CN104892376A - Method for removing phenol during refining process of ethylene glycol phenyl ether - Google Patents

Abstract

The invention discloses a method for removing phenol during the refining process of ethylene glycol phenyl ether. Phenol in the ethylene glycol phenyl ether is gathered through the treatment procedures of dispersing a synthesized adsorption separation material in the ethylene glycol phenyl ether, and the like, so that the original high content of the phenol in the ethylene glycol phenyl ether is reduced. According to the invention, the conventional controlling technology for the phenol content during the refining process of the production technology of the ethylene glycol phenyl ether is improved, and the problem about the control technology for trace phenol is solved, so that the refining purification process for obtaining the phenol with the content of lower than 800 ppm, which is difficult to obtain through conventional distillation, becomes simple, convenient and feasible; the production process cost is low, the refining energy consumption is low, and the method is suitable for ethylene glycol phenyl ether production enterprises to utilize existing equipment and technical conditions to obtain high-quality ethylene glycol phenyl ether products.

Description

The minimizing technology of phenol in a kind of ethylene glycol phenyl ether treating process

Technical field

The present invention relates to the minimizing technology of phenol in a kind of ethylene glycol phenyl ether treating process.

Background technology

Current domestic ethylene glycol phenyl ether synthetic method generally all adopts oxyethane and phenol directly to catalyze and synthesize acquisition.Use this synthetic method, can there is trace phenol impurity unavoidably, the industrial processing method for reducing trace phenol mainly uses the method for rectification under vacuum, removes the phenol in ethylene glycol phenyl ether as much as possible.In common first grade ethylene glycol phenyl ether, phenol content requires lower than 0.1%, and adopt common rectification under vacuum method, not only energy consumption is high, and also higher to manufacturing requirements.For solving this technical barrier, domestic many ethylene glycol phenyl ether manufacturing enterprises have all dropped into a lot of technical study strength, but because in ethylene glycol phenyl ether, trace phenol content reduces further, difficulty is comparatively large, perplexs the product quality problem of domestic ethylene glycol phenyl ether manufacturing enterprise always.

Summary of the invention

The present invention solves the technical problem in above-mentioned background technology, providing a kind of technical scheme adopting fractionation by adsorption, proposing solution easily for thoroughly solving phenol content problem in ethylene glycol phenyl ether product.The object of the invention is to realize as follows: a kind of preparation method of ethylene glycol phenyl ether essence, (1) dispersion in ethylene glycol phenyl ether of the adsorption and separation material (A) of synthesis is used to wait process, phenol (B) in enrichment ethylene glycol phenyl ether, makes the ethylene glycol phenyl ether of former high-content phenol be reduced;

(2) adsorption and separation material (A) synthesized comprising: use the HPMC of gelling temp more than 75 DEG C, uses deionized water at normal temperature to be configured to 0.06% macromolecular solution.Fineness being less than 600 object calcium carbonate is dispersed in this macromolecular solution, and the consumption of calcium carbonate is the 5-9% of deionized water consumption;

(3) functional quality concentration is not higher than the aqueous isopropanol of 7% aluminum isopropylate, joins in aforementioned colloidal sol under normal temperature with the ratio of aluminum isopropylate and calcium carbonate equimolar amount;

(4) after aluminum isopropylate has added, this mixed system is no more than 1.5 DEG C with per minute from normal temperature and is slowly warmed up to 60-65 DEG C, be namely incubated aging 3 hours when temperature reaches 65 DEG C;

(5) after aging end, adopt intensification gel, filter, the impurity such as method removing Virahol wherein such as deionized water at normal temperature washing.The solid material that obtains dry 10-12 hour under not higher than 140 DEG C of conditions will be filtered.

Advantage of the present invention: the control techniques of the present invention to the phenol content in existing ethylene glycol phenyl ether production technique treating process is improved, solve the control techniques problem of trace phenol, make the phenol content being difficult to obtain by conventional distillation become simple and easy to do lower than the polishing purification process of 800ppm.Process of manufacture is with low cost, and refining energy consumption is low, is applicable to ethylene glycol phenyl ether manufacturing enterprise and utilizes existing installation and technical qualification, obtain high-quality ethylene glycol phenyl ether product.

Embodiment:

A kind of preparation method of ethylene glycol phenyl ether essence, (1) dispersion in ethylene glycol phenyl ether of the adsorption and separation material (A) of synthesis is used to wait process, phenol (B) in enrichment ethylene glycol phenyl ether, makes the ethylene glycol phenyl ether of former high-content phenol be reduced;

(2) adsorption and separation material (A) synthesized comprising: use the HPMC of gelling temp more than 75 DEG C, uses deionized water at normal temperature to be configured to 0.06% macromolecular solution.Fineness being less than 600 object calcium carbonate is dispersed in this macromolecular solution, and the consumption of calcium carbonate is the 5-9% of deionized water consumption;

(3) functional quality concentration is not higher than the aqueous isopropanol of 7% aluminum isopropylate, joins in aforementioned colloidal sol under normal temperature with the ratio of aluminum isopropylate and calcium carbonate equimolar amount;

(4) after aluminum isopropylate has added, this mixed system is no more than 1.5 DEG C with per minute from normal temperature and is slowly warmed up to 60-65 DEG C, be namely incubated aging 3 hours when temperature reaches 65 DEG C;

(5) after aging end, adopt intensification gel, filter, the impurity such as method removing Virahol wherein such as deionized water at normal temperature washing.The solid material that obtains dry 10-12 hour under not higher than 140 DEG C of conditions will be filtered.

