Method for preparing pure p-cresol and pure m-cresol by separating industrial mixed p-cresol and m-cresol

A technology for p-cresol and mixed cresol is applied in the field of separating industrial p-cresol to prepare pure p-cresol and pure m-cresol. Efficiency, low equipment requirements, improved safety effects

Active Publication Date: 2013-10-02
BEIJING RISUN TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the azeotropic distillation method is in the presence of sodium p-cresolate, p-cresol can be distilled out with water azeotropically, but this method consumes too much energy; the high-pressure crystallization separation method requires a pressure of 100-300 MPa, which requires too much equipment. High, the investment is too large; the molecular sieve adsorption separation method is difficult to select and prepare molecular sieves, and the adsorption capacity is limited, and less is used; the alkylation separation method requires alkylation and dealkylation, high vacuum distillation, etc., and the equipment is relatively Complex, large investment and high cost; the chelate-like separation method is simple to operate, the raw materials are easy to obtain, and various raw materials can be recycled
[0004] It is known that there are some prior art, such as "Liaoning Chemical Industry" 1977, 04, 8-13; Chemical Research and Application, Volume 15, No. 6, 871-872; patent documents US3855195, CN1127241A, JP1287049A, etc. relate to compound separation method to separate m-cresol and p-cresol, but the ultimate goal of the separation is only to separate m-cresol or p-cresol as a single product, and the remaining m-p-cresol does not mention further processing scheme, if the fraction cannot be further purified, it is not economical to sell it at a low price in the form of a mixture
None of the above-mentioned articles or patents involves an integrated full-flow process for obtaining m-cresol products and p-cresol products at the same time through one separation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Use inter-industrial p-cresol (purchased from Xingtai Xuyang Coal Chemical Co., Ltd.) as raw material, including m-cresol (58.5wt%), p-cresol (27.8wt%), 2,4-xylenol ( 5.7wt%), 2,5-xylenol (4.2wt%), also contains some o-cresol, phenol and 2-ethylphenol. First, add oxalic acid (Beihua Reagent Factory) in the glass three-necked flask, the amount of oxalic acid added is 0.6 times of the molar weight of p-cresol in the raw material mixed cresol, then add solvent cyclohexane, the amount of cyclohexane added is mixed 1 times the volume of cresol, heated to boiling, maintained for 0.5 hours, added raw materials mixed with cresol, kept the reaction solution boiling, maintained for 2 hours, stopped heating, naturally cooled down to 4°C, maintained for 4 hours. Filtration, the solid-liquid mixture is filtered and separated to obtain p-cresol oxalic acid crystals, and the filtrate is cyclohexane and by-product mixed cresol 1. After the obtained p-cresol crystals are drained, they ...

Embodiment 2

[0031] The experimental device and operation are the same as in Example 1, except that in the m-cresol extraction step, the molar ratio of the addition of urea to the m-cresol in mixed cresol 1 is 1:1, and p-cresol extraction efficiency, p-cresol purity, The composition of mixed cresol 1, the extraction efficiency of m-cresol, and the analysis results of m-cresol purity are shown in Table 1.

Embodiment 3

[0033]The experimental device and operation are the same as in Example 1, except that in the p-cresol extraction step, dihydrate oxalic acid is replaced by anhydrous oxalic acid, and the molar amount of anhydrous oxalic acid added remains unchanged; The molar ratio of m-cresol in cresol 1 was changed to 1:1, the extraction efficiency of p-cresol, the purity of p-cresol, the composition of mixed cresol 1 and the extraction efficiency of m-cresol, and the analysis results of m-cresol purity are shown in Table 1.

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Abstract

The invention relates to a method for preparing pure p-cresol and pure m-cresol by separating industrial mixed p-cresol and m-cresol. In specific, the invention relates to a method for preparing pure p-cresol and pure m-cresol through a complexion separation method by taking industrial mixed p-cresol and m-cresol as the raw material. Compared with the separation method in the prior art, the method provided by the invention can obtain p-cresol product and m-cresol product at a time and comprises the advantages that through the coupling of separation processes of p-cresol and m-cresol, the proportion of p-cresol and m-cresol in the m-cresol extraction raw material is increased, the residual p-cresol and m-cresol are separated in a circulatory manner, and the extraction efficiency of m-cresol is improved to the greatest extent; three wastes are not generated in the whole separation process, the operation is carried out under ordinary pressure, the requirement on equipment is low, and the method belongs to an environment-friendly and green separation technological method.

Description

technical field [0001] The present invention relates to a kind of method that separates inter-industrial p-cresol to prepare pure p-cresol and pure m-cresol. A method for preparing pure p-cresol and pure m-cresol. Background technique [0002] The three isomers of cresol (o-cresol, p-cresol and m-cresol) are all important chemical raw materials, but because of their very close properties, especially p-cresol and m-cresol, the two The normal pressure boiling point difference of cresol is only 0.5 degrees, it is difficult to separate by rectification, crystallization separation and extractive distillation will consume a lot of energy, low efficiency and high cost. The cresol produced by refining crude phenol in coal chemical industry or chemical synthesis is basically a mixture of m-cresol and p-cresol. Most of this m-p-cresol mixture is used for the production of low value-added applications such as polyester enameled wire field, failing to make full use of the value of m-c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C39/07C07C37/68C07C37/86
Inventor 杨雪岗张敏生彭永兴孙长江
Owner BEIJING RISUN TECH CO LTD
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