CN105016985A - Preparation method for purifying propylene glycol phenyl ether - Google Patents
Preparation method for purifying propylene glycol phenyl ether Download PDFInfo
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- CN105016985A CN105016985A CN201510325285.0A CN201510325285A CN105016985A CN 105016985 A CN105016985 A CN 105016985A CN 201510325285 A CN201510325285 A CN 201510325285A CN 105016985 A CN105016985 A CN 105016985A
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- China
- Prior art keywords
- propylene glycol
- glycol phenylate
- normal temperature
- phenyl ether
- preparation
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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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
- C07C41/44—Separation; Purification; Stabilisation; Use of additives by treatments giving rise to a chemical modification
Abstract
The present invention discloses a preparation method for purifying propylene glycol phenyl ether. The method comprises: A: dispersing a synthetic adsorption and separation material C in the propylene glycol phenyl ether. The preparation method is an improvement on the control technology for the dipropylene glycol diphenyl ether content in the existing propylene glycol phenyl ether production process refining process, solves the technical problem of controlling a trace amount of dipropylene glycol diphenyl ether, and makes the refining purification process with the dipropylene glycol diphenyl ether content being less than 800 ppm unobtainable by general distillation become simple and easy. The production process is low in cost and refining power consumption, and enables propylene glycol phenyl ether production enterprises to use existing equipment and technical conditions to obtain propylene glycol phenyl ether products of high quality.
Description
Technical field
The present invention relates to a kind of preparation method purifying propylene glycol phenylate.
Background technology
Current domestic propylene glycol phenylate synthetic method generally all adopts propylene oxide and dipropylene glycol phenylate directly to catalyze and synthesize acquisition.Use this synthetic method, can there is micro-dipropylene glycol phenylate impurity unavoidably, the industrial processing method for reducing micro-dipropylene glycol phenylate mainly uses the method for rectification under vacuum, removes the dipropylene glycol phenylate in propylene glycol phenylate as much as possible.In common first grade propylene glycol phenylate, dipropylene glycol phenylate 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 propylene glycol phenylate manufacturing enterprises have all dropped into a lot of technical study strength, but because dipropylene glycol phenylate content micro-in propylene glycol phenylate reduces further, difficulty is comparatively large, perplexs the product quality problem of domestic propylene glycol phenylate 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 dipropylene glycol phenylate content problem in propylene glycol phenyl ether product.
The object of the invention is to realize as follows: a kind of preparation method purifying propylene glycol phenylate, A: use the adsorption and separation material C of synthesis process such as dispersion grade in propylene glycol phenylate
B: the adsorption and separation material C wherein synthesized comprises:
(1) deionized water at normal temperature is used to be configured to 0.07% macromolecular solution.Fineness being less than 900 object calcium carbonate is dispersed in this macromolecular solution, and the consumption of calcium carbonate is the 9-13% of deionized water consumption;
(2) functional quality concentration is not higher than the aqueous isopropanol of 4% 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 DEG C with per minute from normal temperature and is slowly warmed up to 50-75 DEG C, be namely incubated aging 3 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 11-13 hour under not higher than 130 DEG C of conditions will be filtered.
A kind of preparation method purifying propylene glycol phenylate described further, in described enrichment propylene glycol phenylate, dipropylene glycol phenylate process D directly drops under adsorption and separation material C normal temperature in propylene glycol phenylate, and its consumption is the 0.1-5% of propylene glycol phenylate quality.
Advantage of the present invention: the control techniques of the present invention to the dipropylene glycol phenylate content in existing propylene glycol phenylate production technique treating process is improved, solve the control techniques problem of micro-dipropylene glycol phenylate, make the dipropylene glycol phenylate 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 propylene glycol phenylate manufacturing enterprise and utilizes existing installation and technical qualification, obtain high-quality propylene glycol phenyl ether product.
