CN109824499A - A kind of method that microwave reinforced photocatalysis continuously prepares acetylacetone metallic compound - Google Patents
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Abstract
A kind of method that microwave reinforced photocatalysis continuously prepares acetylacetone metallic compound, including the following steps: acetylacetone,2,4-pentanedione is mixed with metal oxide powder, obtains reaction solution after mixing evenly；The reaction solution is added in the reaction unit with reflux unit, air is then discharged out, is then heated to 50-250 DEG C, is reacted, during the reaction, carries out double catalysis；The reaction solution that step 2 is obtained is cooled to room temperature, and crystallizes reaction product, is filtered and is collected the solid matter of retention, obtain coarse crystallization；It disperses coarse crystallization in 110-125 DEG C of acetylacetone,2,4-pentanedione, obtains solution；It then, is acetylacetone metallic compound using the product that the method that microwave assisted crystallizes obtain after recrystallization processing.Method of the invention is easy to operate, the reaction time is short, mild without additional organic solvent, reaction condition.
Description
Technical field
The present invention relates to a kind of methods that microwave reinforced photocatalysis continuously prepares acetylacetone metallic compound, belong to chemical industry
Technical field.
Background technique
Acetylacetone,2,4-pentanedione, alias 2,4- pentanedione are the runny transparency liquid of colourless or micro- Huang under room temperature, there is the gas of ester
Taste congeals into glossiness crystal when cooling.When by light action, it is converted to brown liquid, and generate resin.- 23 DEG C of fusing point, boiling
Point 140.5 DEG C, relative density 0.9753, refractive index 1.4494,40.56 DEG C of flash-point, be dissolved in water, ethyl alcohol, ether, chloroform, acetone,
Benzene, glacial acetic acid.Acetylacetone,2,4-pentanedione is commonly used for solvent, organic synthesis intermediate, metal chelating agent, paint desiccant, lubricant etc..
Currently, the primary synthetic methods of acetylacetone metallic compound have solid phase method and liquid phase method two major classes, liquid phase method is
The main method of current industrial production acetylacetone metallic compound, generates second after mainly reacting by acetylacetone,2,4-pentanedione with alkali
Then metal soluble-salt is added in acyl acetone salt at a certain temperature, complex reaction occurs with acetylacetonate and generates levulinic
The method of ketone metal salt, the method are related to organic solvent, high temperature, complicated for operation etc., can generate a large amount of waste liquid and produce
The disadvantages of unstable factor is more in journey.
Chemical reaction, especially in organic synthesis, photocatalysis is that chemistry is converted into using luminous energy existing for nature instead
Required energy is answered, to generate catalytic action, has many advantages, such as safe, fast, efficient, at low cost, strong applicability.
Microwave is a kind of electromagnetic wave, and frequency is in the region 30GHz ~ 300MHz.In microwave field, microwave field energy can be direct
Go deep into inside substance, material molecule due to distribution of charges unevenly rapid electromagnetic wave absorption and generate strenuous exercise and collision, from
And it quickly reacts with adjacent molecule.It is excellent that Catalytic Technique of Microwave has that reaction condition is mild, environmental-friendly, catalytic rate is high etc.
Point, in organic synthesis field using more and more extensive.
Summary of the invention
The purpose of the present invention is to provide the sides that a kind of microwave reinforced photocatalysis continuously prepares acetylacetone metallic compound
Method.
