Method for directly synthesizing polyoxymethylene dimethyl ether by taking dilute formaldehyde and methylal as raw materials
A technology of polyoxymethylene dimethyl ether and dilute formaldehyde, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as unfavorable process, increased side reactions, increased recycled materials, etc., and achieves technical High comprehensive economic benefits, reduced generation of by-products, and shortened process flow
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Embodiment 1
[0027] A 37% aqueous formaldehyde solution and acetal mixture are used to pass through a series of silica ceramic membranes (the total membrane area is 0.21m 2 ) to synthesize DMM after dehydration n .
[0028] Mix 37% formaldehyde aqueous solution and methylal according to the molar ratio of formaldehyde and methylal 1:1, and then enter the silica ceramic membrane series membrane (the total membrane area is 0.15m 2 ), the membrane pervaporation device was used for dehydration at 85°C. During the dehydration process, analyze the water content of the feed liquid.
[0029] When the water content is 15.1% [water content = m water / (m water + m formaldehyde) × 100%], put about 105g of dehydration feed liquid into the 150mL reaction kettle preset with 4.2g of HZSM-5 catalyst and nitrogen replacement , and then heated to 120°C for reaction. After reacting for 60 minutes, cool to below 10° C., press filter with a 0.2 μm polytetrafluoroethylene membrane, and separate the catalyst...
Embodiment 2
[0032] Synthesis of DMM with 37% formaldehyde aqueous solution and methylal mixture through silica ceramic membrane series membrane dehydration n .
[0033] Mix 37% formaldehyde aqueous solution and methylal according to the molar ratio of formaldehyde and methylal 1:1, and then enter the silica ceramic membrane series membrane (the total membrane area is 0.15m 2 ), the membrane pervaporation device was used for dehydration at 100°C. During the dehydration process, analyze the water content of the feed liquid.
[0034] When the water content is 4.7% [water content = m water / (m water + m formaldehyde) × 100%], put about 105g of dehydration feed liquid into the 150mL reaction kettle preset with 4.2g of HZSM-5 catalyst and nitrogen replacement , and then heated to 120°C for reaction. After reacting for 60 minutes, cool to below 10° C., press filter with a 0.2 μm polytetrafluoroethylene membrane, and separate the catalyst to obtain the product. Get product and carry out chroma...
Embodiment 3
[0036] Synthesis of DMM with 37% formaldehyde aqueous solution and methylal mixture through silica ceramic membrane series membrane dehydration n .
[0037] Mix 37% formaldehyde aqueous solution and methylal according to the molar ratio of formaldehyde and methylal 1:1, and then enter the silica ceramic membrane series membrane (the total membrane area is 0.15m 2 ) Membrane pervaporation device for dehydration at 110°C. During the dehydration process, analyze the water content of the feed liquid.
[0038] When the water content is 1.0% [water content = m water / (m water + m formaldehyde) × 100%], put about 105g of dehydration feed liquid into the 150mL reaction kettle preset with 4.2g HZSM-5 catalyst and nitrogen replacement , and then heated to 120°C for reaction. After reacting for 60 minutes, cool to below 10° C., press filter with a 0.2 μm polytetrafluoroethylene membrane, and separate the catalyst to obtain the product. Get product and carry out chromatographic analy...
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