CN102659550A - Method for producing acetylacetone beryllium - Google Patents
Method for producing acetylacetone beryllium Download PDFInfo
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- CN102659550A CN102659550A CN2012101586035A CN201210158603A CN102659550A CN 102659550 A CN102659550 A CN 102659550A CN 2012101586035 A CN2012101586035 A CN 2012101586035A CN 201210158603 A CN201210158603 A CN 201210158603A CN 102659550 A CN102659550 A CN 102659550A
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- methyl ethyl
- beryllium
- ethyl diketone
- reaction kettle
- oxide powder
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Abstract
The invention relates to a method for producing a compound, in particular to a method for producing acetylacetone beryllium. The method comprises the steps of: dispersing beryllium oxide powder into solvent in a reaction kettle; adding acetylacetone into the reaction kettle, and carrying out reaction under the temperature condition of 50-80 DEG C; filtering while being hot, cooling filtrate and filtering again; and drying to obtain acetylacetone beryllium. The product obtained by the method is high in purity and fine in particles; and the yield is 90-95%, and the product purity reaches 99%. The method is fewer in steps, simple in technology, less in dosage of acetylacetone and low in production cost; and isopropanol or ethanol is used as solvent and can be recycled, so that the environment is not influenced.
Description
Technical field
The present invention relates to a kind of working method of compound.
Background technology
In the prior art, a kind of compound is arranged, its Chinese: the methyl ethyl diketone beryllium; English name: Beryllium acetylacetonate, be called for short Be (acac)
2CAS:NO 10210-64-7; Molecular formula: C
10H
14BeO
4Molecular weight: 207.23; Physico-chemical property: these article are colourless monoclinic crystal.Be soluble in multiple organic solvents such as methyl alcohol, ethanol, acetone, ether, benzene, dithiocarbonic anhydride, chloroform, water insoluble, but can be by the boiling water hydrolysis.109 ℃ of fusing points; 270 ℃ of boiling points.Specific density 1.168.White crystal; Purposes: be the CVD plated film, carried catalyst, contain the desirable presoma of materials such as beryllium pottery, fibre containing beryllium in synthetic, wide application prospect is arranged at novel material and field of fine chemical.
The working method of existing methyl ethyl diketone beryllium is following: with the strong sulfuric acid response of beryllium oxide powder with heat, behind distilled water diluting, dropping sodium is regulated pH between 6.0～8.0; Dropwise add methyl ethyl diketone then; Heating in water bath, temperature are 90 ℃, react to obtain colourless throw out after 5 hours; After washing, vacuum-drying, obtain product, productive rate 80～85%.Its weak point is: (1) this working method productive rate is low, has inorganic salt to generate in the reaction, handles bad meeting environment is polluted; (2) obtaining to need recrystallization before the product, its complex process, production efficiency is low, and productive rate is merely 80～85%; (3) adopt water as solvent, its consumption is big, and aftertreatment is difficult, is difficult for recycling use, is prone to environment is caused detrimentally affect; (4) beryllium has very big toxicity, causes environmental pollution.
Summary of the invention
The working method of the methyl ethyl diketone beryllium that the object of the present invention is to provide that a kind of productive rate is high, technology is simple, environment not have influence.
The present invention includes following steps:
1, in reaction kettle, the beryllium oxide powder is scattered in the solvent;
2, add methyl ethyl diketone to aforesaid reaction vessel, reaction under 50～80 ℃ of temperature condition;
3, filtered while hot refilters after getting filtrating cooling, through dry, obtains the methyl ethyl diketone beryllium.
Compared with prior art, by product of the present invention is a water, and product is purified convenient, and product purity is high; Its productive rate obviously improves, and can reach 90～95%; In addition, need not to carry out the recrystallizing technology process, can directly obtain product, reduced process step, reduced technology difficulty, product purity is up to 99%.
In addition, solvent can be selected Virahol or ethanol for use described in the step 1 of the present invention, can be recycled or recycles solvent, to not influence of environment.
For the beryllium oxide powder is well-dispersed in the solvent, be beneficial to abundant reaction, the present invention adds the beryllium oxide powder after earlier solvent being warming up to 50～70 ℃ in reaction kettle again, disperses through stirring fully.
For abundant reaction, in step 2 according to the invention, methyl ethyl diketone is added dropwise in the reaction kettle.
In addition, in step 2, the mass ratio of the methyl ethyl diketone of adding and beryllium oxide powder is 8～12.5: 1, and the consumption of producing methyl ethyl diketone than prior art has reduced by 1.8～2.5 times, is beneficial to the reduction production cost of products.
The preferable reaction temperature condition of step 2 of the present invention is 60～80 ℃.
Reaction equation of the present invention is:
Description of drawings
Fig. 1 is the methyl ethyl diketone beryllium product infrared spectrum of product of the present invention.
