CN104307568A - Preparation method of hydroxypropyl-beta-cyclodextrin/ aluminium phosphotungstate catalyst used for preparation of dioctyl phthalate - Google Patents
Preparation method of hydroxypropyl-beta-cyclodextrin/ aluminium phosphotungstate catalyst used for preparation of dioctyl phthalate Download PDFInfo
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- CN104307568A CN104307568A CN201410460384.5A CN201410460384A CN104307568A CN 104307568 A CN104307568 A CN 104307568A CN 201410460384 A CN201410460384 A CN 201410460384A CN 104307568 A CN104307568 A CN 104307568A
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- cyclodextrin
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Abstract
The invention discloses a preparation method of hydroxypropyl-beta-cyclodextrin/ aluminium phosphotungstate catalyst used for preparation of dioctyl phthalate, and the method comprises the following steps: aluminium phosphotungstate and hydroxypropyl-beta-cyclodextrin in the molar ratio of 1:1-3 are put into a reactor, and added with water at 50 to 60 DEG C for preparation of a water solution, the water adding amount is 4-15 times of the total weight of the aluminium phosphotungstate and the hydroxypropyl-beta-cyclodextrin, the solution is placed in a microwave reactor, for radiation for 3 to 8 minutes in the 2400-2700MHz frequency, the product moisture is evaporated to obtain the hydroxypropyl-beta-cyclodextrin/ aluminium phosphotungstate catalyst. The hydroxypropyl-beta-cyclodextrin/ aluminium phosphotungstate catalyst has the characteristics to change reaction micro environment, enables esterification reaction of phthalic anhydride and 2-ethyl hexanol to perform in the inner cavity of the cyclodextrin, and has the advantages of simple preparation method and excellent catalytic effect.
Description
Technical field
The present invention relates to technical field of chemistry and chemical engineering, particularly relate to the preparation method of a kind of HP-β-CD for the preparation of dioctyl phthalate/aluminium phosphotungstic acid catalyst.
Background technology
Dioctyl phthalate (DOP) is universal plasticizer, is mainly used in the processing etc. of polyvinyl chloride fat.The consumption figure of dioctyl phthalate class plasticizer accounts for 80% of plasticizer total amount, and output is very large.All industrially that esterification under the acidic catalyst such as sulfuric acid, p-methyl benzenesulfonic acid exists obtains with phthalic anhydride and corresponding alcohol.Because the liquid acid such as sulfuric acid are serious to equipment corrosion, and document [Chen Yongmei, horse is gone away for some great undertakings. and heteropoly acid (salt) catalyzes and synthesizes the research of n-DOP, Chemical Industry in Guangzhou, and 1996,24 (2): 37-39] report employing AlPW
12o
40make catalyst, react 2 hours conversion ratios at 150 DEG C and can reach 94.2%.Heteropolyacid catalyst not only reaction effect is good, does not cause corrosion to equipment installation.
Summary of the invention
The object of the invention is to: in order to make phthalic anhydride and 2-Ethylhexyl Alcohol (isooctanol) fast reaction be converted into DOP, and catalyst not etching apparatus and recycling, spy provides the preparation method of a kind of HP-β-CD/aluminium phosphotungstic acid catalyst.
In order to achieve the above object, the present invention by the following technical solutions: by microwave by aluminium phosphotungstic acid inclusion in HP-β-CD inner chamber, formed HP-β-CD/aluminium phosphotungstic acid catalyst.
The concrete steps of preparation method of the present invention are as follows: be that aluminium phosphotungstic acid and the HP-β-CD of 1:1 ~ 3 puts into reactor by mol ratio, add water at 50 ~ 60 DEG C and be made into the aqueous solution, the dosage of water is 4-15 times of aluminium phosphotungstic acid and HP-β-CD gross weight, above-mentioned solution is put into microwave reactor, radiation 3 ~ 8 minutes under 2400-2700MHz frequency, product is boiled off moisture, obtains HP-β-CD/aluminium phosphotungstic acid catalyst.
The mol ratio of aluminium phosphotungstic acid and HP-β-CD is preferably 1:2.
Preferably add water at 55 DEG C and be made into the aqueous solution, the dosage of water is 10 times of aluminium phosphotungstic acid and HP-β-CD gross weight.
Preferably radiation 5 minutes under 2540MHz frequency.
Good effect of the present invention is as follows:
Aluminium phosphotungstic acid is by after HP-β-CD inclusion, the catalytic esterification of phthalic anhydride and 2-Ethylhexyl Alcohol two kinds of reactants and aluminium phosphotungstic acid carries out in cyclodextrin inner chamber microenvironment, not only reactant concentration is improved significantly, also due to the hydrophobic property of cyclodextrin inner chamber, the water that the reversible esterification of microenvironment generates is discharged by hydrophobic cavity continuously, promotes that reaction is constantly carried out to generation DOP direction.This method for preparing catalyst is easy, has fabulous catalytic effect.
Detailed description of the invention
The following examples describe in further detail of the present invention.
Embodiment 1
Be that aluminium phosphotungstic acid and the HP-β-CD of 1:1 puts into reactor by mol ratio, add water at 50 DEG C and be made into the aqueous solution, the dosage of water is 4 times of aluminium phosphotungstic acid and HP-β-CD gross weight, above-mentioned solution is put into microwave reactor, radiation 8 minutes under 2400MHz frequency, product is boiled off moisture, obtains HP-β-CD/aluminium phosphotungstic acid catalyst.