In order to achieve the above objects and other related objects, present invention provide the technical scheme that a kind of microwave reinforced light is urged
Change the method for continuously preparing acetylacetone metallic compound, including the following steps:
Step 1: acetylacetone,2,4-pentanedione being mixed with metal oxide powder, obtains reaction solution after mixing evenly；
Step 2: the reaction solution being added in the reaction unit with reflux unit, air is then discharged out, then heats
It to 50-250 DEG C, is reacted, during the reaction, carries out following catalysis:
First catalytic stages is reacted 1/3 period for just having started the period, in environment locating for reaction solution, microwave frequency
For 2450MHz, intensity 2.0-2.5w/cm2, intensity of illumination is ten thousand Lx of 50-100；
Second catalytic stages is reacted 1/3 period of intermediate period, in environment locating for reaction solution, microwave frequency is
2450MHz, intensity 1.5-2.0w/cm2, intensity of illumination is ten thousand Lx of 10-50；
Third catalytic stages are reacted 1/3 period of later moments, in environment locating for reaction solution, microwave frequency is
2450MHz, intensity 0.5-1.5w/cm2, intensity of illumination is ten thousand Lx of 1-10；
Step 3: the reaction solution that step 2 is obtained is cooled to room temperature, and crystallizes reaction product, filters and collect the solid of retention
Substance obtains coarse crystallization；
Step 4: dispersing coarse crystallization in 110-125 DEG C of acetylacetone,2,4-pentanedione, obtain solution；Then, it is crystallized using microwave assisted
The product that obtained after recrystallization processing of method be acetylacetone metallic compound.
Preferred technical solution are as follows: the metal oxide is selected from calcium oxide, magnesia, aluminium oxide, iron oxide, oxidation
Zinc, vanadium oxide, molybdenum oxide, lithia, zirconium oxide, nickel oxide, manganese oxide, cobalt oxide, chromium oxide, copper oxide, titanium oxide, oxidation
Beryllium, barium monoxide, lead oxide, gallium oxide, indium oxide, hafnium oxide.
Preferred technical solution are as follows: the molar ratio 5:1-10:1 between the acetylacetone,2,4-pentanedione and metal oxide.
Preferred technical solution are as follows: the reaction time of step 2 is 0.5-2.0h.
Preferred technical solution are as follows: the recrystallization processing includes the following steps:
S1, when the reaction solution temperature is down to 80-85 DEG C, using frequency 2450MHz, intensity 0.25-1.0w/cm2It is micro-
Wave field handles 15-30s；
S2, when the reaction solution temperature is down to 60-65 DEG C, using frequency 2450MHz, intensity 0.25-1.0w/cm2It is micro-
Wave field handles 15-30s；
S3, when the reaction solution temperature is down to 40-45 DEG C, using frequency 2450MHz, intensity 0.25-1.0w/cm2It is micro-
Wave field handles 15-30s；
S4, when the reaction is cooled to room temperature, recrystallized, filter and collect the solid matter of retention to get to levulinic
Ketone metallic compound.
Preferred technical solution are as follows: further include collect with reuse acetylacetone,2,4-pentanedione step, will step 3 separate coarse crystallization after it is anti-
Acetylacetone,2,4-pentanedione solution after answering solution to recrystallize with step 4 mixes, and obtains recycling mixed liquor, spare；Then at room temperature to return
The active carbon for adding its quality 5-10% in mixed liquor is received, mixes uniformly, places 90-120min, then use the sieve of 80-100 mesh
Net filtration obtains filtrate, finally carries out rectifying purification process to the filtrate, collects 138-141 DEG C of fraction.
Preferred technical solution are as follows: the acetylacetone,2,4-pentanedione is the acetylacetone,2,4-pentanedione of 138-141 DEG C of fraction.
Since above-mentioned technical proposal is used, the present invention has the advantage, that compared with prior art
1, the present invention develops a kind of microwave reinforced for the disadvantage in current industrial production acetylacetone metallic compound method
Acetylacetone,2,4-pentanedione had not only been used as solvent but also had been used as reactant by the method that photocatalysis continuously prepares acetylacetone metallic compound, was utilized
Complexing of the microwave field density photocatalysis acetylacetone,2,4-pentanedione to metal ion, while recycling acetylacetone,2,4-pentanedione and continuing on for lower batch production,
To realize high efficiency, the serialization of operation.The inventive method is easy to operate, the reaction time is short, without additional organic solvent, reaction
Mild condition.
2, acetylacetone metallic compound product prepared by the method for the present invention, in PVC auxiliary heat stabilizer, catalyst,
Resin cross-linking agent, hardening of resin promotor, resin, rubber additive, super conducting membranes, hotline-reflective glass film, electrically conducting transparent
The fields such as the forming agent of film are with a wide range of applications.
