CN112239400A - Preparation method of isophorone - Google Patents
Preparation method of isophorone Download PDFInfo
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- CN112239400A CN112239400A CN201910643843.6A CN201910643843A CN112239400A CN 112239400 A CN112239400 A CN 112239400A CN 201910643843 A CN201910643843 A CN 201910643843A CN 112239400 A CN112239400 A CN 112239400A
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- reaction
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- isophorone
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/61—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by reactions not involving the formation of >C = O groups
- C07C45/67—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by reactions not involving the formation of >C = O groups by isomerisation; by change of size of the carbon skeleton
- C07C45/68—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by reactions not involving the formation of >C = O groups by isomerisation; by change of size of the carbon skeleton by increase in the number of carbon atoms
- C07C45/72—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by reactions not involving the formation of >C = O groups by isomerisation; by change of size of the carbon skeleton by increase in the number of carbon atoms by reaction of compounds containing >C = O groups with the same or other compounds containing >C = O groups
- C07C45/74—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by reactions not involving the formation of >C = O groups by isomerisation; by change of size of the carbon skeleton by increase in the number of carbon atoms by reaction of compounds containing >C = O groups with the same or other compounds containing >C = O groups combined with dehydration
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- 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
- B01J27/25—Nitrates
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2601/00—Systems containing only non-condensed rings
- C07C2601/12—Systems containing only non-condensed rings with a six-membered ring
- C07C2601/16—Systems containing only non-condensed rings with a six-membered ring the ring being unsaturated
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a preparation method of isophorone, and relates to the technical field of isophorone. The method comprises the following steps: carrying out impregnation reaction on alumina and aluminum oxide serving as carriers and a potassium hydroxide solution and a magnesium nitrate solution to generate a catalyst; adding a reaction solvent into a reaction kettle, setting the rotating speed of the reaction kettle to be 200-250 r/min, adjusting the pH value of the reaction solvent to be 3-3.5, adding acetone, adjusting the reaction temperature to be 200-210 ℃, adding alkaline anion exchange resin, and reacting for 7-8 hours to obtain a reactant A; adjusting the pressure of the reaction kettle to be 1.6-1.9 MPa and the temperature to be 175-185 ℃, adding the catalyst into the reactant A, and carrying out condensation reaction to obtain a reactant B; and diluting the reactant B by adding distilled water, and then obtaining the isophorone by using a rectifying agent. The scheme can improve the selectivity and the product yield of the isophorone, wherein the selectivity can reach 89%, and the product yield can reach 70.9%.
Description
Technical Field
The invention relates to the technical field of isophorone, and particularly relates to a preparation method of isophorone.
Background
Isophorone is a good solvent for high molecular materials, and is widely applied to industries of plastics, pesticides, medicines, coatings and the like. At present, more methods for preparing isophorone exist, but the conversion rate of isophorone is low, so that the production cost is high.
Disclosure of Invention
The invention aims to solve the technical problems of how to improve the conversion rate of the isophorone and reduce the production cost of the isophorone.
In order to solve the above technical problems, the present invention provides a method for preparing isophorone, comprising:
carrying out impregnation reaction on alumina and aluminum oxide serving as carriers and a potassium hydroxide solution and a magnesium nitrate solution to generate a catalyst;
adding a reaction solvent into a reaction kettle, setting the rotating speed of the reaction kettle to be 200-250 r/min, adjusting the pH value of the reaction solvent to be 3-3.5, adding acetone, adjusting the reaction temperature to be 200-210 ℃, adding alkaline anion exchange resin, and reacting for 7-8 hours to obtain a reactant A;
adjusting the pressure of the reaction kettle to be 1.6-1.9 MPa and the temperature to be 175-185 ℃, adding the catalyst into the reactant A, and carrying out condensation reaction to obtain a reactant B;
and diluting the reactant B by adding distilled water, and then obtaining the isophorone by using a rectifying agent.
The technical scheme of the invention is further defined as follows:
further, the step of using alumina as a carrier to perform an impregnation reaction with a potassium hydroxide solution and a magnesium nitrate solution to generate the catalyst comprises:
putting 13-32 mesh aluminum oxide into a potassium hydroxide solution, soaking at room temperature for 35-40 min, and then drying to obtain a solid A; putting the solid A into a magnesium nitrate solution, and soaking for 1-1.5h at room temperature; drying in an oven at 80 ℃, then roasting, and impregnating for multiple times to obtain the catalyst.
