CN101462043A - Catalyst for preparing isophorone using condensation of acetone and preparation method thereof - Google Patents
Catalyst for preparing isophorone using condensation of acetone and preparation method thereof Download PDFInfo
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- CN101462043A CN101462043A CN 200710307288 CN200710307288A CN101462043A CN 101462043 A CN101462043 A CN 101462043A CN 200710307288 CN200710307288 CN 200710307288 CN 200710307288 A CN200710307288 A CN 200710307288A CN 101462043 A CN101462043 A CN 101462043A
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Abstract
The invention discloses a catalyst for preparing isophorone by condensing acetone and a preparation method thereof. The catalyst is composite oxide Mg(M)AlO, a molecular general formula of the catalyst is represented by Mg(Mx)AlyOz, wherein M represents lithium, barium or calcium, x is more than or equal to 0.05 and is less than or equal to 0.3, y is more than or equal to 0.25 and is less than or equal to 0.75, z is equal to 1+nx/2+3y/2, and n is a chemical valence of the doped metal element M. The catalyst is used for a reaction that the acetone is condensed to prepare the isophorone, the highest conversion rate under normal pressure reaches 38.2 percent, the selectivity of the isophorone is 77.8 percent, and the total selectivity of the isophorone and mesityl oxide reaches 87.8 percent.
Description
Technical field
The invention belongs to a kind of catalyst for preparing isophorone using condensation of acetone and preparation method thereof.
Background technology
Isophorone (CAS RN 78-59-1, isophorone are called for short IP) be a kind of be good high boiling solvent, be the important source material of fine chemistry industry industry.In addition, because isophorone has conjugation beta-unsaturated ketone structure, its pair key can further react and obtain alcohol, acid, amine, ester and isocyanide ester etc., is the important chemical intermediate.Isophorone is one of derived product of acetone, is obtained through condensation, dehydration, Mecheal addition, Cheng Huan by acetone.At present, the main production firm of isophorone is some external major companies, as: German goldschmidt chemical corporation, U.S. rom Haars Co., Ltd, Dow Chemical, Britain BP company, Japanese contest Lopa Nationality company.China does not still have formal manufacturer at present, and the bench-scale testing production of reagent manufacturing enterprise of a few family is only arranged, and output seldom.
At present to produce the catalyst of isophorone mainly be some solid bases to condensation of acetone, as the oxide or the hydroxide of alkali metal, alkaline-earth metal, the mixed-alkali oxide, report mainly be the magnalium mixed oxide of various method preparation.Many about isophorone Preparation of catalysts United States Patent (USP) report, make catalyst after the mixture roasting such as US5627303 employing magnesium carbonate, aluminium carbonate, best result is that conversion ratio is 31.34% under 290 ℃, 4psig condition, and the total selectivity of isophorone and isopropylidene acetone is 77.67%.The catalyst of report generally carries out under pressurized conditions at present, and reaction temperature is generally more than 280 ℃.
Summary of the invention
The object of the present invention is to provide a kind of catalyst for preparing isophorone using condensation of acetone and preparation method thereof.
A kind of catalyst for preparing isophorone using condensation of acetone is characterized in that catalyst is composite oxides Mg (M) AlO, its general molecular formula Mg (M
x) Al
yO
zExpression, wherein M represents lithium, barium or calcium, 0.05≤x≤0.3,0.25≤y≤0.75, z=1+nx/2+3y/2, n are the chemical valence of doped metallic elements M.
Preparation of catalysts method of the present invention comprises the steps:
The mixed solution of A, preparation magnesium nitrate, aluminum nitrate and doping M nitrate, wherein ratio Mg:M:Al=1:0.05～0.3:0.25～0.75 of three's amount of substance;
B, preparation aqueous slkali are by stoichiometric NaOH of metalline and small amount of N a
2CO
3Form Na
2CO
3Amount be controlled at the 10-30% of NaOH amount;
Under C, the mechanical agitation, two kinds of mixed solutions and drip are added in the distilled water, the rate of addition of controlling two solution maintains between the 8-10 pH value of gained slurries;
D, dropwise after, crystallization at a certain temperature refluxes;
E, the cold back of slurries that the backflow crystallization is good are filtered, and are washed with a large amount of distillations; Filter cake at 100-150 ℃ of dry 15-35h, is made catalyst at 350-600 ℃ of roasting 3-10h at last.
In above-mentioned Preparation of catalysts method, crystallization temperature is between 60-85 ℃, and crystallization process is finished in 15-35h.
The catalyst of preparation can directly use in atmospheric fixed bed, and reaction temperature is between 220-300 ℃.The accessory substance kind of reaction is few, mainly is isopropylidene acetone and micro-high-boiling components.
Catalyst provided by the invention, the kind of accessory substance is few in the product, makes product be easy to separate from mix products; Use this catalyst also to reduce requirement simultaneously, good active is just arranged under normal pressure reaction condition.
Catalyst is used for the reaction of preparing isophorone using condensation of acetone, and conversion ratio is up to 38.2% under the normal pressure, and the selectivity of isophorone is 77.8%, and the total selectivity of isophorone and isopropylidene acetone reaches 87.8%.
Embodiment 1
With nitrate Mg:Ca:Al=8:1:3 preparation in molar ratio salting liquid, prepare Na simultaneously by stoichiometric NaOH and 25%
2CO
3The aqueous slkali of forming.Under the mechanical agitation two solution and drip are added in a small amount of 80 ℃ distilled water, regulate rate of addition the pH value is maintained between the 8-10.Drip the back and keep 80 ℃ of mechanical agitation 24h, cooled and filtered is washed with massive laundering.Filter cake is put into 120 ℃ of dry 24h of baking oven, get catalyst sample at 500 ℃ of roasting 8h afterwards.