Specific embodiment
Embodiments of the present invention are illustrated by particular specific embodiment below, those skilled in the art can be by this explanation
Content disclosed by book is understood other advantages and efficacy of the present invention easily.
The term of such as "upper", "lower", "left", "right", " centre " and " one " cited in this specification, is also only just
In being illustrated for narration, rather than to limit the scope of the invention, relativeness is altered or modified, without substantive change
Under more technology contents, when being also considered as the enforceable scope of the present invention.
A kind of embodiment 1: method that microwave reinforced photocatalysis continuously prepares acetylacetone metallic compound
A kind of method that microwave reinforced photocatalysis continuously prepares acetylacetone metallic compound, which is characterized in that including following skill
Art content.
(1) pretreatment of raw material
By metal oxide by crushing, sieving processing, wherein sieve aperture is 50-80 mesh, collects metallic oxide fine powder, standby
With.The metal oxide is calcium oxide, magnesia, aluminium oxide, iron oxide, zinc oxide, vanadium oxide, molybdenum oxide, oxidation
Lithium, zirconium oxide, nickel oxide, manganese oxide, cobalt oxide, chromium oxide, copper oxide, titanium oxide, beryllium oxide, barium monoxide, lead oxide, oxidation
One of gallium, indium oxide, hafnium oxide.
Acetylacetone,2,4-pentanedione is subjected to rectifying purifying, collects 138-141 DEG C of fraction, it is spare.
(2) reaction solution is prepared
Acetylacetone,2,4-pentanedione both as reaction complexing agent, was also used as reaction dissolvent.Pretreated acetylacetone,2,4-pentanedione, metal oxide are pressed
Molar ratio 7.5:1 mixing, stirring or shaken well, obtain reaction solution.The metal oxide of the present embodiment is specially to aoxidize
Zinc.
(3) reaction unit is set up
Reaction solution is placed into the reaction unit with reflux unit, the reaction unit can be heated simultaneously, light
According to, microwave treatment, i.e. the reaction vessel of reaction unit such as balloon flask can be put into microwave device, and high-pressure sodium lamp can also will
Light is irradiated on the reaction solution in balloon flask；Nitrogen (or a certain amount of liquid nitrogen is added), emptying are filled with into reaction vessel
Air.
(4) composite catalyzing reacts
It is 150 DEG C that reaction temperature, which is arranged, using composite catalyzing method, reaction time 1.25h.
The composite catalyzing is microwave catalysis and the catalysis process that photocatalysis carries out simultaneously.Composite catalyzing is divided into three
Reaction time is uniformly divided into three time phases, each time phase, using different catalytic conditions by the stage.
First catalytic stages is reacted 1/3 period for just having started the period, in environment locating for reaction solution, microwave
Frequency is 2450MHz, intensity 2.2w/cm2, intensity of illumination is 7,500,000 Lx.
Second catalytic stages is reacted 1/3 period of intermediate period, in environment locating for reaction solution, Microwave Frequency
Rate is 2450MHz, intensity 1.7w/cm2, intensity of illumination is 300,000 Lx.
Third catalytic stages are reacted 1/3 period of later moments, in environment locating for reaction solution, Microwave Frequency
Rate is 2450MHz, intensity 1w/cm2, intensity of illumination is 50,000 Lx.
The photocatalysis, light source is from high-pressure sodium lamp.
(5) refining reaction product
After reaction, reaction solution is cooled to room temperature, crystallizes reaction product, filtered using 60 mesh filter screens and collect retention
Solid matter, obtain coarse crystallization.
Coarse crystallization is dissolved in 115 DEG C of acetylacetone,2,4-pentanediones of same molar, solution is obtained.Then, using microwave assisted
The method of crystallization carries out recrystallization processing, and the specific method is as follows: solution is in natural cooling state；When solution temperature is down to 82
DEG C when, using frequency 2450MHz, intensity 0.65w/cm2Microwave field handle 20s；When solution temperature is down to 62 DEG C, using frequency
Rate 2450MHz, intensity 0.65w/cm2Microwave field handle 20s；When solution temperature is down to 42 DEG C, using frequency 2450MHz, by force
Spend 0.65w/cm2Microwave field handle 20s；Solution is cooled to room temperature, and is recrystallized, and 60 mesh filter screens filter and collect retention
Solid matter is to get the acetylacetone metallic compound product for arriving purification.
