CN1746180A - Preparation of acetylacetone cobalt - Google Patents
Preparation of acetylacetone cobalt Download PDFInfo
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- CN1746180A CN1746180A CN 200510070769 CN200510070769A CN1746180A CN 1746180 A CN1746180 A CN 1746180A CN 200510070769 CN200510070769 CN 200510070769 CN 200510070769 A CN200510070769 A CN 200510070769A CN 1746180 A CN1746180 A CN 1746180A
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- cobalt
- methyl ethyl
- acetylacetone
- preparation
- ethyl diketone
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Abstract
Production of cobalt acetylacetone is carried out by reacting soluble ceramic cobalt blue solution with NAOH solution to generate cobaltous hydroxide deposit, and adding into acetylacetone to generate cobaltous acetylacetone crystal at 130 Deg C.. It achieves simple process, higher production efficiency and recovery rate.
Description
Technical field:
The present invention relates to a kind of method that methyl ethyl diketone carries out the prepared in reaction acetylacetone cobalt that directly in the reaction mixture of solubility cobalt salt solution and alkaline solution, adds.
Technical background:
Acetylacetone cobalt is a kind of noble metal organic coordination compounds, it is dissolved in organic solvent is mixed with the catalyzer that organic dipping solution dipping porous carrier can prepare the cobalt high dispersing.Because the organic solution catalyst prepared has very high activity, so acetylacetone cobalt has obtained to use comparatively widely at catalytic field.
Document [1] U.S. Pat P 20040127690 has reported a kind of preparation method of acetylacetone cobalt.This method is soluble salt solution and the NaOH solution reaction generation cobaltous hydroxide precipitation of elder generation with cobalt, then precipitation is carried out thorough washing to remove the alkali of absorption fully, under the reflux temperature about 130 ℃, react generation acetylacetone cobalt crystal with purified cobaltous hydroxide pressed powder and methyl ethyl diketone at last.The characteristics of this method are at first to prepare purified cobaltous hydroxide, and then generate acetylacetone cobalt with the methyl ethyl diketone reaction, and its technology comprises two main processes, and operation is comparatively complicated.At present, the report of relevant acetylacetone based metal complexes is few, and there are shortcomings such as preparation facilities complexity, many, the time-consuming length of operation steps, product yield are low in existing preparation method.
Summary of the invention:
The objective of the invention is in order to overcome the shortcoming that existing acetylacetone cobalt technology of preparing exists, a kind of new preparation process of easy to operate, preparation technology is simple and product yield is high acetylacetone cobalt is provided.
The present invention generates the cobaltous hydroxide precipitation with the soluble salt solution and the NaOH solution reaction of cobalt, without separation of hydrogen cobalt oxide precipitation, directly adds methyl ethyl diketone and makes it react generation acetylacetone cobalt crystal under the reflux temperature about 130 ℃.The present invention controls the transforming degree of main reaction and side reaction by the consumption of adjusting precipitation process alkali and the consumption that changes brilliant process methyl ethyl diketone, thereby promotes the yield of main reaction, raising acetylacetone cobalt.
Concrete preparation method is as follows:
A. in the reactor that has chuck and whipping appts the solubility cobalt salt being dissolved in deionized water preparation cobalt salt concentration is the solution of 10-20wt%, other makes, and NaOH is water-soluble to be made into the alkaline solution that concentration is 5-15wt%, and under room temperature and vigorous stirring alkaline solution being joined the pH value that makes reaction mixture in the cobalt salt solution is 7～10.Cobalt salt solution and NaOH solution reaction initial stage generate blue precipitation, are transformed into green after 15 minutes, continue stirring and generate the baby pink cobaltous hydroxide.Reacting used solubility cobalt salt can be crystallization cobalt chloride (CoCl
26H
2O) or crystallization Xiao Suangu (Co (NO
3)
26H
2O) etc.
B. in the mol ratio of cobaltous hydroxide/methyl ethyl diketone 1/2 ratio, the cobaltous hydroxide that generates with steps A is precipitated as benchmark, measuring excessive 1～5 times methyl ethyl diketone adds in the above-mentioned reactor, be warming up to reflux temperature and under 600～2500 rev/mins stirring velocity back flow reaction 2～3h, have pinkish acetylacetone cobalt crystal to generate in the process.
C. with the reaction mixture suction filtration, with deionized water precipitation is washed after lowering the temperature, vacuum-drying gets product under 30-50 ℃ of condition.
Determine crystal water quantity in the acetylacetone cobalt crystal with the weight loss of fs on thermogravimetric (TG) curve, in conjunction with total carbon content analytical results and X-ray fluorescence spectra measurement result, the chemical formula of determining product is Co (CH
3COCHCOCH
3)
22H
2O.