Embodiment:
Purify a preparation method for propylene glycol phenylate, A: use the adsorption and separation material C of synthesis dispersion in propylene glycol phenylate to wait process
B: the adsorption and separation material C wherein synthesized comprises:
(1) deionized water at normal temperature is used to be configured to 0.07% macromolecular solution.Fineness being less than 900 object calcium carbonate is dispersed in this macromolecular solution, and the consumption of calcium carbonate is the 9-13% of deionized water consumption;
(2) functional quality concentration is not higher than the aqueous isopropanol of 4% 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 DEG C with per minute from normal temperature and is slowly warmed up to 50-75 DEG C, be namely incubated aging 3 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 11-13 hour under not higher than 130 DEG C of conditions will be filtered.
In described enrichment propylene glycol phenylate, dipropylene glycol phenylate process D directly drops under adsorption and separation material C normal temperature in propylene glycol phenylate, and its consumption is the 0.1-5% of propylene glycol phenylate quality.
Implement example 1
A adsorption separating agent preparation technology
Starting material and control condition:
| Control condition | Reference mark | Remarks |
| Calcium carbonate % | 5％ | |
| Aluminum isopropylate concentration | 1.5％ | |
| Heat-up rate DEG C/min | 0.5 | |
| Drying temperature DEG C | 125 |
B fractionation by adsorption operates
With propylene glycol phenylate for benchmark, drop into the solid absorption parting material of propylene glycol phenylate 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 dipropylene glycol phenylate enrichment in propylene glycol phenylate out.
| The first two propylene glycol phenyl ether content of fractionation by adsorption | Dipropylene glycol phenylate 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
With propylene glycol phenylate for benchmark, drop into the solid absorption parting material of propylene glycol phenylate 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 dipropylene glycol phenylate enrichment in propylene glycol phenylate out.
| The first two propylene glycol phenyl ether content of fractionation by adsorption | Dipropylene glycol phenylate content after process |
| 0.2％ | 280ppm |
The solid absorption parting material of enrichment dipropylene glycol phenylate, 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 propylene glycol phenylate, dipropylene glycol phenylate 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
With propylene glycol phenylate for benchmark, drop into the solid absorption parting material of propylene glycol phenylate 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 dipropylene glycol phenylate enrichment in propylene glycol phenylate out.
| The first two propylene glycol phenyl ether content of fractionation by adsorption | Dipropylene glycol phenylate content after process |
| 0.3％ | 630ppm |
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. purify a preparation method for propylene glycol phenylate, it is characterized in that: A: use the adsorption and separation material C of synthesis dispersion in propylene glycol phenylate to wait process
B: the adsorption and separation material C wherein synthesized comprises:
(1) deionized water at normal temperature is used to be configured to 0.07% macromolecular solution.Fineness being less than 900 object calcium carbonate is dispersed in this macromolecular solution, and the consumption of calcium carbonate is the 9-13% of deionized water consumption;
(2) functional quality concentration is not higher than the aqueous isopropanol of 4% 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 DEG C with per minute from normal temperature and is slowly warmed up to 50-75 DEG C, be namely incubated aging 3 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 11-13 hour under not higher than 130 DEG C of conditions will be filtered.
2. a kind of preparation method purifying propylene glycol phenylate according to claim 1, it is characterized in that: in described enrichment propylene glycol phenylate, dipropylene glycol phenylate process D directly drops under adsorption and separation material C normal temperature in propylene glycol phenylate, and its consumption is the 0.1-5% of propylene glycol phenylate quality.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201510325285.0A CN105016985A (en) | 2015-06-15 | 2015-06-15 | Preparation method for purifying propylene glycol phenyl ether |
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| CN201510325285.0A CN105016985A (en) | 2015-06-15 | 2015-06-15 | Preparation method for purifying propylene glycol phenyl ether |
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| CN105016985A true CN105016985A (en) | 2015-11-04 |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104326886A (en) * | 2014-10-11 | 2015-02-04 | 江苏常州酞青新材料科技有限公司 | Method for removing dipropylene glycol phenyl ether in propylene glycol phenyl ether refining process |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104326886A (en) * | 2014-10-11 | 2015-02-04 | 江苏常州酞青新材料科技有限公司 | Method for removing dipropylene glycol phenyl ether in propylene glycol phenyl ether refining process |
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Application publication date: 20151104 |