Embodiment 2
Be that aluminium phosphotungstic acid and the HP-β-CD of 1:3 puts into reactor by mol ratio, add water at 60 DEG C and be made into the aqueous solution, the dosage of water is 15 times of aluminium phosphotungstic acid and HP-β-CD gross weight, above-mentioned solution is put into microwave reactor, radiation 3 minutes under 2700MHz frequency, product is boiled off moisture, obtains HP-β-CD/aluminium phosphotungstic acid catalyst.
Embodiment 3
Be that aluminium phosphotungstic acid and the HP-β-CD of 1:2 puts into reactor by mol ratio, add water at 55 DEG C and be made into the aqueous solution, the dosage of water is 10 times of aluminium phosphotungstic acid and HP-β-CD gross weight, above-mentioned solution is put into microwave reactor, radiation 5 minutes under 2540MHz frequency, product is boiled off moisture, obtains HP-β-CD/aluminium phosphotungstic acid catalyst.
Embodiment 4
Get the phthalic anhydride of 0.2mol and the 2-Ethylhexyl Alcohol of 0.44mol, HP-β-CD/aluminium phosphotungstic acid catalyst prepared by 25mL cyclohexane and 3g embodiment 3, react 20 minutes at 150 DEG C, esterification yield 94.5%.
Reference examples 2
Get the phthalic anhydride of 0.2mol and the 2-Ethylhexyl Alcohol of 0.44mol, 25mL cyclohexane and 3gAlPW
12o
40catalyst, reacts 2 hours, esterification yield 82.5% at 150 DEG C.
Although illustrate and describe embodiments of the invention, for the ordinary skill in the art, be appreciated that and can carry out multiple change, amendment, replacement and modification to these embodiments without departing from the principles and spirit of the present invention, scope of the present invention is by claims and equivalents thereof.
Claims (4)
1. the preparation method of the HP-β-CD for the preparation of dioctyl phthalate/aluminium phosphotungstic acid catalyst, it is characterized in that: the concrete steps of described preparation method are as follows: be that aluminium phosphotungstic acid and the HP-β-CD of 1:1 ~ 3 puts into reactor by mol ratio, add water at 50 ~ 60 DEG C and be made into the aqueous solution, the dosage of water is 4-15 times of aluminium phosphotungstic acid and HP-β-CD gross weight, above-mentioned solution is put into microwave reactor, radiation 3 ~ 8 minutes under 2400-2700MHz frequency, product is boiled off moisture, obtain HP-β-CD/aluminium phosphotungstic acid catalyst.
2., as claimed in claim 1 for the preparation of the preparation method of the HP-β-CD/aluminium phosphotungstic acid catalyst of dioctyl phthalate, it is characterized in that: the mol ratio of aluminium phosphotungstic acid and HP-β-CD is 1:2.
3. as claimed in claim 1 for the preparation of the preparation method of the HP-β-CD/aluminium phosphotungstic acid catalyst of dioctyl phthalate, it is characterized in that: adding water at 55 DEG C is made into the aqueous solution, the dosage of water is 10 times of aluminium phosphotungstic acid and HP-β-CD gross weight.
4., as claimed in claim 1 for the preparation of the preparation method of the HP-β-CD/aluminium phosphotungstic acid catalyst of dioctyl phthalate, it is characterized in that: radiation 5 minutes under 2540MHz frequency.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410460384.5A CN104307568A (en) | 2014-09-10 | 2014-09-10 | Preparation method of hydroxypropyl-beta-cyclodextrin/ aluminium phosphotungstate catalyst used for preparation of dioctyl phthalate |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410460384.5A CN104307568A (en) | 2014-09-10 | 2014-09-10 | Preparation method of hydroxypropyl-beta-cyclodextrin/ aluminium phosphotungstate catalyst used for preparation of dioctyl phthalate |
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| CN104307568A true CN104307568A (en) | 2015-01-28 |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0039878B1 (en) * | 1980-05-08 | 1983-12-28 | Basf Wyandotte Corporation | Method of making mixed esters of phthalic acid |
| CN1768937A (en) * | 2004-11-05 | 2006-05-10 | 中国石油化工股份有限公司 | Microcellular structured heteropoly acid/ silicon dioxide catalyst |
-
2014
- 2014-09-10 CN CN201410460384.5A patent/CN104307568A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0039878B1 (en) * | 1980-05-08 | 1983-12-28 | Basf Wyandotte Corporation | Method of making mixed esters of phthalic acid |
| CN1768937A (en) * | 2004-11-05 | 2006-05-10 | 中国石油化工股份有限公司 | Microcellular structured heteropoly acid/ silicon dioxide catalyst |
Non-Patent Citations (6)
| Title |
|---|
| ALPANA PARIKH ET AL.: "Metal(Ⅳ)tungstates as solid acid catalysts for the synthesis of phthalate diester-dioctyl phthalate(DOP)", 《INDIAN JOURNAL OF CHEMICAL TECHNOLOGY》 * |
| HONGLIANG LI ET AL.: "Synthesis of dioctyl phthalate using acid functionalized ionic liquid as catalyst", 《CATALYSIS COMMUNICATIONS》 * |
| 余新武 等: "TiSiW12O40/TiO2催化合成邻苯二甲酸二辛酯", 《东北师大学报自然科学版》 * |
| 姚志臣 等: "邻苯二甲酸二辛酯增塑剂合成催化剂与工艺条件研究", 《精细石油化工进展》 * |
| 段颖波 等: "杂多酸盐多相催化法制备绝缘级DOP", 《辽宁化工》 * |
| 陆勇: "介孔分子筛负载杂多酸催化剂催化合成邻苯二甲酸二辛酯", 《化工时刊》 * |
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Application publication date: 20150128 |