The process as described before, said subsequent drying, obtaining a solid a comprising: drying in an oven at 75-90 ℃ for 3-3.5h to obtain the solid A.
The method as described above, wherein the firing comprises: roasting in a furnace at 600-650 ℃ for 3-3.5 h.
In the method, the reaction solvent is one or more of benzene, toluene, xylene and trimethylbenzene.
In the method, the ratio of the alumina to the aluminum oxide is 2 (1-1.2).
In the method, the rectification agent comprises propylene and butane, and the component ratio of the propylene to the butane is 1 (1.2-1.5).
The invention has the beneficial effects that: in the invention, acetone and a catalyst are used for reaction and condensation to obtain isophorone, in the first step, the acetone and the alkaline anion exchange resin are reacted to obtain a reactant A, in the step, the alkaline anion exchange resin is used as the catalyst for reaction, so that the conversion rate of the acetone can reach more than 70%, in the second step, alumina and aluminum oxide are used as carriers and are subjected to impregnation reaction with a potassium hydroxide solution and a magnesium nitrate solution to generate the catalyst and the reactant A for reaction, wherein a proper amount of potassium hydroxide solution can effectively inhibit the generation of byproduct mesitylene and improve the conversion rate of the isophorone, and because the aluminum oxide and the aluminum oxide are in a porous structure, the potassium hydroxide and the magnesium nitrate can be uniformly dispersed on the surfaces of the aluminum oxide and the aluminum oxide, the specific surface area of the catalyst is larger, the activity of the catalyst is higher, and the conversion rates of the acetone and the isophorone can be greatly improved, wherein the selectivity of the isophorone is 89%, and the yield of the product reaches 70.9%.
Detailed Description
Example (b): a preparation method of isophorone comprises the following steps:
alumina and aluminum oxide are used as carriers, and are subjected to impregnation reaction with a potassium hydroxide solution and a magnesium nitrate solution to generate the catalyst. Specifically, the step is used for obtaining the high-efficiency catalyst for subsequent reaction so as to improve the selectivity and the conversion rate of the isophorone.
Adding a reaction solvent into a reaction kettle, setting the rotating speed of the reaction kettle to be 200-250 r/min, adjusting the pH value of the reaction solvent to be 3-3.5, adding acetone, adjusting the reaction temperature to be 200-210 ℃, adding alkaline anion exchange resin, and reacting for 7-8 hours to obtain a reactant A.
And (3) adjusting the pressure of the reaction kettle to be 1.6-1.9 MPa and the temperature to be 175-185 ℃, adding a catalyst into the reactant A, and carrying out condensation reaction to obtain a reactant B.
And diluting the reactant B by adding distilled water, and then obtaining isophorone by using a rectifying agent.
The method for preparing the catalyst by using the alumina as a carrier and carrying out impregnation reaction on the alumina, a potassium hydroxide solution and a magnesium nitrate solution to generate the catalyst comprises the following steps:
putting 13-32 mesh aluminum oxide into a potassium hydroxide solution, soaking at room temperature for 35-40 min, and then drying to obtain a solid A; putting the solid A into a magnesium nitrate solution, and soaking for 1-1.5h at room temperature; drying in an oven at 80 ℃, then roasting, and carrying out multiple times of impregnation to obtain the catalyst, wherein the roasting environment is that roasting is carried out for 3-3.5h at 600-650 ℃ in a furnace.
Specifically, the ratio of alumina to alumina is 2 (1-1.2), and in this embodiment, the ratio of alumina to alumina is preferably 2: 1.1.
Wherein, when the catalyst is prepared, the drying is carried out to obtain the solid A, and the specific steps comprise: drying in an oven at 75-90 ℃ for 3-3.5h to obtain solid A.
The reaction solvent is one or more of benzene, toluene, xylene and trimethylbenzene. In this embodiment, the reaction solvent is preferably a mixture of benzene, xylene and trimethylbenzene. The rectification agent comprises propylene and butane, wherein the component ratio of the propylene to the butane is 1 (1.2-1.5), the component ratio is the weight fraction ratio, and in the embodiment, the component ratio of the propylene to the butane is preferably 1: 1.3.