Embodiment
One, production example:
Embodiment 1
The Virahol that in reaction kettle, adds 45kg is made solvent, is warming up to 50～60 ℃, under agitation in reaction kettle, adds the beryllium oxide powder of 2.4kg; The beryllium oxide powder is dispersed in the Virahol, drips the methyl ethyl diketone of 22kg again, temperature is controlled at 50～60 ℃; Until drip finishing, reaction kettle is suitably heated up, 60 ℃ of insulation reaction 5 hours; Filtered while hot, remove a spot of insolubles, refilter after the filtrating cooling, filter cake dries or vacuum-drying gets clear crystal 18.38kg; Be product, productive rate 92.5%.
Embodiment 2
The ethanol that in reaction kettle, adds 50kg is made solvent, is warming up to 50～60 ℃, under agitation in reaction kettle, adds the beryllium oxide powder of 2.5kg; The beryllium oxide powder is dispersed in the ethanol, drips the methyl ethyl diketone of 20kg again, temperature is controlled at 50～60 ℃; Until drip finishing, reaction kettle is suitably heated up, 70 ℃ of insulation reaction 3.5 hours; Filtered while hot, remove a spot of insolubles, refilter after the filtrating cooling, filter cake dries or vacuum-drying gets clear crystal 18.94kg; Be product, productive rate 91.5%.
Embodiment 3
The ethanol that in reaction kettle, adds 55kg is made solvent, is warming up to 50～70 ℃, under agitation in reaction kettle, adds the beryllium oxide powder of 2.5kg; The beryllium oxide powder is dispersed in the ethanol, drips the methyl ethyl diketone of 24kg again, temperature is controlled at 50～70 ℃; Until drip finishing, reaction kettle is suitably heated up, 75 ℃ of insulation reaction 4 hours; Filtered while hot, remove a spot of insolubles, refilter after the filtrating cooling, filter cake dries or vacuum-drying gets clear crystal 19.42kg; Be product, productive rate 93.8%.
Embodiment 4
The Virahol that in reaction kettle, adds 50kg is made solvent, is warming up to 50～70 ℃, under agitation in reaction kettle, adds the beryllium oxide powder of 2.4kg; The beryllium oxide powder is dispersed in the Virahol, drips the methyl ethyl diketone of 20kg again, temperature is controlled at 50～70 ℃; Until drip finishing, reaction kettle is suitably heated up, 70 ℃ of insulation reaction 5 hours; Filtered while hot, remove a spot of insolubles, refilter after the filtrating cooling, filter cake dries or vacuum-drying gets clear crystal 18.74kg; Be product, productive rate 94.3%.
Embodiment 5
The ethanol that in reaction kettle, adds 52kg is made solvent, is warming up to 50～70 ℃, under agitation in reaction kettle, adds the beryllium oxide powder of 2.3kg; The beryllium oxide powder is dispersed in the ethanol, drips the methyl ethyl diketone of 20.5kg again, temperature is controlled at 50～70 ℃; Until drip finishing, reaction kettle is suitably heated up, 70 ℃ of insulation reaction 3.5 hours; Filtered while hot, remove a spot of insolubles, refilter after the filtrating cooling, filter cake dries or vacuum-drying gets clear crystal 17.83kg; Be product, productive rate 93.6%.
Embodiment 6
The Virahol that in reaction kettle, adds 53kg is made solvent, is warming up to 50～70 ℃, under agitation in reaction kettle, adds the beryllium oxide powder of 2.2kg; The beryllium oxide powder is dispersed in the Virahol, drips the methyl ethyl diketone of 20kg again, temperature is controlled at 50～70 ℃; Until drip finishing, reaction kettle is suitably heated up, 75 ℃ of insulation reaction 4.5 hours; Filtered while hot, remove a spot of insolubles, refilter after the filtrating cooling, filter cake dries or vacuum-drying gets clear crystal 17.16kg; Be product, productive rate 94.2%.
Embodiment 7
The ethanol that in reaction kettle, adds 56kg is made solvent, is warming up to 50～60 ℃, under agitation in reaction kettle, adds the beryllium oxide powder of 2.2kg; The beryllium oxide powder is dispersed in the ethanol,, drip the methyl ethyl diketone of 22kg again; Temperature is controlled at 50～60 ℃, finishes until dripping, and reaction kettle is suitably heated up; 70 ℃ of insulation reaction 3.5 hours, filtered while hot, remove a spot of insolubles, refilter after the filtrating cooling; Filter cake dries or vacuum-drying gets clear crystal 16.90kg, is product, productive rate 92.8%.
Embodiment 8
The Virahol that in reaction kettle, adds 48kg is made solvent, is warming up to 50～70 ℃, under agitation in reaction kettle, adds the beryllium oxide powder of 2.2kg; The beryllium oxide powder is dispersed in the Virahol, drips the methyl ethyl diketone of 25kg again, temperature is controlled at 50～70 ℃; Until drip finishing, reaction kettle is suitably heated up, 70 ℃ of insulation reaction 5 hours; Filtered while hot, remove a spot of insolubles, refilter after the filtrating cooling, filter cake dries or vacuum-drying gets clear crystal 17.00kg; Be product, productive rate 93.3%.