The present invention finds that the consumption of alkali in the precipitation process and the consumption that changes methyl ethyl diketone in the brilliant process all have a significant effect to reaction yield.
The pH value of hour precipitin reaction mixture is lower when the alkali consumption, and cobaltous hydroxide can not precipitate fully, directly influences the end reaction yield; The pH value of precipitin reaction mixture is higher when the alkali large usage quantity, and cobaltous hydroxide precipitates fully, but excessive alkali is easy and be the reaction of tart methyl ethyl diketone, thus the carrying out that has quickened side reaction.Therefore, the consumption of alkali should be able to make the pH value of precipitin reaction mixture be controlled at 7～10 and be advisable, and best alkali consumption should make the pH value be controlled at 8～9.
The consumption of methyl ethyl diketone is too little, and reaction can not be carried out fully, and on the contrary, the acetylacetone cobalt that generates when its consumption is too big will dissolve wherein, thereby reduce product yield and caused burden to aftertreatment.Be precipitated as benchmark with the cobaltous hydroxide that generates, calculate the consumption of methyl ethyl diketone by stoichiometric ratio and answer excessive 1～5 to be advisable preferably excessive 2～3 times.Press above-mentioned raw materials consumption and reaction conditions, the yield of acetylacetone cobalt can remain on more than 90%.
The present invention has omitted the sedimentary washing of cobaltous hydroxide, drying process, thereby has improved preparation efficiency, and the more important thing is can be by the consumption of alkali in the control precipitation process and the yield of the consumption raising product that changes methyl ethyl diketone in the brilliant process.The preparation technology of acetylacetone cobalt of the present invention is simple, easy to operate, and the yield of products obtained therefrom is greater than 90%.
Embodiment:
Embodiment 1:
Weighing 10kg crystallization cobalt chloride (CoCl
26H
2O) mix with the 50kg deionized water that to be made into concentration be 16.7% crystallization cobalt chloride solution, and join and have in the reactor that stirs with heating unit; 3.5kgNaOH is dissolved in to be made into NaOH content in the 50kg deionized water be 6.5% solution, adds in the reactor to mix with the crystallization cobalt chloride solution and generate cobaltous hydroxide and precipitate, after precipitin reaction was finished, the pH value of reaction mixture was 8; The 25.2kg methyl ethyl diketone is added reactor mix, under 800 rev/mins stirring velocity, be warming up to reflux temperature reaction 3h, generate pinkish acetylacetone cobalt crystal with above-mentioned precipitin reaction mixture.Carry out thorough washing with the reaction mixture suction filtration and to precipitation after the cooling, obtain the 11.7kg product in 40 ℃ of vacuum-dryings at last.After measured, the chemical formula of products therefrom is Co (CH
3COCHCOCH
3)
22H
2O, product yield are 95.2%.
Embodiment 2:
Keep other condition constant in embodiment 1, the consumption of NaOH is reduced to 3.2kg, the pH value that the afterreaction mixture is finished in precipitin reaction is 7.Operate by the preparation method among the embodiment 1, obtain the 11.2kg product.After measured, the chemical formula of products therefrom is Co (CH
3COCHCOCH
3)
22H
2O, yield are 90.8%.
Embodiment 3:
In embodiment 1, keep other condition constant, the consumption of methyl ethyl diketone is increased to 33.6kg, operate, obtain the 11.3kg product by the preparation method among the embodiment 1.After measured, the chemical formula of products therefrom is Co (CH
3COCHCOCH
3)
22H
2O, yield are 91.7%.
Embodiment 4:
In embodiment 1, keep other condition constant, change the crystallization cobalt chloride into crystallization Xiao Suangu (Co (NO
3)
26H
2O), consumption is 12.2kg, operates by the preparation method among the embodiment 1, obtains the 11.6kg product.After measured, the chemical formula of products therefrom is Co (CH
3COCHCOCH
3)
22H
2O, yield are 94.3%.
Claims (2)
1. the preparation method of an acetylacetone cobalt, concrete steps are:
A. in the reactor that has chuck and whipping appts the solubility cobalt salt being dissolved in deionized water preparation cobalt salt concentration is the solution of 10-20wt%, other makes, and NaOH is water-soluble to be made into the alkaline solution that concentration is 5-15wt%, under room temperature and vigorous stirring alkaline solution being joined the pH value that makes reaction mixture in the cobalt salt solution is 7～10, all changes into baby pink cobaltous hydroxide precipitation until cobalt salt;
B. the mol ratio of cobaltous hydroxide/methyl ethyl diketone is 1/2 ratio, the cobaltous hydroxide that generates with steps A is precipitated as benchmark, measuring excessive 1～5 times methyl ethyl diketone adds in the above-mentioned reactor, be warming up to reflux temperature and back flow reaction 2～3h under 600～2500 rev/mins stirring velocity, there is pinkish acetylacetone cobalt crystal to generate in the process
C. with the reaction mixture suction filtration, with deionized water precipitation is washed after lowering the temperature, vacuum-drying under 30-50 ℃ of condition obtains products C o (CH
3COCHCOCH
3)
22H
2O.