(6) it collects and reuse acetylacetone,2,4-pentanedione
It collects.Reaction solution, the metallization of separating acetyl acetone after collecting separating acetyl acetone metallic compound coarse crystallization respectively
Acetylacetone,2,4-pentanedione solution after closing object recrystallization, above two solution is mixed, and obtains recycling mixed liquor, spare.
Treatment for Reuse.The active carbon of its quality 7m% is added in the first step, activated carbon adsorption into recycling mixed liquor at room temperature,
It mixes uniformly, places 105min.Second step, filtering will recycle mixed liquor and Mixture of Activated Carbon at room temperature and filter by 90 mesh.
Filtered material is carried out rectifying purification process, collects 138-141 DEG C of fraction by third step, rectifying purifying.By above-mentioned processing
Collected fraction afterwards can be used as the reaction complexing agent and reaction dissolvent of acetylacetone metallic compound again.
A kind of embodiment 2: method that microwave reinforced photocatalysis continuously prepares acetylacetone metallic compound
A kind of method that microwave reinforced photocatalysis continuously prepares acetylacetone metallic compound, including the following steps:
Step 1: acetylacetone,2,4-pentanedione being mixed with metal oxide powder, obtains reaction solution after mixing evenly；
Step 2: the reaction solution being added in the reaction unit with reflux unit, air is then discharged out, then heats
It to 50 DEG C, is reacted, during the reaction, carries out following catalysis:
First catalytic stages is reacted 1/3 period for just having started the period, in environment locating for reaction solution, microwave frequency
For 2450MHz, intensity 2.0w/cm2, intensity of illumination is 500,000 Lx；
Second catalytic stages is reacted 1/3 period of intermediate period, in environment locating for reaction solution, microwave frequency is
2450MHz, intensity 1.5w/cm2, intensity of illumination is 100,000 Lx；
Third catalytic stages are reacted 1/3 period of later moments, in environment locating for reaction solution, microwave frequency is
2450MHz, intensity 0.5w/cm2, intensity of illumination is 10,000 Lx；
Step 3: the reaction solution that step 2 is obtained is cooled to room temperature, and crystallizes reaction product, filters and collect the solid of retention
Substance obtains coarse crystallization；
Step 4: dispersing coarse crystallization in 110 DEG C of acetylacetone,2,4-pentanedione, obtain solution；Then, the side crystallized using microwave assisted
The product that method obtain after recrystallization processing is acetylacetone metallic compound.
Preferred embodiment are as follows: the metal oxide zinc and lithia are constituted according to the mass ratio of 1:1
Mixture.
Preferred embodiment are as follows: the molar ratio 5:1 between the acetylacetone,2,4-pentanedione and metal oxide.
Preferred embodiment are as follows: the reaction time of step 2 is 0.5h.
Preferred embodiment are as follows: the recrystallization processing includes the following steps:
S1, when the reaction solution temperature is down to 80 DEG C, using frequency 2450MHz, intensity 0.25w/cm2Microwave field processing
15s；
S2, when the reaction solution temperature is down to 60 DEG C, using frequency 2450MHz, intensity 0.25w/cm2Microwave field processing
15s；
S3, when the reaction solution temperature is down to 40 DEG C, using frequency 2450MHz, intensity 0.25w/cm2Microwave field processing
15s；
S4, when the reaction is cooled to room temperature, recrystallized, filter and collect the solid matter of retention to get to levulinic
Ketone metallic compound.
Preferred embodiment are as follows: further include collect with reuse acetylacetone,2,4-pentanedione step, will step 3 separate coarse crystallization after it is anti-
Acetylacetone,2,4-pentanedione solution after answering solution to recrystallize with step 4 mixes, and obtains recycling mixed liquor, spare；Then at room temperature to return
The active carbon for adding its quality 5% in mixed liquor is received, mixes uniformly, places 90min, then obtained using the screen to filtrate of 80 mesh
Filtrate finally carries out rectifying purification process to the filtrate, collects 138-141 DEG C of fraction.
