CN104892375A - Removal method for purifying ethelene glycol monophenyl ether - Google Patents
Removal method for purifying ethelene glycol monophenyl ether Download PDFInfo
- Publication number
- CN104892375A CN104892375A CN201510325183.9A CN201510325183A CN104892375A CN 104892375 A CN104892375 A CN 104892375A CN 201510325183 A CN201510325183 A CN 201510325183A CN 104892375 A CN104892375 A CN 104892375A
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- CN
- China
- Prior art keywords
- monophenyl ether
- glycol monophenyl
- phenyl ether
- glycol phenyl
- normal temperature
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/34—Separation; Purification; Stabilisation; Use of additives
- C07C41/36—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
Abstract
The invention discloses a removal method for purifying ethelene glycol monophenyl ether. A synthesized adsorption separation material is dispersed in ethelene glycol monophenyl ether, a content control technology of diethelene glycol monophenyl ether during the refining process in the conventional ethelene glycol monophenyl ether refining production process is improved, the technical problem of control of a trace of diethelene glycol monophenyl ether is solved, and the refining and purifying processes, through which the content of diethelene glycol monophenyl ether is lower than 800 ppm being difficult to achieve through common rectificating, become simple, convenient and easy. During the production and processing processes, the cost is low, the refining energy consumption is low, the removal method is suitable for ethelene glycol monophenyl ether production enterprises to use traditional equipment and traditional technical conditions, and a high-quality ethelene glycol monophenyl ether product is obtained.
Description
Technical field
The present invention relates to a kind of minimizing technology of purification of glycol phenylate.
Background technology
Current domestic ethylene glycol phenyl ether synthetic method generally all adopts propylene oxide and diethylene glycol phenyl ether directly to catalyze and synthesize acquisition.Use this synthetic method, can there is micro-diethylene glycol phenyl ether impurity unavoidably, the industrial processing method for reducing micro-diethylene glycol phenyl ether mainly uses the method for rectification under vacuum, removes the diethylene glycol phenyl ether in ethylene glycol phenyl ether as much as possible.In common first grade ethylene glycol phenyl ether, diethylene glycol phenyl ether content requirement is 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 diethylene glycol phenyl ether content micro-in ethylene glycol phenyl ether 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 diethylene glycol phenyl ether content problem in ethylene glycol phenyl ether product.
The object of the invention is to realize as follows: a kind of minimizing technology of purification of glycol phenylate, use the process such as dispersion grade in ethylene glycol phenyl ether of the adsorption and separation material (A) of synthesis.
The scheme more optimized is, the minimizing technology of above-mentioned a kind of purification of glycol phenylate, and the adsorption and separation material (A) of synthesis comprises:
(1) use the HPMC of gelling temp more than 80 DEG C, use deionized water at normal temperature to be configured to 0.05% macromolecular solution.Fineness being less than 700 object calcium carbonate is dispersed in this macromolecular solution, and the consumption of calcium carbonate is 10% of deionized water consumption;
(2) 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;
(3) 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 50-65 DEG C, be namely incubated aging 4 hours when temperature reaches 75 DEG C;
(4) 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 11-12 hour under not higher than 130 DEG C of conditions will be filtered.
Advantage of the present invention: the control techniques of the present invention to the diethylene glycol phenyl ether content in existing ethylene glycol phenyl ether production technique treating process is improved, solve the control techniques problem of micro-diethylene glycol phenyl ether, make the diethylene glycol phenyl ether 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 minimizing technology for purification of glycol phenylate, uses the dispersion in ethylene glycol phenyl ether of the adsorption and separation material (A) of synthesis to wait process.The adsorption and separation material (A) wherein synthesized comprising:
(1) use the HPMC of gelling temp more than 80 DEG C, use deionized water at normal temperature to be configured to 0.05% macromolecular solution.Fineness being less than 700 object calcium carbonate is dispersed in this macromolecular solution, and the consumption of calcium carbonate is 10% of deionized water consumption;
(2) 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;
(3) 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 50-65 DEG C, be namely incubated aging 4 hours when temperature reaches 75 DEG C;
(4) 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 11-12 hour under not higher than 130 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 |
| Calcium carbonate % | 7％ | |
| Aluminum isopropylate concentration | 1.5％ | |
| 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 1% 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 diethylene glycol phenyl ether enrichment in ethylene glycol phenyl ether out.
