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High-pressure fixed bed alkylation method for mixed m-cresol and p-cresol

A technology of p-cresol and fixed bed is applied in the field of separation of p-cresol between mixed materials, which can solve the problems of low utilization rate of raw materials, long reaction time, subsequent separation of unfavorable products, etc. Conversion rate boost

Inactive Publication Date: 2017-06-13
HEBEI UNIV OF TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The object of the present invention is to aim at the defect that in the current mixed p-cresol alkylation reaction, the alkylation reaction time is too long, the utilization rate of raw materials is not high, and it is not conducive to the subsequent separation of products, and a high-pressure p-cresol mixture is adopted A fixed-bed alkylation reaction method, which uses a mixed solution of isobutene as the alkylating agent for the reaction

Method used

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  • High-pressure fixed bed alkylation method for mixed m-cresol and p-cresol
  • High-pressure fixed bed alkylation method for mixed m-cresol and p-cresol
  • High-pressure fixed bed alkylation method for mixed m-cresol and p-cresol

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Alkylation agent composition: butane volume content 70% isobutene content 30%;

[0040] Fixed bed reactor operating pressure: 1.7MPa;

[0041] Fixed bed reactor operating temperature: 50°C

[0042] Airspeed: 0.1h -1

[0043] Molar ratio isobutylene: mixed phenol = 0.5:1

[0044] Mass fraction of p-cresol: 10%

[0045] 100ml of catalyst is filled in a single-stage fixed-bed reactor with an inner diameter of 25mm and a height of 400mm;

[0046] The first step: the determination of each flow

[0047] Because the space velocity of the fixed bed reactor is 0.1h -1 , the amount of catalyst is 100ml, according to the formula

[0048]

[0049] Where V is the catalyst volume, τ is the space velocity, a is the molar ratio of enphenol, b is the volume fraction of isobutene, M 1 and ρ 1 is the molar mass and density of isobutene, M 2 and ρ 2 is the molar mass and density of cresol, V 1 is the volume flow rate of isobutene, V 2 Be the volume flow of mixing p-cresol; (f...

Embodiment 2

[0054] Alkylating agent composition: butane content 80% isobutene content 20%

[0055] Fixed bed reactor operating pressure: 4.2MPa

[0056] Fixed bed reactor operating temperature: 70°C

[0057] Airspeed: 4.2h -1

[0058] Enol molar ratio: 2:1

[0059] Mass fraction of p-cresol: 50%

[0060] Reactor used and catalyst loading are the same as embodiment one

[0061] The first step: the determination of each flow

[0062] Because the space velocity of the fixed bed reactor is 4.2h -1 , the amount of catalyst is 100ml, calculated by the formula in Example 1, the flow rate of mixed phenol is 46.33ml / h, the flow rate of isobutene is 74.73ml / h, the flow rate of butane is 298.94ml / h, and the flow rate of isobutane and propane is 0;

[0063] The second step: Alkylation reaction

[0064] Adjust the parameters of each flowmeter according to the above calculation results, and at the same time pressurize and liquefy the isobutylene and additives separately and mix them fully, inje...

Embodiment 3

[0066] Alkylating agent composition: butane content 90% isobutene content 10%

[0067] Fixed bed reactor reaction pressure: 4.2MPa

[0068] Fixed bed reactor operating temperature: 110°C

[0069] Airspeed: 5h -1

[0070] Enol molar ratio: 3:1

[0071] Mass fraction of p-cresol: 90%

[0072] Reactor used and catalyst loading are the same as embodiment one

[0073] The first step: the determination of each flow

[0074] Because the fixed bed reactor space velocity is 5h -1 , the amount of catalyst is 100ml, calculated by the formula in Example 1, the flow rate of mixed phenol is 19.85ml / h, the flow rate of isobutene is 48.02ml / h, the flow rate of butane is 432.13ml / h, and the flow rate of isobutane and propane is 0;

[0075] The second step: Alkylation reaction

[0076] Adjust the parameters of each flowmeter according to the above calculation results, and at the same time pressurize and liquefy the isobutylene and additives separately and mix them fully, inject them tog...

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Abstract

The invention discloses a high-pressure fixed bed alkylation method for mixed m-cresol and p-cresol. The method comprises the following steps: pressurizing and liquefying alkylating agents, injecting the alkylating agents and mixed cresol into a reactor, maintaining the pressure of a fixed bed reactor to be 1.7-4.2MPa at the temperature of 50-110 DEG C, reacting under the space velocity of 0.1-5h<-1>, thereby obtaining a self-polymerized product of isobutene, mono-tert-butyl products of m-cresol and p-cresol and di-tert-butyl products of m-cresol and p-cresol, wherein the reactor is the fixed bed reactor; the alkylating agents refer to isobutene and aids; the volume of the aids accounts for 70-90% of the total volume of the alkylating agents; and a molar ratio of the isobutene to the mixed m-cresol and p-cresol is (0.5-3):1. According to the method disclosed by the invention, the utilization efficiency of the raw materials is improved, the conversion rate of the m-cresol in the method can reach 94.22%, and the conversion rate of the p-cresol can reach 89.46%.

Description

technical field [0001] The present invention relates to the separation of p-cresol in a mixing room and the technical field thereof. Specifically, it utilizes an isobutene mixed solution in the high-pressure fixed-bed alkylation reaction of p-cresol in a mixing room to effectively control the reaction temperature and make the reaction efficient and continuous. conduct. Background technique [0002] The separation of m-p-cresol by alkylation method has been paid more and more attention by various scientific research departments due to the advantages of low comprehensive cost and good product quality, and the alkylation reaction of mixed m-p-cresol and isobutene to obtain the self-polymerization product of isobutene, m- The mono-tert-butyl product of p-cresol and the di-tert-butyl product of m-p-cresol are an important process in the mixed m-p-cresol alkylation separation process, but at present, such experiments in China only exist in the laboratory stage , and the batch rea...

Claims

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Application Information

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IPC IPC(8): C07C39/06C07C37/14C10G50/00
CPCC07C37/14C10G50/00C07C39/06
Inventor 吕建华刘志远高姗姗李品
Owner HEBEI UNIV OF TECH
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