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Purifying method for dibenzyl alcohol

A purification method and technology of dibenzyl alcohol, applied in the field of purification of organic raw materials, can solve the problems of long time consumption, residues, high energy consumption and the like

Active Publication Date: 2019-06-07
WUHAN YOUJI IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method also has certain inconveniences in production: 1. The steaming process of the crude product after the reaction, because the specific heat of water is relatively large, the whole process takes too long, consumes a lot of energy, and often due to the material being The water vapor is brought out and cooled and crystallized at the top of the equipment, which leads to blockage of the top pipe; 2. After steaming, the material remains in the brine, and the brine cannot be recycled and reused, and the material consumption is large; 3. The two-step crystallization step is cumbersome, which is not conducive to application in mass production

Method used

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  • Purifying method for dibenzyl alcohol
  • Purifying method for dibenzyl alcohol
  • Purifying method for dibenzyl alcohol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] In order to achieve the purpose of extracting the finished product dibenzyl alcohol to the organic phase by means of solvent extraction, and then realize the purification of dibenzyl alcohol by means of solvent crystallization. The present invention examines a variety of common organic solvents.

[0029] After the step of synthesizing terephthalic benzyl alcohol (yield 37g, water amount 600g) is completed, add 100g of extractant for extraction, separate the liquid while hot, then extract the water phase once with 100g of extractant, and collect the oil layer. The above two collected oil phases were naturally cooled to room temperature, recrystallized to obtain a white needle-like solid, and the extraction rate was calculated. In this embodiment, the internal standard method is used to determine the mass of the product in the extraction solvent / total mass of the crude product; the extraction temperature is 70°C. Obtain the extraction data of terephthalbenzyl alcohol in ...

Embodiment 2

[0042] Based on the best extraction effect of n-butanol obtained in Example 1, this example will investigate the optimum extraction temperature of n-butanol. In the investigation of temperature, different temperatures also have a significant impact on the extraction effect. At room temperature, the extraction efficiency of n-butanol is poor due to the slow molecular motion rate of the two phases at low temperature; as the temperature rises, the extraction efficiency of n-butanol increases gradually, and it is the best at 75°C; , because n-butanol and water are azeotropic at 93°C, the extraction and separation effects are reduced. The extraction efficiency of n-butanol-p-phenylene benzyl alcohol under different temperatures is shown in Table 4:

[0043] Table 4 Extraction efficiency table of n-butanol-p-phenylene benzyl alcohol at different temperatures

[0044]

[0045]

[0046]

[0047]

Embodiment 3

[0049] Based on the optimal result in Example 2, after the reacted aqueous solution was extracted twice, the oil phase was collected and concentrated for post-treatment. A small amount of product dibenzyl alcohol and n-butanol are entrained in the water phase, which is applied to the next batch of reactions. After applying mechanically for 5 times, after the salt content in the water is basically saturated, all the water phase is evaporated, and the mechanical application is continued, and the solid salt is harmlessly treated.

[0050]1. Add 30g (1.1equiv.) of sodium carbonate and 600g of water to the three-necked flask, stir evenly, then add 45g (1.0euqiv.) of p-dichlorobenzyl, 4.5g of n-butanol, heat up and reflux for 4.5 hours, and the reaction ends When cooled to about 80°C, add 100g of n-butanol for extraction, separate the liquid while it is hot, then extract the water phase with 100g of n-butanol once, collect the oil layer, concentrate until the weight of the oil phase...

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Abstract

The invention provides a method for efficiently separating dibenzyl alcohol in the production process of the dibenzyl alcohol. The method comprises the steps of performing extraction on the product dibenzyl alcohol obtained after a reaction is completed by using a solvent extraction manner to an organic phase, and performing purification on the dibenzyl alcohol by utilizing a same-solvent crystallization manner. The method provided by the invention solves the following technical problems: 1, in the reacted crude product water evaporation process, water with a mass equivalent of 15 times by mass of raw material dichlorobenzyl needs to be added in an alkali hydrolysis reaction to ensure sufficient hydrolysis of the dichlorobenzyl, 65-75% of the water is required to be evaporated out after the alkali hydrolysis reaction is completed, specific heat of the water is large, so that time consumed in the whole process is too long, the energy consumption is huge, and a pipeline located at the top is blocked because a material taken out by water vapor is cooled and crystallized at the top; 2, after water is evaporated, the material remains in brine, so that the brine cannot be recycled or reused, and the material consumption is larger; and 3, two-step crystallization is cumbersome and does not facilitate large-scale production.

Description

technical field [0001] The invention relates to a method for purifying organic raw materials, in particular to a method for purifying dibenzyl alcohol. Background technique [0002] In the field of materials science, dibenzyl alcohol is an important organic chemical functional block. Two benzyl hydroxyl skeletons make the benzene ring chemical structure of dibenzyl alcohol (ortho-phthalyl dimethanol, m-xylylene dimethanol, tere-xylylene dimethanol collectively) very suitable for synthesizing polymers or long-chain functional materials. Therefore, dibenzyl alcohol has good uses in some high-end functional materials. Among them, phthalic dimethanol is an important organic fine chemical and intermediate, which can be mainly used as a resin additive. Tere-Phenyldimethanol is an important chemical intermediate building block with unique characteristics in the field of high-end materials. [0003] Due to the structural characteristics of dibenzyl alcohol, the 1,2 or 1,3 or 1,4 ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C33/26C07C29/86C07C29/78
Inventor 舒振操代飞程娟朱明伟蔡峰孙波黄正望毛利民
Owner WUHAN YOUJI IND
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