| Diethylene glycol phenyl ether content before fractionation by adsorption | Diethylene glycol phenyl ether content after process |
| 0.3％ | 600ppm |
Implement example 2
A adsorption separating agent preparation technology
Starting material and control condition:
| Control condition | Reference mark | Remarks |
| Calcium carbonate % | 7％ | |
| Aluminum isopropylate concentration | 3％ | |
| 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 3.5% quality, disperse stirring under normal temperature 5 hours, the method for rear employing precipitate and separate separates out solid absorption parting material, can by the diethylene glycol phenyl ether enrichment in ethylene glycol phenyl ether out.
| Diethylene glycol phenyl ether content before fractionation by adsorption | Diethylene glycol phenyl ether content after process |
| 0.2％ | 280ppm |
The solid absorption parting material of enrichment diethylene glycol phenyl ether, 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, diethylene glycol phenyl ether ability is as follows:
Implement example 3
A adsorption separating agent preparation technology
Starting material and control condition:
| Control condition | Reference mark | Remarks |
| Calcium carbonate % | 3％ | Concentration after deionized water dilution |
| 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 2.0% 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 diethylene glycol phenyl ether enrichment in ethylene glycol phenyl ether out.
| Diethylene glycol phenyl ether content before fractionation by adsorption | Diethylene glycol phenyl ether content after process |
| 0.3％ | 530ppm |
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 (2)
1. a minimizing technology for purification of glycol phenylate, is characterized in that: use the dispersion in ethylene glycol phenyl ether of the adsorption and separation material (A) of synthesis to wait process.
2. the minimizing technology of a kind of purification of glycol phenylate according to claim 1, is characterized in that: the adsorption and separation material (A) of synthesis comprises:
(1) use the HPMC of gelling temp more than 80 DEG C, use deionized water at normal temperature to be configured to 0.05% macromolecular solution.Fineness being less than 700 object calcium carbonate is dispersed in this macromolecular solution, and the consumption of calcium carbonate is 10% of deionized water consumption;
(2) 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;
(3) 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 50-65 DEG C, be namely incubated aging 4 hours when temperature reaches 75 DEG C;
(4) 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 11-12 hour under not higher than 130 DEG C of conditions will be filtered.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510325183.9A CN104892375A (en) | 2015-06-15 | 2015-06-15 | Removal method for purifying ethelene glycol monophenyl ether |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510325183.9A CN104892375A (en) | 2015-06-15 | 2015-06-15 | Removal method for purifying ethelene glycol monophenyl ether |
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| CN104892375A true CN104892375A (en) | 2015-09-09 |
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| CN201510325183.9A Pending CN104892375A (en) | 2015-06-15 | 2015-06-15 | Removal method for purifying ethelene glycol monophenyl ether |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110642706A (en) * | 2019-10-08 | 2020-01-03 | 江苏东南纳米材料有限公司 | Preparation method of high-purity phenoxyethanol |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104355971A (en) * | 2014-10-11 | 2015-02-18 | 江苏常州酞青新材料科技有限公司 | Method for removing diethylene glycol phenyl ether in ethylene glycol phenyl ether refining process |
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- 2015-06-15 CN CN201510325183.9A patent/CN104892375A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104355971A (en) * | 2014-10-11 | 2015-02-18 | 江苏常州酞青新材料科技有限公司 | Method for removing diethylene glycol phenyl ether in ethylene glycol phenyl ether refining process |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110642706A (en) * | 2019-10-08 | 2020-01-03 | 江苏东南纳米材料有限公司 | Preparation method of high-purity phenoxyethanol |
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Application publication date: 20150909 |