A method for separating and purifying p-cresol

A technology for p-cresol and mixed cresol, which is applied in chemical instruments and methods, preparation of organic compounds, and organic chemistry, etc. Separation effect, effect of reducing process cost

Active Publication Date: 2016-08-17
江苏富比亚化学品有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] 1) The content of p-cresol in mixed cresol is less, only 27.8wt%, and the use of oxalic acid method is limited, and the best effect cannot be brought into play;
[0005] 2) use volatile low-boiling solvents in the reaction process, such as cyclohexane, sherwood oil, thereby increasing the loss of solvent, and the proportion of solvent loss accounts for the largest proportion of process cost;
[0006] 3) The p-cresol-oxalic acid complex is directly decomplexed without purification, and the quality index of the obtained p-cresol is difficult to meet the requirements of relevant standards;
[0007] 4) Two different organic solvents are used in the complexation reaction and decomplexation process, and it is difficult to achieve effective separation between the solvents, thus increasing the complexity of the actual operation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] The mixed cresol produced by Feixiang Chemical Group is used as raw material, including 71.3wt% p-cresol, 28.2wt% m-cresol and 0.5wt% 2,6-dimethylcresol. First, add toluene and oxalic acid (Anhui Anhydrous Oxalic Acid Co., Ltd.) to the glass three-necked bottle. The amount of oxalic acid added is 1.0 times the molar weight of p-cresol in the raw material mixed cresol, and the added amount of toluene is 2.1 times the mass of mixed cresol. , heated to 70°C, added mixed cresols, kept warm for 2h after adding, cooled to 5°C, and crystallized for 1h. Solid-liquid separation, the solid is the crude p-cresol-oxalic acid complex, and the filtrate is the toluene solution enriched in m-cresol. Add the crude product of p-cresol-oxalic acid complex to toluene-methanol, wherein the volume content of methanol is 4%, the amount of mixed solvent is 1 times the mass of the crude product of p-cresol-oxalic acid complex, stir at 5°C for 1 h, Solid-liquid separation, the solid is pure p-c...

Embodiment 2

[0030] The experimental device and operation are the same as in Example 1, except that anhydrous oxalic acid is replaced by dihydrate oxalic acid, and the molar amount of dihydrate oxalic acid added remains unchanged.

Embodiment 3

[0032] The experimental device and operation are the same as in Example 1, only the purification step is changed: the purification solvent is a mixture of toluene-methanol. Wherein the content of methanol is 2%, the amount of purification solvent is 1.5 times of the crude p-cresol-oxalic acid complex, and the filtration temperature is 0°C.

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Abstract

The invention discloses a method for separation and purification of p-cresol. The method comprises the following steps: 1) complexation: adding toluene and a complexing agent of oxalic acid into a reaction kettle, heating, adding mixed cresol, insulating for reaction, and filtering to obtain a cresol- oxalic acid complex crude product; 2) purification: adding the p-cresol-oxalic acid complex crude product into a purification solvent, stirring and filtering to obtain a p-cresol-oxalic acid complex; 3) decomplexation: adding the p-cresol-oxalate complex into water, insulating for reaction, separating an upper organic phase while hot, extracting the lower aqueous phase by toluene, and merging the extraction liquid into the upper organic phase; and 4) distillation: distilling the upper organic phase to remove solvent so as to obtain p-cresol. Compared with the prior art, a purification step is added to ensure that the final isolated p-cresol has purity of no less than 99%; the amount of organic solvents is reduced, the complexation step employs water, and the organic solvent and water involved in the separation process can be used indiscriminately, thereby saving cost.

Description

technical field [0001] The invention relates to a method for separating industrial p-cresol and m-cresol mixture, in particular to a method for obtaining p-cresol by purifying the industrial p-cresol and m-cresol mixture by selective complexation separation method. Background technique [0002] Phenol and methanol carry out the methylation reaction of phenol under the action of a solid catalyst, and the product is mixed cresol, which mainly contains o-cresol, p-cresol and m-cresol, and a small amount of xylenol. The development of the chemical industry and the development of new products put forward higher requirements for the purity of p-cresol. O-cresol can be separated by rectification, and the residual mother liquor includes p-cresol, m-cresol and a small amount of xylenol. Because the difference between m / p-cresol boiling points at atmospheric pressure is less than 1.0°C, it is difficult to separate them by rectification. At present, the separation methods of m / p-cres...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C39/07C07C37/68C07C37/86
CPCC07C37/685C07C39/07
Inventor 杜成堂施波屈良端庄东青葛芳荪
Owner 江苏富比亚化学品有限公司
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