Preferred technical solution are as follows: the acetylacetone,2,4-pentanedione is the acetylacetone,2,4-pentanedione of 138-141 DEG C of fraction.
A kind of embodiment 3: method that microwave reinforced photocatalysis continuously prepares acetylacetone metallic compound
A kind of method that microwave reinforced photocatalysis continuously prepares acetylacetone metallic compound, including the following steps:
Step 1: acetylacetone,2,4-pentanedione being mixed with metal oxide powder, obtains reaction solution after mixing evenly；
Step 2: the reaction solution being added in the reaction unit with reflux unit, air is then discharged out, then heats
It to 250 DEG C, is reacted, during the reaction, carries out following catalysis:
First catalytic stages is reacted 1/3 period for just having started the period, in environment locating for reaction solution, microwave frequency
For 2450MHz, intensity 2.5w/cm2, intensity of illumination is 1,000,000 Lx；
Second catalytic stages is reacted 1/3 period of intermediate period, in environment locating for reaction solution, microwave frequency is
2450MHz, intensity 2.0w/cm2, intensity of illumination is 500,000 Lx；
Third catalytic stages are reacted 1/3 period of later moments, in environment locating for reaction solution, microwave frequency is
2450MHz, intensity 1.5w/cm2, intensity of illumination is 100,000 Lx；
Step 3: the reaction solution that step 2 is obtained is cooled to room temperature, and crystallizes reaction product, filters and collect the solid of retention
Substance obtains coarse crystallization；
Step 4: dispersing coarse crystallization in 125 DEG C of acetylacetone,2,4-pentanedione, obtain solution；Then, the side crystallized using microwave assisted
The product that method obtain after recrystallization processing is acetylacetone metallic compound.
Preferred embodiment are as follows: the metal oxide copper.
Preferred embodiment are as follows: the molar ratio 10:1 between the acetylacetone,2,4-pentanedione and metal oxide.
Preferred embodiment are as follows: the reaction time of step 2 is 2.0h.
Preferred embodiment are as follows: the recrystallization processing includes the following steps:
S1, when the reaction solution temperature is down to 85 DEG C, using frequency 2450MHz, intensity 1.0w/cm2Microwave field processing
30s；
S2, when the reaction solution temperature is down to 65 DEG C, using frequency 2450MHz, intensity 1.0w/cm2Microwave field processing
30s；
S3, when the reaction solution temperature is down to 45 DEG C, using frequency 2450MHz, intensity 1.0w/cm2Microwave field processing
30s；
S4, when the reaction is cooled to room temperature, recrystallized, filter and collect the solid matter of retention to get to levulinic
Ketone metallic compound.
Preferred embodiment are as follows: further include collect with reuse acetylacetone,2,4-pentanedione step, will step 3 separate coarse crystallization after it is anti-
Acetylacetone,2,4-pentanedione solution after answering solution to recrystallize with step 4 mixes, and obtains recycling mixed liquor, spare；Then at room temperature to return
The active carbon for adding its quality 10% in mixed liquor is received, mixes uniformly, places 120min, then obtained using the screen to filtrate of 100 mesh
To filtrate, rectifying purification process finally is carried out to the filtrate, collects 138-141 DEG C of fraction.
Preferred technical solution are as follows: the acetylacetone,2,4-pentanedione is the acetylacetone,2,4-pentanedione of 138-141 DEG C of fraction.
As described above is only to be not intended to tool to explain the preferred embodiments of the invention to do any shape to the present invention
Limitation in formula should all wrap therefore all have any modification or change for making the related present invention under identical spirit
It includes in the scope that the invention is intended to protect.
