Method for separating m-cresol and p-cresol mixture by liquid-phase alkylation method

An alkylation method and p-cresol technology, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as high production costs, polluting the environment, low utilization rate of alkylating agents, etc., and achieve improvement Effect of conversion rate, reduction of environment, and improvement of throughput

Inactive Publication Date: 2017-06-09
HEBEI UNIV OF TECH +1
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  • Abstract
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  • Claims
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AI Technical Summary

Problems solved by technology

The method utilizes isobutene mixed gas and m-p-cresol mixture to undergo alkylation reaction in liquid phase at the same time and separate m-cresol and p-cresol. The mixture is used as a raw material, and the pure products of m-cresol and p-cresol are obtained through liquid-phase alkylation reaction and separation, which overcomes the shortcomings of low utilization rate of alkylating agent and serious environmental pollution in gas-phase alkylation reaction in the prior art, and at the same time Solved the defect of high production cost caused by the use of high-purity isobutene as the alkylating agent in the gas-phase alkylation reaction

Method used

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  • Method for separating m-cresol and p-cresol mixture by liquid-phase alkylation method
  • Method for separating m-cresol and p-cresol mixture by liquid-phase alkylation method
  • Method for separating m-cresol and p-cresol mixture by liquid-phase alkylation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Inner diameter 20mm, high 400mm tubular fixed-bed reactor is filled with 100ml of Amberlyst 15 type ion exchange resin, this catalyst is a known product, sold by Rohm and Haas China.

[0037] Step 1: Alkylation Process

[0038] Alkylating agent (volume ratio): 10% isobutene, 20% isobutane, 20% butane, 30% propane;

[0039] Mixed phenols (mass ratio): m-cresol 10%, p-cresol 90%;

[0040] Turn on the alkylating agent pump 1 and keep the pressure, the pressure keeping condition is 1.7MPa, and the space velocity is 0.8h -1 , adjust the temperature of the fixed bed reactor 3 to 50°C, turn on the mixed phenol pump 2, and feed the phenol at a molar ratio of 0.5:1 to carry out the alkylation reaction, and the product tank 5 obtains the alkylated product. The alkylation product that obtains is carried out GC-MS analysis, the result shows: p-cresol accounts for 68.24%, m-cresol accounts for 8.28%, 4-tert-butyl p-cresol accounts for 16.53%, 6-tert-butyl m-cresol accounted for 2...

Embodiment example 2

[0047] Reactor used and catalyzer and its consumption are with embodiment case one.

[0048] Step 1: Alkylation Process

[0049] Alkylating agent (volume ratio): isobutene 15%, isobutane 30%, butane 25%, propane 30%;

[0050] Mixed phenols (mass ratio): m-cresol 50%, p-cresol 50%;

[0051] Turn on the alkylating agent pump 1 and keep the pressure, the pressure keeping condition is 2.3MPa, and the space velocity is 1.5h -1 , adjust the temperature of the fixed bed reactor 3 to 70°C, turn on the mixed phenol pump 2, and feed the alkenyl phenol at a molar ratio of 1:1 to carry out the alkylation reaction, and the product tank 5 obtains the alkylated product. The obtained alkylated product was analyzed by GC-MS, and the results are shown in Table 1.

[0052] Step Two: Separation Process

[0053] The obtained alkylation product enters the atmospheric pressure tower 6, and the isobutene self-polymerization product is separated at the top of the tower, and the tower bottom liquid...

Embodiment 3

[0058] The reactor, catalyst and mixed phenol composition used are the same as those in Example 1.

[0059] Step 1: Alkylation Process

[0060] Alkylating agent (volume ratio): 20% isobutene, 30% isobutane, 25% butane, 25% propane;

[0061] Mixed phenols (mass ratio): m-cresol 50%, p-cresol 50%;

[0062] Turn on the alkylating agent pump 1 and keep the pressure, the pressure keeping condition is 2.8MPa, and the space velocity is 2.5h -1 , adjust the temperature of the fixed bed reactor 3 to 85°C, turn on the mixed phenol pump 2, and feed the phenol at a molar ratio of 1.5:1 to carry out the alkylation reaction, and the product tank 5 obtains the alkylated product. The obtained alkylated product was analyzed by GC-MS, and the results are shown in Table 1.

[0063] Step Two: Separation Process

[0064] The obtained alkylation product enters the atmospheric pressure tower 6, and the isobutene self-polymerization product is separated at the top of the tower, and the tower bott...

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Abstract

The invention discloses a method for separating an m-cresol and p-cresol mixture by a liquid-phase alkylation method. According to the method, alkylation reaction between isobutene mixed gas and the m-cresol and p-cresol mixture are performed through a fixed-bed reactor under the liquid phase state, the reacted mixture is separated to obtain metacresol and paracresol, the isobutene mixed gas serves as an alkylating agent, the m-cresol and p-cresol mixture serves as a raw material, the alkylation reaction is performed for the alkylating agent and the m-cresol and p-cresol mixture, and the treated mixture is separated to obtain pure metacresol and pure paracresol. The method overcomes the shortcomings of low utilization rate and serious environmental pollution of alkylating agents in gas-phase alkylation reaction in the prior art and solves the problems that production cost is high as high-purity isobutene serves as the alkylating agent in the gas-phase alkylation reaction.

Description

technical field [0001] The present invention relates to a method for separating m-cresol by liquid-phase alkylation method, specifically, liquid-phase alkylation simultaneously separates m-cresol and a mixture of p-cresol, thereby obtaining high-purity m-cresol and p-cresol p-cresol belongs to the field of separation and purification of chemical products. Background technique [0002] Cresol is a widely used organic chemical intermediate. Among them, p-cresol can be used in industrial sectors such as pesticides, dyes, plastics, and medicine. m-cresol is an important raw material for the synthesis of organic intermediates, and also has important applications in color film developers, synthetic resins, and adhesives. Therefore, high-purity m-p-cresol has a good market prospect and great development potential, and has an extremely important impact on the development of my country's economy and chemical industry. But so far, although a lot of work on the separation of m-p-cre...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C37/50C07C39/07
CPCC07C37/50C07C37/14C07C37/70C07C37/74C07C39/07C07C39/06
Inventor 吕建华高姗姗刘志远李品
Owner HEBEI UNIV OF TECH
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