CN104292083A - Method for removing phenol in refining process of propylene glycol monophenyl ether - Google Patents
Method for removing phenol in refining process of propylene glycol monophenyl ether Download PDFInfo
- Publication number
- CN104292083A CN104292083A CN201410531686.7A CN201410531686A CN104292083A CN 104292083 A CN104292083 A CN 104292083A CN 201410531686 A CN201410531686 A CN 201410531686A CN 104292083 A CN104292083 A CN 104292083A
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- CN
- China
- Prior art keywords
- propylene glycol
- phenol
- glycol phenylate
- adsorption
- monophenyl ether
- Prior art date
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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
- B01J20/223—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material containing metals, e.g. organo-metallic compounds, coordination complexes
-
- 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
- B01J20/30—Processes for preparing, regenerating, or reactivating
-
- 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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/46—Materials comprising a mixture of inorganic and organic materials
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for removing phenol in the refining process of propylene glycol monophenyl ether. Through treatments, e.g., a synthetized adsorptive separation material (A) is dispersed in the propylene glycol monophenyl ether, phenol (B) in propylene glycol monophenyl ether is enriched, so that the original high phenol content of the propylene glycol monophenyl ether is reduced. The method disclosed by the invention is low in production and machining process cost, low in refining energy consumption, and suitable for producing high-quality propylene glycol monophenyl ether products through using the existing equipment and technical conditions in 3-Phenoxy-1-propanol production enterprises production enterprises.
Description
Technical field
The present invention relates to the minimizing technology of phenol in a kind of propylene glycol phenylate treating process.
Background technology
Current domestic propylene glycol phenylate synthetic method generally all adopts propylene oxide 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 propylene glycol phenylate as much as possible.In common first grade propylene glycol phenylate, 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 propylene glycol phenylate manufacturing enterprises have all dropped into a lot of technical study strength, but because in propylene glycol phenylate, trace phenol content 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 phenol content problem in propylene glycol phenyl ether product.
The object of the invention is to realize as follows: the minimizing technology of phenol in a kind of propylene glycol phenylate treating process, the dispersion in propylene glycol phenylate of the adsorption and separation material (A) of synthesis is used to wait process, phenol (B) in enrichment propylene glycol phenylate, makes the propylene glycol phenylate of former high-content phenol be reduced;
Further prioritization scheme is, the minimizing technology of phenol in above-mentioned a kind of propylene glycol phenylate treating process, and the adsorption and separation material (A) of synthesis comprises:
(1) use deionization water-reducible water glass 10-20% concentration, use acetic acid to neutralize pH value not higher than 7.5, form silicon dioxide gel;
(2) functional quality concentration is not higher than the aqueous isopropanol of 3% aluminum isopropylate, joins in aforementioned silicas colloidal sol under normal temperature with the ratio of aluminum isopropylate and silicon-dioxide 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 75-80 DEG C, be namely incubated aging 3 hours when temperature reaches 80 DEG C;
(4) after aging end, adopt and filter, the impurity such as method removing Virahol wherein such as deionized water wash.The solid material that obtains dry 10-12 hour under not higher than 140 DEG C of conditions will be filtered;
Further prioritization scheme is, the minimizing technology of phenol in above-mentioned a kind of propylene glycol phenylate treating process, in enrichment propylene glycol phenylate, phenol process (B) directly drops under adsorption and separation material (A) normal temperature in propylene glycol phenylate, and its consumption is the 0.5-4.5% of propylene glycol phenylate quality;
Further prioritization scheme is, the minimizing technology of phenol in above-mentioned a kind of propylene glycol phenylate treating process, adsorption and separation material (A) can be reused, after needing the toluene solution washing of the quality such as use before reusing, through not higher than 140 DEG C of dryings.
Advantage of the present invention: the control techniques of the present invention to the phenol content in existing propylene glycol phenylate 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 propylene glycol phenylate manufacturing enterprise and utilizes existing installation and technical qualification, obtain high-quality propylene glycol phenyl ether product.
embodiment:
The minimizing technology of phenol in a kind of propylene glycol phenylate treating process, it is characterized in that: use the dispersion in propylene glycol phenylate of the adsorption and separation material (A) of synthesis to wait process, phenol (B) in enrichment propylene glycol phenylate, makes the propylene glycol phenylate of former high-content phenol be reduced; The adsorption and separation material (A) of synthesis comprises:
(1) use deionization water-reducible water glass 10-20% concentration, use acetic acid to neutralize pH value not higher than 7.5, form silicon dioxide gel;
(2) functional quality concentration is not higher than the aqueous isopropanol of 3% aluminum isopropylate, joins in aforementioned silicas colloidal sol under normal temperature with the ratio of aluminum isopropylate and silicon-dioxide 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 75-80 DEG C, be namely incubated aging 3 hours when temperature reaches 80 DEG C;
(4) after aging end, adopt and filter, the impurity such as method removing Virahol wherein such as deionized water wash.The solid material that obtains dry 10-12 hour under not higher than 140 DEG C of conditions will be filtered; In enrichment propylene glycol phenylate, phenol process (B) directly drops under adsorption and separation material (A) normal temperature in propylene glycol phenylate, and its consumption is the 0.5-4.5% of propylene glycol phenylate quality; Adsorption and separation material (A) can be reused, after needing the toluene solution washing of the quality such as use before reusing, through not higher than 140 DEG C of dryings.