Claims (7)
1. a kind of method that microwave reinforced photocatalysis continuously prepares acetylacetone metallic compound, it is characterised in that: including following
Step:
Step 1: acetylacetone,2,4-pentanedione being mixed with metal oxide powder, obtains reaction solution after mixing evenly；
Step 2: the reaction solution being added in the reaction unit with reflux unit, air is then discharged out, then heats
It to 50-250 DEG C, is reacted, during the reaction, carries out following catalysis:
First catalytic stages is reacted 1/3 period for just having started the period, in environment locating for reaction solution, microwave frequency
For 2450MHz, intensity 2.0-2.5w/cm2, intensity of illumination is ten thousand Lx of 50-100；
Second catalytic stages is reacted 1/3 period of intermediate period, in environment locating for reaction solution, microwave frequency is
2450MHz, intensity 1.5-2.0w/cm2, intensity of illumination is ten thousand Lx of 10-50；
Third catalytic stages are reacted 1/3 period of later moments, in environment locating for reaction solution, microwave frequency is
2450MHz, intensity 0.5-1.5w/cm2, intensity of illumination is ten thousand Lx of 1-10；
Step 3: the reaction solution that step 2 is obtained is cooled to room temperature, and crystallizes reaction product, filters and collect the solid of retention
Substance obtains coarse crystallization；
Step 4: dispersing coarse crystallization in 110-125 DEG C of acetylacetone,2,4-pentanedione, obtain solution；Then, it is crystallized using microwave assisted
The product that obtained after recrystallization processing of method be acetylacetone metallic compound.
2. the method that microwave reinforced photocatalysis according to claim 1 continuously prepares acetylacetone metallic compound, special
Sign is: the metal oxide is selected from calcium oxide, magnesia, aluminium oxide, iron oxide, zinc oxide, vanadium oxide, molybdenum oxide, oxygen
Change lithium, zirconium oxide, nickel oxide, manganese oxide, cobalt oxide, chromium oxide, copper oxide, titanium oxide, beryllium oxide, barium monoxide, lead oxide, oxygen
Change gallium, indium oxide, hafnium oxide.
3. the method that microwave reinforced photocatalysis according to claim 1 continuously prepares acetylacetone metallic compound, special
Sign is: the molar ratio 5:1-10:1 between the acetylacetone,2,4-pentanedione and metal oxide.
4. the method that microwave reinforced photocatalysis according to claim 1 continuously prepares acetylacetone metallic compound, special
Sign is: the reaction time of step 2 is 0.5-2.0h.
5. the method that microwave reinforced photocatalysis according to claim 1 continuously prepares acetylacetone metallic compound, special
Sign is: the recrystallization processing includes the following steps:
S1, when the reaction solution temperature is down to 80-85 DEG C, using frequency 2450MHz, intensity 0.25-1.0w/cm2Microwave
Field processing 15-30s；
S2, when the reaction solution temperature is down to 60-65 DEG C, using frequency 2450MHz, intensity 0.25-1.0w/cm2Microwave
Field processing 15-30s；
S3, when the reaction solution temperature is down to 40-45 DEG C, using frequency 2450MHz, intensity 0.25-1.0w/cm2Microwave
Field processing 15-30s；
S4, when the reaction is cooled to room temperature, recrystallized, filter and collect the solid matter of retention to get to levulinic
Ketone metallic compound.
6. the method that microwave reinforced photocatalysis according to claim 1 continuously prepares acetylacetone metallic compound, special
Sign is: further including collecting to tie again with reuse acetylacetone,2,4-pentanedione step, the reaction solution after step 3 to be separated to coarse crystallization with step 4
Acetylacetone,2,4-pentanedione solution mixing after crystalline substance obtains recycling mixed liquor, spare；Then its matter is added into recycling mixed liquor at room temperature
The active carbon for measuring 5-10% is mixed uniformly, places 90-120min, then obtains filtrate using the screen to filtrate of 80-100 mesh, most
Rectifying purification process is carried out to the filtrate afterwards, collects 138-141 DEG C of fraction.
7. the method that microwave reinforced photocatalysis according to claim 1 continuously prepares acetylacetone metallic compound, special
Sign is: the acetylacetone,2,4-pentanedione is the acetylacetone,2,4-pentanedione of 138-141 DEG C of fraction.
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| CN111848381A (en) * | 2020-08-10 | 2020-10-30 | 中山华明泰科技股份有限公司 | Preparation method and application of copper acetylacetonate |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111848381A (en) * | 2020-08-10 | 2020-10-30 | 中山华明泰科技股份有限公司 | Preparation method and application of copper acetylacetonate |
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