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Method for adsorbing and separating p-cresol and m-cresol

An adsorption separation and p-cresol technology, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as difficult separation, and achieve the effect of improving the efficiency of adsorption and separation

Active Publication Date: 2020-09-22
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The boiling point difference between o-cresol, m-cresol and p-cresol is relatively large (greater than 10°C), and it is usually separated by rectification; but the boiling point of m-cresol and p-cresol is very close, and the boiling point difference is less than 1°C. Therefore, it is difficult to separate the two using conventional distillation methods.

Method used

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  • Method for adsorbing and separating p-cresol and m-cresol

Examples

Experimental program
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preparation example Construction

[0023] In the method of the present invention, the preparation method of described adsorbent comprises the steps:

[0024] (1) Mix NaX or NaY molecular sieve and binder at a mass ratio of 90-95:5-10, add molding aids and mix evenly, and spray the mixed powder into water while rolling to make a diameter of 0.1mm-1.2 mm pellets, then dried at 60-120°C for 2-24 hours, and then fired at 500-560°C for 4-10 hours.

[0025] (2) The above-mentioned calcined pellets are treated with an aqueous solution of NaOH and sodium silicate, or an aqueous solution of NaOH is used for alkali treatment at 80-120°C, and the basic pellets are obtained after drying,

[0026] (3) For the basic pellet containing X molecular sieve, use a solution containing soluble barium salt and potassium salt, or carry out cation exchange with a soluble barium salt solution, and make BaKX or BaX adsorbent after activation; for the basic pellet containing Y molecular sieve The spheres are exchanged with a potassium sa...

example 1

[0034] The following example prepares the adsorbent.

[0035]Mix 9.4kg of NaX molecular sieve with a molar ratio of silica / alumina of 2.3, 0.6kg of kaolin and 0.2kg of cornstarch, put them into a sugar coating pan, and spray 2.2kg of water rolling balls while rolling to form a ball with a diameter of 0.3 mm ~ 0.8mm pellets, then dried at 100°C for 4 hours, and then fired at 540°C for 6 hours.

[0036] Soak the above roasted pellets in 20 liters of aqueous solution containing NaOH and sodium silicate at 98°C for alkali treatment for 5 hours, so that kaolin can be crystallized into X molecular sieves in situ. The concentration of NaOH in the solution used for alkali treatment is 1.5mol / L, SiO 2 The concentration is 10 g / L, and the alkali-treated pellets are washed with deionized water until the pH value of the washing solution is lower than 10, to obtain basic pellets.

[0037] Put the above basic pellets in a solution containing barium chloride and potassium chloride at 90°C ...

example 2

[0039] Mix 9.2kg of NaX molecular sieve with a silica / alumina molar ratio of 2.6, 0.8kg of kaolin and 0.3kg of cornstarch, put them into a sugar coating pan, and spray 2.2kg of water rolling balls while rolling to form a ball with a diameter of 0.3 mm ~ 0.8mm pellets, then dried at 100°C for 4 hours and fired at 500°C for 6 hours.

[0040] Soak the above roasted pellets in 20 liters of aqueous solution containing NaOH and sodium silicate at 98°C for alkali treatment for 5 hours, the concentration of NaOH in the solution used for alkali treatment is 1.5mol / L, SiO 2 The concentration is 4g / L, and the alkali-treated pellets are washed with deionized water until the pH value of the washing liquid is lower than 10 to obtain basic pellets.

[0041] The above basic pellets were soaked in barium nitrate solution at 95°C for 5.5h -1 Ion exchange was carried out at a volume space velocity of 6 h until the degree of barium ion exchange was greater than 97 mol%, and then the temperature ...

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Abstract

The invention discloses a method for adsorbing and separating p-cresol and m-cresol. The method comprises the following steps: feeding a mixture of p-cresol and m-cresol into an adsorption zone of a liquid-phase simulated moving bed to be in contact with an adsorbent, wherein the p-cresol is adsorbed by the adsorbent while the m-cresol is not adsorbed; extracting the liquid as raffinate, introducing a desorption agent into the adsorbent for desorbing the adsorption components and obtaining an extract liquid; wherein the liquid-phase simulated moving bed comprises the following four functionalareas: a first functional area, a second functional area and a third functional area, a desorption zone, a purification zone, an adsorption zone and a buffer zone, the temperature of feeding an adsorption raw material into the adsorption area is 100-230 DEG C; the temperature of feeding a desorption agent into the desorption area is 120-250 DEG C; the temperature of the desorption agent introducedinto the desorption area is controlled to be 10-100 DEG C higher than the temperature of the adsorption raw material introduced into the adsorption area; the active component of the adsorbent is selected from any one of BaX, BaKX and KY molecular sieves, and the desorption agent is a mixture of 30-96% by mass of C3-C5 fatty alcohol and 4-70% by mass of C7-C9 alkane. The method is used for adsorbing and separating a mixture of p-cresol and m-cresol, and high-purity p-cresol and m-cresol products can be respectively obtained.

Description

technical field [0001] The invention relates to an adsorption separation method for p-cresol and m-cresol, in particular to a method for producing p-cresol products and m-cresol products by using liquid-phase simulated moving bed adsorption separation. Background technique [0002] Cresol is an important intermediate in fine chemical industry, and there are three isomers of o-cresol, m-cresol and p-cresol. Direct extraction from natural resources and chemical synthesis are the main ways to obtain cresol, but generally a mixture of three isomers is obtained. The boiling point difference between o-cresol, m-cresol and p-cresol is relatively large (greater than 10°C), and it is usually separated by rectification; but the boiling point of m-cresol and p-cresol is very close, and the boiling point difference is less than 1°C. Therefore, it is difficult to separate the two by conventional rectification. [0003] In fine chemical industry, when p-cresol and m-cresol are used as i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C37/82C07C39/07
CPCC07C37/82C07C39/07
Inventor 杨彦强王德华王辉国刘宇斯马剑锋王红超乔晓菲高宁宁
Owner CHINA PETROLEUM & CHEM CORP
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