Embodiment 2
Preparation process is with embodiment 1, and the mol ratio of nitrate changes Mg:Ca:Al=19:1:10 into.
Embodiment 3
Preparation process is with embodiment 1, the doped barium ion, and the mol ratio of nitrate is Mg:Ba:Al=8:1:3.
Embodiment 4
Preparation process is with embodiment 1, the doped barium ion, and the mol ratio of nitrate changes Mg:Ba:Al=19:1:10 into.
The catalyst of gained among the embodiment 1,2,3,4 is pulverized, got 20-60 purpose sample and install in the fixed bed reaction pipe, squeeze into acetone with constant-flux pump and keep the liquid air speed at 3h
-1Acetone is bathed with cryosel after by reaction bed and is accepted.Be reflected at normal pressure, 240 ℃ of reactions, the product of getting condensation after two hours carries out chromatography, and the result of analysis is as shown in the table, and conversion ratio and selectivity are calculated according to amount of substance.
Claims (3)
1, a kind of catalyst for preparing isophorone using condensation of acetone is characterized in that catalyst is composite oxides Mg (M) AlO, its general molecular formula Mg (M
x) Al
yO
zExpression, wherein M represents lithium, barium or calcium, 0.05≤x≤0.3,0.25≤y≤0.75, z=1+nx/2+3y/2, n are the chemical valence of doped metallic elements M.
2, Preparation of catalysts method according to claim 1 is characterized in that the preparation method comprises the steps:
The mixed solution of A, preparation magnesium nitrate, aluminum nitrate and doping M nitrate, wherein ratio Mg:M:Al=1:0.05～0.3:0.25～0.75 of three's amount of substance;
B, preparation aqueous slkali are by stoichiometric NaOH of metalline and small amount of N a
2CO
3Form Na
2CO
3Amount be controlled at the 10-30% of NaOH amount;
Under C, the mechanical agitation, two kinds of mixed solutions and drip are added in the distilled water, the rate of addition of controlling two solution maintains between the 8-10 pH value of gained slurries;
D, dropwise after, crystallization at a certain temperature refluxes;
E, the cold back of slurries that the backflow crystallization is good are filtered, and are washed with a large amount of distillations; Filter cake at 100-150 ℃ of dry 15-35h, is made catalyst at 350-600 ℃ of roasting 3-10h at last.
3, method as claimed in claim 2 is characterized in that crystallization temperature between 60-85 ℃, and crystallization process is finished in 15-35h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200710307288 CN101462043A (en) | 2007-12-18 | 2007-12-18 | Catalyst for preparing isophorone using condensation of acetone and preparation method thereof |
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|---|---|---|---|
| CN 200710307288 CN101462043A (en) | 2007-12-18 | 2007-12-18 | Catalyst for preparing isophorone using condensation of acetone and preparation method thereof |
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| CN101462043A true CN101462043A (en) | 2009-06-24 |
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| CN 200710307288 Pending CN101462043A (en) | 2007-12-18 | 2007-12-18 | Catalyst for preparing isophorone using condensation of acetone and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101698147B (en) * | 2009-10-23 | 2012-01-25 | 广州大学 | Catalyst for preparing isophorone by acetone condensation method |
| CN105126801A (en) * | 2015-08-28 | 2015-12-09 | 厦门大学 | Catalyst used for synthesizing isophorone and preparation method thereof |
| CN105268422A (en) * | 2014-07-11 | 2016-01-27 | 中国石油化工股份有限公司 | Preparation method of isophorone catalyst |
| CN104549371B (en) * | 2013-10-22 | 2016-11-23 | 中国石油化工股份有限公司 | Catalyst of preparing isophorone using condensation of acetone and preparation method thereof |
| CN106824159A (en) * | 2015-12-03 | 2017-06-13 | 中国石油化工股份有限公司 | Isophorone catalyst and preparation method thereof |
| CN106824299A (en) * | 2015-12-03 | 2017-06-13 | 中国石油化工股份有限公司 | The renovation process of isophorone catalyst |
-
2007
- 2007-12-18 CN CN 200710307288 patent/CN101462043A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101698147B (en) * | 2009-10-23 | 2012-01-25 | 广州大学 | Catalyst for preparing isophorone by acetone condensation method |
| CN104549371B (en) * | 2013-10-22 | 2016-11-23 | 中国石油化工股份有限公司 | Catalyst of preparing isophorone using condensation of acetone and preparation method thereof |
| CN105268422A (en) * | 2014-07-11 | 2016-01-27 | 中国石油化工股份有限公司 | Preparation method of isophorone catalyst |
| CN105268422B (en) * | 2014-07-11 | 2018-09-14 | 中国石油化工股份有限公司 | The preparation method of isophorone catalyst |
| CN105126801A (en) * | 2015-08-28 | 2015-12-09 | 厦门大学 | Catalyst used for synthesizing isophorone and preparation method thereof |
| CN106824159A (en) * | 2015-12-03 | 2017-06-13 | 中国石油化工股份有限公司 | Isophorone catalyst and preparation method thereof |
| CN106824299A (en) * | 2015-12-03 | 2017-06-13 | 中国石油化工股份有限公司 | The renovation process of isophorone catalyst |
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Open date: 20090624 |