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Purifying method of dihydroxy alcohol ester compound
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The technology of a glycol ester and a purification method is applied in the field of purification of glycol ester compounds, which can solve the problems of low preparation efficiency and high preparation cost, avoid the use of organic solvents, reduce the impact on the environment, and improve the purification yield Effect
Active Publication Date: 2014-12-03
CHINA PETROLEUM & CHEM CORP +1
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As we all know, the column chromatography method is a method that is often used in the laboratory, but if this method is used in a large-scale preparation process with commercial significance, it will result in low preparation efficiency, high preparation cost and impossibility. Avoid using a large amount of organic solvents to affect the environment and other issues
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Embodiment 1
[0017] In a 1000ml glass there-necked flask, add the 2,4-pentanediol dibenzoate crude product 720g that needs to be purified, this material contains 3% (mass percentage) light component, contains 90% alcohol ester, all the other are needing to remove Impurities. Under the condition of absolute pressure of 1.0KPa, the method of vacuum distillation is used to distill until the temperature of the kettle exceeds 160°C to remove the light components in the material. According to GC analysis, the content of light components is less than 0.1%.
[0018] The above-mentioned treated material is subjected to molecular distillation for the first time in a glass molecular distillation apparatus, the distillation pressure is 1.5 Pa, and the distillation temperature is 175° C., so as to remove impurities with lower boiling points than alcohol esters.
[0019] Carry out the second molecular distillation in the same glass molecular distillation apparatus, the distillation pressure is 0.1Pa, a...
Embodiment 2
[0021] The same alcohol ester feed as described in Example 1 was processed continuously at a feed rate of 12 kg per hour in a three-stage distillation apparatus consisting of a thin film evaporator and two molecular stills. The operating temperature and pressure are as follows:
[0022]
[0023] Remove the light components in the thin film evaporator, remove the impurities with a lower boiling point than the alcohol ester in the first molecular still, and distill the product in the second molecular still to separate it from the heavy component impurities, so that it is continuously operated for 20 hours. About 200 kg of materials are processed, the purity of the product obtained is greater than 99%, and the yield of the product obtained is greater than 95%.
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Abstract
The invention discloses a purifying method of organic dihydroxy alcohol ester compound, and particularly relates to a purifying method for dihydroxy alcohol ester compound, which is mainly characterized by carrying out purification by adopting a molecular distillation method. The purifying method for the dihydroxy alcohol ester compound comprises the following steps: first, removing light components in a reaction coarse product, and then, enabling a vacuum to refer to an absolute pressure in the range of 0-3000 Pa; and finally, carrying out molecular distillation at a temperature in the range of 50-300 DEG C. By using the method, the prior art can be simplified; the depuration yield of a product is improved; the usage of lots of organic solvents is avoided, thereby reducing the influence on the environment; and the purifying method for the dihydroxy alcohol ester compound is a depurating method suitable for commercial compound.
Description
technical field [0001] The invention relates to a method for purifying organic glycol ester compounds, in particular to a method for purifying glycol ester compounds. Background technique [0002] The glycol ester compound of following general formula can be used as the catalyst component of olefin polymerization reaction: [0003] [0004] Wherein: R1 and R2 may be the same or different, selected from linear or branched C1-C20 alkyl, cycloalkyl, aryl, alkaryl, aralkyl, alkenyl or fused ring aryl, R3- R6 groups can be the same or different, selected from hydrogen, halogen or straight chain or branched C1-C20 alkyl, cycloalkyl, aryl, alkaryl, aralkyl, alkenyl or condensed ring aryl, R7-R8 is selected from hydrogen, halogen or straight chain or branched C1-C20 alkyl, cycloalkyl, aryl, alkaryl, aralkyl, alkenyl or condensed ring aryl, above-mentioned R1-R8 group Optionally contains or does not contain one or more halogen atoms as carbon or hydrogen atoms or both substituen...
Claims
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