Method for synthesizing methylal
A synthesis method, methylal technology, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as environmental pollution, high cost, equipment corrosion, etc., and achieve cost reduction, low cost, and equipment less corrosive effect
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Embodiment 1
[0020] In the reactor, formaldehyde and methanol were reacted at 40°C for 240min under the action of a solid acid catalyst with a molar ratio of 1:1.5, and the reflux ratio was controlled to be 1:1, and the fraction at the top of the tower was collected at 40°C. Analysis shows that the methylal content is 73%, wherein the solid acid catalyst is acidified aluminum pillared montmorillonite, the dosage is 2% of the total mass of methanol and formaldehyde, and the loading capacity of the main active component sulfuric acid is 30wt%.
[0021] The preparation of acidified aluminum pillared montmorillonite comprises the following steps:
[0022] (1) Preparation of columnar agent: AlCl 3 ·6H 2 Add NaOH solution dropwise into the O aqueous solution, after the dropwise addition is completed, stir at constant temperature for 1 hour, and age for 16 hours to obtain a columnar agent, in which NaOH and AlCl 3 ·6H 2 The molar ratio of O is 1:1, AlCl 3 ·6H 2 The molar concentration of the...
Embodiment 2
[0026] In the reactor, formaldehyde and methanol were reacted at 70°C for 190min under the action of a solid acid catalyst at a molar ratio of 1:2.7, and the reflux ratio was controlled to be 1:1.8. The fraction at the top of the tower was collected at 43°C, and the reaction product was analyzed by gas chromatography. Analysis showed that the methylal content was 76%. Among them, the solid acid catalyst was acidified aluminum pillared montmorillonite, the dosage was 15% of the total mass of methanol and formaldehyde, and the loading amount of sulfuric acid, the main active component, was 5 wt %.
[0027] The preparation of acidified aluminum pillared montmorillonite comprises the following steps:
[0028] (1) Preparation of columning agent: AlCl 3 ·6H 2 Add NaOH solution dropwise into the O aqueous solution, after the dropwise addition is completed, stir at constant temperature for 3 hours, and age for 24 hours to obtain a columnar agent, in which NaOH and AlCl 3 ·6H 2 The ...
Embodiment 3
[0032]In the reactor, formaldehyde and methanol reacted at 60°C for 140min under the action of a solid acid catalyst with a molar ratio of 1:3, and the reflux ratio was controlled to be 1:2.7. The fraction at the top of the tower was collected at 47°C, and the reaction product was analyzed by gas chromatography. Analysis shows that the methylal content is 78%. Among them, the solid acid catalyst is acidified aluminum pillared montmorillonite, the dosage is 8% of the total mass of methanol and formaldehyde, and the loading amount of sulfuric acid, the main active component, is 10 wt%.
[0033] The preparation of acidified aluminum pillared montmorillonite comprises the following steps:
[0034] (1) Preparation of columnar agent: AlCl 3 ·6H 2 Add NaOH solution dropwise into the O aqueous solution, after the dropwise addition, stir at constant temperature for 2 hours, and age for 8 hours to obtain a columnar agent, in which NaOH and AlCl 3 ·6H 2 The molar ratio of O is 1.7:1, ...
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