Embodiment 9
The Virahol that in reaction kettle, adds 55kg is made solvent, is warming up to 50～70 ℃, under agitation in reaction kettle, adds the beryllium oxide powder of 2.0kg; The beryllium oxide powder is dispersed in the Virahol, drips the methyl ethyl diketone of 25kg again, temperature is controlled at 50～70 ℃; Until drip finishing, reaction kettle is suitably heated up, 80 ℃ of insulation reaction 5 hours; Filtered while hot, remove a spot of insolubles, refilter after the filtrating cooling, filter cake dries or vacuum-drying gets clear crystal 15.75kg; Be product, productive rate 95.1%.
Embodiment 10
The ethanol that in reaction kettle, adds 58kg is made solvent, is warming up to 50～70 ℃, under agitation in reaction kettle, adds the beryllium oxide powder of 2.1kg; The beryllium oxide powder is dispersed in the ethanol, drips the methyl ethyl diketone of 25kg again, temperature is controlled at 50～70 ℃; Until drip finishing, reaction kettle is suitably heated up, 80 ℃ of insulation reaction 5 hours; Filtered while hot, remove a spot of insolubles, refilter after the filtrating cooling, filter cake dries or vacuum-drying gets clear crystal 16.48kg; Be product, productive rate 94.8%.
Two, product is identified:
Clear crystal product that above each example is produced is tested through infrared spectrum, as shown in Figure 1, on spectrogram, found the charateristic avsorption band of methyl ethyl diketone beryllium as shown in the table, confirmed that the product of producing is the methyl ethyl diketone beryllium.
Claims (6)
1. the working method of a methyl ethyl diketone beryllium is characterized in that may further comprise the steps:
1) in reaction kettle, the beryllium oxide powder is scattered in the solvent;
2) add methyl ethyl diketone to aforesaid reaction vessel, reaction under 50～80 ℃ of temperature condition;
3) filtered while hot refilters after getting filtrating cooling, through dry, obtains the methyl ethyl diketone beryllium.
2. according to the working method of the said methyl ethyl diketone beryllium of claim 1, it is characterized in that solvent described in the step 1) is Virahol or ethanol.
3. according to the working method of claim 1 or 2 said methyl ethyl diketone berylliums, after it is characterized in that earlier solvent being warming up to 50～70 ℃ in reaction kettle, add the beryllium oxide powder again, disperse through stirring fully.
4. according to the working method of the said methyl ethyl diketone beryllium of claim 1, it is characterized in that said step 2) in, said methyl ethyl diketone is added dropwise in the reaction kettle.
5. according to the working method of claim 1 or 2 or 4 said methyl ethyl diketone berylliums, it is characterized in that said step 2) in, the mass ratio of the methyl ethyl diketone of adding and beryllium oxide powder is 8～12.5: 1.
6. according to the working method of the said methyl ethyl diketone beryllium of claim 1, it is characterized in that said step 2) the temperature of reaction condition be 60～80 ℃.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2012101586035A CN102659550A (en) | 2012-05-22 | 2012-05-22 | Method for producing acetylacetone beryllium |
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| CN2012101586035A CN102659550A (en) | 2012-05-22 | 2012-05-22 | Method for producing acetylacetone beryllium |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106748697A (en) * | 2016-12-09 | 2017-05-31 | 湖南博翔新材料有限公司 | A kind of preparation method of acetylacetone,2,4-pentanedione beryllium |
| CN106916311A (en) * | 2015-12-24 | 2017-07-04 | 中南大学 | A kind of preparation method containing beryllium ceramic precursor |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1044953A1 (en) * | 1998-07-10 | 2000-10-18 | Daicel Chemical Industries, Ltd. | Process for the preparation of alkaline earth metal salts of beta-diketo compounds |
| CN101857537A (en) * | 2010-06-10 | 2010-10-13 | 扬州工业职业技术学院 | Method for preparing ferric acetyl acetonade |
-
2012
- 2012-05-22 CN CN2012101586035A patent/CN102659550A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1044953A1 (en) * | 1998-07-10 | 2000-10-18 | Daicel Chemical Industries, Ltd. | Process for the preparation of alkaline earth metal salts of beta-diketo compounds |
| CN101857537A (en) * | 2010-06-10 | 2010-10-13 | 扬州工业职业技术学院 | Method for preparing ferric acetyl acetonade |
Non-Patent Citations (2)
| Title |
|---|
| 刘青宝: "乙酰丙酮金属化合物合成及其对PVC的热稳定作用研究", 《北京化工大学硕士研究生学位论文》 * |
| 杨兵初等: "乙酰丙酮铍的合成与结构研究", 《北京化工大学学报（自然科学版）》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106916311A (en) * | 2015-12-24 | 2017-07-04 | 中南大学 | A kind of preparation method containing beryllium ceramic precursor |
| CN106748697A (en) * | 2016-12-09 | 2017-05-31 | 湖南博翔新材料有限公司 | A kind of preparation method of acetylacetone,2,4-pentanedione beryllium |
| CN106748697B (en) * | 2016-12-09 | 2020-02-21 | 湖南博翔新材料有限公司 | Preparation method of acetylacetone beryllium |
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Application publication date: 20120912 |