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Method for refining phenol by acid-treated aluminium cross-linked montmorillonite catalyst

A montmorillonite and catalyst technology, which is applied in the field of phenol purification, can solve the problems of undetermined product impurity composition, limited adsorption and catalytic performance, and small number of active sites, so as to increase the interlayer spacing and porosity of montmorillonite , many active sites, simple preparation process

Inactive Publication Date: 2009-11-11
BEIJING UNIV OF CHEM TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] Li Shufen et al. ("research on refining phenol by activated clay method, chemical engineering, 2002, 30 (1), 72-76.") reported that the use of granular activated clay as a catalyst can significantly reduce the content of ketone impurities in phenol and improve the sulfuric acid coloring rate ( UVT), the main component of its catalyst is montmorillonite activated by sulfuric acid, but the acidity is weak, the number of active sites is small, the adsorption and catalytic performance is limited, and the product must be further rectified to obtain high-quality phenol, the final product specific Impurity composition also could not be determined

Method used

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  • Method for refining phenol by acid-treated aluminium cross-linked montmorillonite catalyst

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Experimental program
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Effect test

Embodiment 1

[0023] Embodiment 1: Preparation of acidified aluminum crosslinked montmorillonite catalyst

[0024] (1) Prepare montmorillonite solution: acidify sodium-based montmorillonite with sulfuric acid with a mass concentration of 15% at 80° C., stir for 5 hours, and use deionized water to make the acidified sodium-based montmorillonite into a concentration of 5% wt The montmorillonite slurry;

[0025] (2) Preparation of aluminum crosslinking agent: Take 1.0 mol / L sodium hydroxide solution and add dropwise at a rate of 10 ml / min to a concentration of 0.5 mol / L aluminum trichloride solution, add dropwise at a constant temperature of 60°C and stir vigorously, then Aging at 70°C for more than 10 hours to prepare the aluminum crosslinking agent.

[0026] (3) Acidified aluminum cross-linked montmorillonite: drop an equal volume of aluminum cross-linking agent solution into the montmorillonite slurry at a rate of 5.0ml / min, stir for 4 hours, let stand, filter with a vacuum pump, and wash ...

Embodiment 2

[0030] Example 2: The acidified aluminum cross-linked montmorillonite catalyst prepared in Example 1-A was added to a three-necked flask containing molten raw material phenol at a volume ratio of 4%, and reacted at 120° C. for 2 hours under nitrogen protection. After the reaction stopped, A syringe with a strainer was used to suck out the phenol, and the product was analyzed for impurity content by gas chromatography after simple distillation. (See Table 3)

[0031] table 3

[0032]

Embodiment 3

[0033] Embodiment 3 (acidified aluminum cross-linked montmorillonite continuous reaction process refining phenol)

[0034] Continuous reaction test adopts fixed-bed reactor, and the aluminum cross-linked montmorillonite catalyst (20~40) of 20ml acidification prepared in embodiment 1-B is housed in the reactor, and upstream raw material phenol directly enters catalyst bed layer without heat exchange, The reaction temperature is controlled at 150°C, and the volumetric space velocity of the phenol material is 1.0h -1 , the pressure is 1.0MPa. After the reaction was carried out for 1 day, the refined phenol product was analyzed for impurity content by gas chromatography. (See Table 4)

[0035] Table 4

[0036]

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Abstract

The invention provides a method for refining phenol by an acid-treated aluminium cross-linked montmorillonite catalyst, which comprises the following steps: acidizing Na-montmorillonite by sulfuric acid to obtain montmorillonite slurry; preparing an aluminium cross linking agent from aluminium choride; dripping the aluminium cross linking agent solution in the same volume into the montmorillonite slurry to prepare the acid-treated aluminium cross-linked montmorillonit catalyst; and intermittently or continuously catalyzing and refining the raw material phenol by the acid-treated aluminium cross-linked montmorillonite catalyst. The method of the invention adopts the acid-treated aluminium cross-linked montmorillonite catalyst which has B acid and L acid centers, multiple active spots, strong acidity, can effectively remove impurities such as acetol, mesityl oxide and the like, simultaneously can reduce contents of methylbenzofuran impurities, and has wide applicable raw material range.

Description

technical field [0001] The invention relates to a method for refining phenol, in particular to a method for purifying phenol through an acidified aluminum crosslinked montmorillonite catalyst process. It can be used to prepare high-purity and ultra-high-purity phenol required by bisphenol A. Background technique [0002] At present, 90% of phenol in the world is produced by cumene method. The production of phenol by the cumene method uses cumene as a raw material. First, cumene hydroperoxide is generated through air oxidation. Under the action of an acidic catalyst, it is decomposed to generate phenol and acetone, and the decomposition products are obtained through rectification. Many side reactions occur in the oxidation and decomposition reactions, and the impurities generated by these side reactions bring great difficulties to the purification of phenol. It is difficult to remove organic impurities by general rectification method, and only phenol with resin grade purity...

Claims

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Application Information

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IPC IPC(8): C07C39/04C07C37/68B01J21/16B01J21/04
CPCY02P20/52
Inventor 李英霞胡雪生陈标华
Owner BEIJING UNIV OF CHEM TECH
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