Implement example 1

A adsorption separating agent preparation technology

Starting material and control condition:

Control condition	Reference mark	Remarks
			Water glass weaker concn %	15％	Concentration after deionized water dilution
PH after acidifying with acetic acid	7.0
			Aluminum isopropylate concentration	5％
Heat-up rate DEG C/min	0.5

Drying temperature DEG C

125

B fractionation by adsorption operates

Take ethylene glycol phenyl ether as benchmark, drop into the solid absorption parting material of ethylene glycol phenyl ether quality 0.5% quality, disperse stirring under normal temperature 1 hour, the method for rear employing precipitate and separate separates out solid absorption parting material, can by the phenol rich in ethylene glycol phenyl ether out.

Phenol content before fractionation by adsorption	Phenol content after process
		0.15％	480ppm

Implement example 2

A adsorption separating agent preparation technology

Starting material and control condition:

Control condition	Reference mark	Remarks
			Water glass weaker concn %	18％	Concentration after deionized water dilution
PH after acidifying with acetic acid	6.5
			Aluminum isopropylate concentration	8％
Heat-up rate DEG C/min	1.5
			Drying temperature DEG C	140

B fractionation by adsorption operates

Take ethylene glycol phenyl ether as benchmark, drop into the solid absorption parting material of ethylene glycol phenyl ether quality 1% quality, disperse stirring 5 hours under normal temperature, the method for rear employing precipitate and separate separates out solid absorption parting material, can by the phenol rich in ethylene glycol phenyl ether out.

Phenol content before fractionation by adsorption	Phenol content after process
		0.1％	80ppm

The solid absorption parting material of enrichment phenol, the dry toluene washing 2-3 time of the quality such as use, after seasoning, drying 2 hours at 140 DEG C, in its process ethylene glycol phenyl ether, phenol ability is as follows:

Reuse number of times	Phenol content in original ethylene glycol phenyl ether	Phenol content after process
			1	0.1％	81ppm
5	0.1％	84ppm
			6	0.1％	82ppm
7	0.1％	83ppm
			8	0.1％	86ppm
9	0.1％	85ppm
			10	0.1％	84ppm
11	0.1％	88ppm
			12	0.1％	86ppm
13	0.1％	90ppm
			14	0.1％	150ppm
15	0.1％	240ppm

Implement example 3

A adsorption separating agent preparation technology

Starting material and control condition:

Control condition	Reference mark	Remarks
			Water glass weaker concn %	10％	Concentration after deionized water dilution
PH after acidifying with acetic acid	7.5
			Aluminum isopropylate concentration	2.5％
Heat-up rate DEG C/min	1.0
			Drying temperature DEG C	135

B fractionation by adsorption operates

Take ethylene glycol phenyl ether as benchmark, drop into the solid absorption parting material of ethylene glycol phenyl ether quality 2.5% quality, disperse stirring under normal temperature 3 hours, the method for rear employing precipitate and separate separates out solid absorption parting material, can by the phenol rich in ethylene glycol phenyl ether out.

Phenol content before fractionation by adsorption	Phenol content after process
		0.2％	220ppm

Above-described specific embodiment; object of the present invention, technical scheme and beneficial effect are further described; be understood that; the foregoing is only specific embodiments of the invention; be not limited to the present invention; within the spirit and principles in the present invention all, any amendment made, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.

Claims (1)

1. the preparation method of an ethylene glycol phenyl ether essence, it is characterized in that: (1) uses the dispersion in ethylene glycol phenyl ether of the adsorption and separation material (A) of synthesis to wait process, phenol (B) in enrichment ethylene glycol phenyl ether, makes the ethylene glycol phenyl ether of former high-content phenol be reduced;

(2) adsorption and separation material (A) synthesized comprising: use the HPMC of gelling temp more than 75 DEG C, uses deionized water at normal temperature to be configured to 0.06% macromolecular solution.Fineness being less than 600 object calcium carbonate is dispersed in this macromolecular solution, and the consumption of calcium carbonate is the 5-9% of deionized water consumption;

(3) functional quality concentration is not higher than the aqueous isopropanol of 7% aluminum isopropylate, joins in aforementioned colloidal sol under normal temperature with the ratio of aluminum isopropylate and calcium carbonate equimolar amount;

(4) after aluminum isopropylate has added, this mixed system is no more than 1.5 DEG C with per minute from normal temperature and is slowly warmed up to 60-65 DEG C, be namely incubated aging 3 hours when temperature reaches 65 DEG C;

(5) after aging end, adopt intensification gel, filter, the impurity such as method removing Virahol wherein such as deionized water at normal temperature washing.The solid material that obtains dry 10-12 hour under not higher than 140 DEG C of conditions will be filtered.