In the invention, acetone and a catalyst are used for reaction and condensation to obtain isophorone, in the first step, the acetone and the alkaline anion exchange resin are reacted to obtain a reactant A, in the step, the alkaline anion exchange resin is used as the catalyst for reaction, so that the conversion rate of the acetone can reach more than 70%, in the second step, alumina and aluminum oxide are used as carriers and are subjected to impregnation reaction with a potassium hydroxide solution and a magnesium nitrate solution to generate the catalyst and the reactant A for reaction, wherein a proper amount of potassium hydroxide solution can effectively inhibit the generation of byproduct mesitylene and improve the conversion rate of the isophorone, and because the aluminum oxide and the aluminum oxide are in a porous structure, the potassium hydroxide and the magnesium nitrate can be uniformly dispersed on the surfaces of the aluminum oxide and the aluminum oxide, the specific surface area of the catalyst is larger, the activity of the catalyst is higher, and the conversion rates of the acetone and the isophorone can be greatly improved, wherein the selectivity of the isophorone is 89%, and the yield of the product reaches 70.9%.
In addition to the above embodiments, the present invention may have other embodiments. All technical solutions formed by adopting equivalent substitutions or equivalent transformations fall within the protection scope of the claims of the present invention.
Claims (7)
1. A method for preparing isophorone, which is characterized by comprising the following steps:
carrying out impregnation reaction on alumina and aluminum oxide serving as carriers and a potassium hydroxide solution and a magnesium nitrate solution to generate a catalyst;
adding a reaction solvent into a reaction kettle, setting the rotating speed of the reaction kettle to be 200-250 r/min, adjusting the pH value of the reaction solvent to be 3-3.5, adding acetone, adjusting the reaction temperature to be 200-210 ℃, adding alkaline anion exchange resin, and reacting for 7-8 hours to obtain a reactant A;
adjusting the pressure of the reaction kettle to be 1.6-1.9 MPa and the temperature to be 175-185 ℃, adding the catalyst into the reactant A, and carrying out condensation reaction to obtain a reactant B;
and diluting the reactant B by adding distilled water, and then obtaining the isophorone by using a rectifying agent.
2. The method of claim 1, wherein: the method for preparing the catalyst by using the alumina as a carrier and carrying out an impregnation reaction with a potassium hydroxide solution and a magnesium nitrate solution comprises the following steps:
putting 13-32 mesh aluminum oxide into a potassium hydroxide solution, soaking at room temperature for 35-40 min, and then drying to obtain a solid A; putting the solid A into a magnesium nitrate solution, and soaking for 1-1.5h at room temperature; drying in an oven at 80 ℃, then roasting, and impregnating for multiple times to obtain the catalyst.
3. The method of claim 2, wherein: said subsequent drying to give solid a comprising:
drying in an oven at 75-90 ℃ for 3-3.5h to obtain the solid A.
4. The method of claim 2, wherein: the roasting comprises the following steps:
roasting in a furnace at 600-650 ℃ for 3-3.5 h.
5. The method of claim 1, wherein: the reaction solvent is one or more of benzene, toluene, xylene and trimethylbenzene.
6. The method of claim 1, wherein: the proportion of the alumina to the aluminum oxide is 2 (1-1.2).
7. The method of claim 1, wherein: the rectification agent comprises propylene and butane, and the component ratio of the propylene to the butane is 1 (1.2-1.5).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910643843.6A CN112239400A (en) | 2019-07-17 | 2019-07-17 | Preparation method of isophorone |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910643843.6A CN112239400A (en) | 2019-07-17 | 2019-07-17 | Preparation method of isophorone |
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| CN112239400A true CN112239400A (en) | 2021-01-19 |
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| CN201910643843.6A Pending CN112239400A (en) | 2019-07-17 | 2019-07-17 | Preparation method of isophorone |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117024258A (en) * | 2023-10-08 | 2023-11-10 | 山东富宇石化有限公司 | Method for preparing beta-isophorone by catalysis of modified X-type molecular sieve |
-
2019
- 2019-07-17 CN CN201910643843.6A patent/CN112239400A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 刘秋菊: "镁铝钾氧化物固体碱催化剂的制备、表征及合成应用", 《中国优秀硕士学位论文全文数据库工程科技I辑》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117024258A (en) * | 2023-10-08 | 2023-11-10 | 山东富宇石化有限公司 | Method for preparing beta-isophorone by catalysis of modified X-type molecular sieve |
| CN117024258B (en) * | 2023-10-08 | 2023-12-15 | 山东富宇石化有限公司 | Method for preparing beta-isophorone by catalysis of modified X-type molecular sieve |
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Application publication date: 20210119 |