Method for refining and purifying polyformaldehyde dialkyl ether
A formaldehyde dialkyl ether and product technology, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of poor extraction rate of extraction unit, poor extraction product purity, poor extraction efficiency, etc., and meet the reaction conditions Gentle, high operational safety effect
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Embodiment 1
[0051] This embodiment provides a method for refining and purifying polyoxymethylene dialkyl ether, which specifically includes the following steps:
[0052] S1. Add sodium percarbonate to the equilibrium product of polyoxymethylene dialkyl ether, the input amount of sodium percarbonate is 1% of the mass of the equilibrium product, heat to 50°C for reaction, and treat for 1 hour;
[0053] S2, performing solid-liquid separation on the product obtained after the reaction in step S1, and collecting the liquid phase product;
[0054] S3. Carry out fractional atmospheric pressure distillation on the liquid phase product, and distill out the fraction before 60°C. The initial boiling point ~60°C is the unreacted raw material (formaldehyde, methanol and methylal), and the fraction collected at ~110°C is divided into two poly product (PODE 2 ), the fraction collected at ~160°C was the trimerization product (PODE 3 ), collecting fractions at ~200°C as tetramerization products (PODE 4...
Embodiment 2
[0056] This embodiment provides a method for refining and purifying polyoxymethylene dialkyl ether, which specifically includes the following steps:
[0057] S1. Add sodium percarbonate to the equilibrium product of polyoxymethylene dialkyl ether, the input amount of sodium percarbonate is 3% of the mass of the equilibrium product, heat to 50°C for reaction, and treat for 1 hour;
[0058] S2, performing solid-liquid separation on the product obtained after the reaction in step S1, and collecting the liquid phase product;
[0059] S3. The liquid phase product is rectified at atmospheric pressure, the temperature at the bottom of the tower is 100° C., and the reflux ratio is 1. The production liquid at the top of the tower consists of methanol, methylal and a small amount of dimerization products; Then carry out fractional atmospheric pressure distillation on the polymer products with a degree of polymerization of 2 to 8, and collect the fractions at ~110°C as dimerization prod...
Embodiment 3
[0061] This embodiment provides a method for refining and purifying polyoxymethylene dialkyl ether, which specifically includes the following steps:
[0062] S1. Add sodium percarbonate to the equilibrium product of polyoxymethylene dialkyl ether, the input amount of sodium percarbonate is 5% of the mass of the equilibrium product, heat to 50°C for reaction, and treat for 1 hour;
[0063] S2, performing solid-liquid separation on the product obtained after the reaction in step S1, and collecting the liquid phase product;
[0064] S3. Carry out fractional atmospheric pressure distillation on the liquid phase product, distill out the fraction before 60°C, the initial boiling point ~60°C is the unreacted raw material (formaldehyde, methanol and methylal), and the fraction collected at ~110°C is dimerization Product (PODE 2 ), the fraction collected at ~160°C was the trimerization product (PODE 3 ), collecting fractions at ~200°C as tetramerization products (PODE 4 ); the fract...
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