry out The cyclization reaction, like this, is technically demanding and the reaction selectivity is low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Embodiment 1: a kind of method that catalyzes the synthesis of N-methylmorpholine with granular solid superacid,

[0023] (1) Add catalyst: In a fixed bed with a diameter of 3 cm and a length of 25 cm, the granular SO of Φ=4~6 is loaded. 4 2～ / M x o y 100g of quasi-solid superacid catalyst;

[0024] (2) Heating: heating to raise the temperature to 260-280°C;

[0025] (3) Introduce nitrogen: 27h at volumetric space velocity -1 Feed nitrogen into the fixed bed, and keep the catalyst under nitrogen protection all the time;

[0026] (4) Input N-methyldiethanolamine: with mass space velocity of 0.18h -1 Input N-methyldiethanolamine aqueous solution (the volume ratio of N-methylmorpholine and water is 1: 0.5) to fixed bed;

[0027] (5) product generation: N-methylmorpholine is dehydrated under the continuous catalytic action of hot catalyst to generate N-methylmorpholine;

[0028] (6) Product post-treatment: After the above reaction, the mixed gas of N-methylmorpholin...

Embodiment 2

[0029] Embodiment 2: a kind of method that catalyzes the synthesis of N-methylmorpholine with granular solid superacid,

[0030] (1) Add catalyst: In a fixed bed with a diameter of 3 cm and a length of 25 cm, the granular SO of Φ=4~6 is loaded. 4 2～ / M x o y 110g of quasi-solid superacid catalyst;

[0031] (2) Heating: heating to raise the temperature to 280-300°C;

[0032] (3) Introduce nitrogen: at a volumetric space velocity of 31.5h -1 Feed nitrogen into the fixed bed, and keep the catalyst under nitrogen protection all the time;

[0033] (4) Input N-methyldiethanolamine: with mass space velocity of 0.24h -1 Input N-methyldiethanolamine aqueous solution (the volume ratio of N-methylmorpholine and water is 1: 0.7) to fixed bed;

[0034] (5) product generation: N-methylmorpholine is dehydrated under the continuous catalytic action of hot catalyst to generate N-methylmorpholine;

[0035] (6) Product post-treatment: After the above reaction, the mixed gas of N-methylmo...

Embodiment 3

[0036] Embodiment 3: a kind of method that catalyzes the synthesis of N-methylmorpholine with granular solid superacid,

[0037] (1) Add catalyst: In a fixed bed with a diameter of 3 cm and a length of 25 cm, the granular SO of Φ=4~6 is loaded. 4 2～ / M x o y 120g of quasi-solid superacid catalyst;

[0038] (2) Heating: heating to raise the temperature to 320-340°C;

[0039] (3) Introduce nitrogen: 36h at volumetric space velocity -1 Feed nitrogen into the fixed bed, and keep the catalyst under nitrogen protection all the time;

[0040] (4) Input N-methyldiethanolamine: with mass space velocity of 0.3h -1 Input N-methyldiethanolamine aqueous solution (the volume ratio of N-methylmorpholine and water is 1: 0.9) to fixed bed;

[0041] (5) product generation: N-methylmorpholine is dehydrated under the continuous catalytic action of hot catalyst to generate N-methylmorpholine;

[0042] (6) Product post-treatment: After the above reaction, the mixed gas of N-methylmorpholine...

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Abstract

A method for synthesizing N-methylmorpholine with granular solid superacid as a catalyst comprises the following steps: loading an SO4<2-> / MxOy super acidic catalyst into a fixed bed; heating the fixed bed to the temperature of 260-360 DEG C; pumping nitrogen into the fixed bed to ensure the catalysts under the protection of the nitrogen; introducing N-methyldiethanolamine aqueous solution into the fixed bed; dehydrating the N-methyldiethanolamine aqueous solution in the presence of the catalyst to generate the N-methylmorpholine; collecting mixed gas of the N-methylmorpholine and water, whichis discharged from the discharge hole of the fixed bed and passes through a condensing unit, into a flask, then adding solid NaOH for alkaline separation to separate supernatant; drying the supernatant with NaOH, removing the drying agent and carrying out rectification to collect distillates at a temperature of 104-106 DEG C to obtain the product of N-methylmorpholine. The invention has the effect as follows: the invention is fixed bed catalysis under normal pressure; the catalyst has stability and resistance to carbon deposition, and the method has the advantages of simple catalytic process,high product yield and purity, low cost and the like.

Description

technical field [0001] The invention relates to a method for synthesizing fine chemical raw materials, in particular to a method for catalyzing and synthesizing N-methylmorpholine with granular solid superacid. Background technique [0002] N-methylmorpholine is an important fine chemical raw material. It can be used not only as a catalyst for the production of polyurethane foam, but also for the synthesis of medicines, pesticides, surfactants, emulsifiers, and corrosion inhibitors. In addition, it can be used as a solvent, extractant and curing agent for polyurethane coatings. The most important future use of N-methylmorpholine is the synthesis of N-methylmorpholine oxide, which is currently known as the "green fiber" Lyocell (commonly known as Tencel) and Newcell rayon filament spinning solvent, can also be used as a solvent Used in the production of vegetable casings. [0003] At present, there are five main methods for synthesizing N-methylmorpholine: the morpholine me...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D295/03B01J27/053B01J35/02
Inventor 李修刚吴会林张玲钰
Owner 曲阜市圣泉催化应用科技有限公司
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