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 | 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 0.5% quality, disperse stirring 1 hour under normal temperature, the method for rear employing precipitate and separate separates out solid absorption parting material, can by the phenol rich in propylene glycol phenylate out,
| Phenol content before fractionation by adsorption | Phenol content after process |
| 0.15% | 600ppm |
Implement example 2
A adsorption separating agent preparation technology
Starting material and control condition:
| Control condition | Reference mark | Remarks |
| Water glass weaker concn % | 25% | Concentration after deionized water dilution |
| PH after acidifying with acetic acid | 6.5 | ? |
| 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% 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 propylene glycol phenylate 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 propylene glycol phenylate, phenol ability is as follows:
| Reuse number of times | Phenol content in original propylene glycol phenylate | Phenol content after process |
| 1 | 0.1% | 81ppm |
| 5 | 0.1% | 84ppm |
| 10 | 0.1% | 82ppm |
| 20 | 0.1% | 83ppm |
| 30 | 0.1% | 86ppm |
| 40 | 0.1% | 85ppm |
| 43 | 0.1% | 90ppm |
| 44 | 0.1% | 100ppm |
| 45 | 0.1% | 150ppm |
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
With propylene glycol phenylate for benchmark, drop into the solid absorption parting material of propylene glycol phenylate quality 4.5% quality, disperse stirring 3 hours under normal temperature, the method for rear employing precipitate and separate separates out solid absorption parting material, can by the phenol rich in propylene glycol phenylate 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 (4)
1. the minimizing technology of phenol in a propylene glycol phenylate treating process, it is characterized in that: use the dispersion in propylene glycol phenylate of the adsorption and separation material (A) of synthesis to wait process, phenol (B) in enrichment propylene glycol phenylate, makes the propylene glycol phenylate of former high-content phenol be reduced.
2. the minimizing technology of phenol in a kind of propylene glycol phenylate treating process according to claim 1, is characterized in that: the adsorption and separation material (A) of synthesis comprises:
(1) use deionization water-reducible water glass 10-20% concentration, use acetic acid to neutralize pH value not higher than 7.5, form silicon dioxide gel;
(2) functional quality concentration is not higher than the aqueous isopropanol of 3% aluminum isopropylate, joins in aforementioned silicas colloidal sol under normal temperature with the ratio of aluminum isopropylate and silicon-dioxide 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 75-80 DEG C, be namely incubated aging 3 hours when temperature reaches 80 DEG C;
(4) after aging end, adopt and filter, the impurity such as the method such as deionized water wash removing Virahol wherein, will the solid material that obtains dry 10-12 hour under not higher than 140 DEG C of conditions be filtered.
3. the minimizing technology of phenol in a kind of propylene glycol phenylate treating process according to claim 1, it is characterized in that: in enrichment propylene glycol phenylate, phenol process (B) directly drops under adsorption and separation material (A) normal temperature in propylene glycol phenylate, and its consumption is the 0.5-4.5% of propylene glycol phenylate quality.
4. the minimizing technology of phenol in a kind of propylene glycol phenylate treating process according to claim 1, it is characterized in that: adsorption and separation material (A) can be reused, after needing the toluene solution washing of the quality such as use before reusing, through not higher than 140 DEG C of dryings.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410531686.7A CN104292083A (en) | 2014-10-11 | 2014-10-11 | Method for removing phenol in refining process of propylene glycol monophenyl ether |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410531686.7A CN104292083A (en) | 2014-10-11 | 2014-10-11 | Method for removing phenol in refining process of propylene glycol monophenyl ether |
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| Publication Number | Publication Date |
|---|---|
| CN104292083A true CN104292083A (en) | 2015-01-21 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410531686.7A Pending CN104292083A (en) | 2014-10-11 | 2014-10-11 | Method for removing phenol in refining process of propylene glycol monophenyl ether |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104909996A (en) * | 2015-06-15 | 2015-09-16 | 江苏常州酞青新材料科技有限公司 | Fine preparation method of phenoxy propandiol subjected to phenol removal |
| CN106478385A (en) * | 2015-09-02 | 2017-03-08 | 奇里茨应用技术（上海）有限公司 | A kind of prepare high-purity propylene glycol phenylate of Determination of Trace Phenol or the method for ethylene glycol phenyl ether |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101712600A (en) * | 2008-10-07 | 2010-05-26 | 抚顺佳化聚氨酯有限公司 | Method for preparing ethylene glycol phenyl ether, propylene glycol phenyl ether and butylene glycol phenyl ether |
| WO2013180888A1 (en) * | 2012-05-31 | 2013-12-05 | Exxonmobil Chemical Patents Inc. | Phenol removal in paraxylene recovery process |
-
2014
- 2014-10-11 CN CN201410531686.7A patent/CN104292083A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101712600A (en) * | 2008-10-07 | 2010-05-26 | 抚顺佳化聚氨酯有限公司 | Method for preparing ethylene glycol phenyl ether, propylene glycol phenyl ether and butylene glycol phenyl ether |
| WO2013180888A1 (en) * | 2012-05-31 | 2013-12-05 | Exxonmobil Chemical Patents Inc. | Phenol removal in paraxylene recovery process |
Non-Patent Citations (1)
| Title |
|---|
| 陶绪泉 等: "新型水性环境友好型涂料成膜助剂-丙二醇苯醚的制备", 《涂料工业》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104909996A (en) * | 2015-06-15 | 2015-09-16 | 江苏常州酞青新材料科技有限公司 | Fine preparation method of phenoxy propandiol subjected to phenol removal |
| CN106478385A (en) * | 2015-09-02 | 2017-03-08 | 奇里茨应用技术（上海）有限公司 | A kind of prepare high-purity propylene glycol phenylate of Determination of Trace Phenol or the method for ethylene glycol phenyl ether |
| CN106478385B (en) * | 2015-09-02 | 2019-07-23 | 奇里茨应用技术（上海）有限公司 | A method of preparing the high-purity propylene glycol phenylate or ethylene glycol phenyl ether of Determination of Trace Phenol |
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Application publication date: 20150121 |