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A technology of methylmorpholine and morpholine, applied in the field of preparation of organic compounds, to achieve the effects of cost reduction, low production cost and high product purity
Active Publication Date: 2014-11-05
ZHEJIANG JIANYE CHEM +1
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[0010] It can be seen that the existing methods are only suitable for small-scale production in the laboratory, and none of the methods are suitable for large-scale production
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Embodiment 1
[0032] Embodiment 1, a kind of preparation method of N-methylmorpholine, carry out following steps successively:
[0033] 1), preparation of supported catalyst:
[0034] a), the commercially available γ-Al 2 o 3 With a volume concentration of 5% H 3 PO 4 Soak the solution at 40-50°C for 60 minutes, filter out and dry, then bake at 400°C for 2 hours and 750°C for 6 hours to obtain the treated γ-Al 2 o 3 ,spare.
[0035] b) Add distilled water to 28.1g of copper nitrate and 13.3g of zinc nitrate solid (excluding crystal water) to make the volume to 50mL. After the copper nitrate and zinc nitrate are dissolved, 50mL of metal salt solution is obtained for later use.
[0036] With 1.2mL metal salt solution / 1.0gγ-Al 2 o 3 The ratio of the carrier, the γ-Al after the above treatment 2 o 3 Soak in the prepared solution for 36 hours; filter to obtain filtrate and catalyst.
[0037] c) The catalyst obtained after the above-mentioned filtration was dried at 60° C. for 2 hours ...
Embodiment 2
[0043] Embodiment 2, a kind of preparation method of N-methylmorpholine:
[0044] In step 2), the mol ratio of morpholine and methyl formate is changed to 1:0.9, the reaction temperature is controlled at 120°C, the hydrogen pressure is adjusted so that the reactor pressure remains at 0.15Mpa, and the raw material is 0.3g / h / mL catalyst The space velocity enters the catalyst bed layer to react. All the other are equal to embodiment 1.
[0045] The gas chromatographic analysis content of the obtained product is 90%, and the product yield is 95%.
Embodiment 3
[0046] Embodiment 3, a kind of preparation method of N-methylmorpholine:
[0047] In step 2), the molar ratio of morpholine and methyl formate is changed to 1:0.7, the reaction temperature is controlled at 125°C, the hydrogen pressure is adjusted so that the reactor pressure remains at 0.12MPa, and the raw material is 0.1g / h / mL catalyst The space velocity enters the catalyst bed layer to react. All the other are equal to embodiment 1.
[0048] The gas chromatographic analysis content of the obtained product is 97%, and the product yield is 93%.
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Abstract
A disclosed preparation method for N-methylmorpholine comprises: taking a normal-pressure fixed bed reactor as a reaction apparatus, arranging a supported catalyst in the normal-pressure fixed bed reactor, taking a mixture of morpholine and methyl formate as raw materials, and controlling the molar ratio of methyl formate to morpholine to be 0.5-0.9:1; enabling gasified raw materials to pass through the fixed bed reactor comprising the supported catalyst, so as to perform amination reaction in the presence of hydrogen, and controlling the reaction pressure to be 0.12-0.19 MPa, the temperature to be 120-130 DEG C and the reaction volume space velocity to be 0.05-0.3 g/(h*mL); and after the reaction is finished, condensing and collecting reactants, and performing dewatering and rectification to obtain N-methylmorpholine. The preparation process of the supported catalyst comprises: utilizing a metal salt solution and a carrier to prepare the supported catalyst, wherein the metal accounts for 22%-32% by weight of the whole supported catalyst, and the metal salt is a copper salt or a zinc salt.
Description
technical field [0001] The invention relates to a preparation method of an organic compound, in particular to a preparation method of an organic chemical intermediate - N-methylmorpholine. Background technique [0002] N-Methylmorpholine is an important organic chemical intermediate, an excellent solvent, emulsifier, corrosion inhibitor, polyurethane foam catalyst, and can also be used as a pesticide intermediate. The synthesis methods mainly include N-methylation method using morpholine as raw material, cyclization method using diethanolamine as raw material, cyclization method using diethyl alcohol as raw material, and synthesis method using dichloroethane as raw material. These methods are generally catalyzed by metal catalysts and carried out at higher temperatures and pressures. The most convenient method is to use morpholine as a raw material and directly select different methylating reagents for N-methylation reaction. [0003] At present, take morpholine as the met...
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