2. the preparation method of acetylacetone cobalt according to claim 1 is characterized in that the used solubility cobalt salt of steps A is crystallization cobalt chloride (CoCl
26H
2O) or crystallization Xiao Suangu (Co (NO
3)
26H
2O); The add-on of alkaline solution should make the pH value of reaction mixture be controlled at 8～9;
The amount of methyl ethyl diketone that step B adds is calculated excessive 2～3 times by the cobaltous hydroxide precipitation complete reaction that methyl ethyl diketone and steps A generate.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100707691A CN1313473C (en) | 2005-05-19 | 2005-05-19 | Preparation of acetylacetone cobalt |
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|---|---|---|---|
| CNB2005100707691A CN1313473C (en) | 2005-05-19 | 2005-05-19 | Preparation of acetylacetone cobalt |
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| CN1746180A true CN1746180A (en) | 2006-03-15 |
| CN1313473C CN1313473C (en) | 2007-05-02 |
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ID=36165921
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101565364B (en) * | 2009-06-02 | 2012-10-03 | 安徽佳先功能助剂股份有限公司 | Synthetic method of Beta-diketone metal salt |
| CN105820111A (en) * | 2016-04-21 | 2016-08-03 | 鹤壁市赛科化工有限公司 | Preparation method of catalyst and method for preparing 2,2-dipyridyl through catalysis by virtue of catalyst |
| CN108863754A (en) * | 2018-07-17 | 2018-11-23 | 山东阳谷华泰化工股份有限公司 | A kind of preparation method of acetylacetone cobalt (II) |
| WO2019234356A1 (en) | 2018-06-05 | 2019-12-12 | Compagnie Generale Des Etablissements Michelin | Method for producing acetylacetonate from a hydrated or anhydrous chemical element |
| WO2023134036A1 (en) * | 2022-01-12 | 2023-07-20 | 广东美亨新材料科技有限公司 | Environment-friendly vinyl ester resin |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE4035032C1 (en) * | 1990-11-03 | 1992-04-30 | Degussa Ag, 6000 Frankfurt, De | |
| NZ236906A (en) * | 1991-01-25 | 1995-03-28 | Warner Lambert Co Substituted | Amino complexes of cobalt and pharmaceuticals therefrom having antitumour activity |
| CN1176957C (en) * | 2002-12-12 | 2004-11-24 | 中山大学 | Titanium-cobalt acetylacetonate composite catalyst for preparing branched polyethylene and its preparation method |
| WO2004056737A1 (en) * | 2002-12-23 | 2004-07-08 | Council Of Scientific And Industrial Research | Process for the preparation of metal acetylacetonates |
| CN1197884C (en) * | 2003-06-18 | 2005-04-20 | 中山大学 | Polar monomer homopolymerizatino and copolymerization titanium-cobalt acetylacetonate composite catalyst and its preparing method |
| CN1197883C (en) * | 2003-06-18 | 2005-04-20 | 中山大学 | Polor monomer homopolymerization and copolymerization titanium-substituted beta-dione-cobalt acetylacetonate composite catalyst and its preparing method |
-
2005
- 2005-05-19 CN CNB2005100707691A patent/CN1313473C/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101565364B (en) * | 2009-06-02 | 2012-10-03 | 安徽佳先功能助剂股份有限公司 | Synthetic method of Beta-diketone metal salt |
| CN105820111A (en) * | 2016-04-21 | 2016-08-03 | 鹤壁市赛科化工有限公司 | Preparation method of catalyst and method for preparing 2,2-dipyridyl through catalysis by virtue of catalyst |
| CN105820111B (en) * | 2016-04-21 | 2018-07-24 | 鹤壁市赛科化工有限公司 | The method that a kind of preparation method of catalyst and its catalysis prepare 2,2- bipyridyls |
| WO2019234356A1 (en) | 2018-06-05 | 2019-12-12 | Compagnie Generale Des Etablissements Michelin | Method for producing acetylacetonate from a hydrated or anhydrous chemical element |
| US20210238118A1 (en) * | 2018-06-05 | 2021-08-05 | Compagnie Generale Des Etablissements Michelin | Method for producing acetylacetonate from a hydrated or anhydrous chemical element |
| CN108863754A (en) * | 2018-07-17 | 2018-11-23 | 山东阳谷华泰化工股份有限公司 | A kind of preparation method of acetylacetone cobalt (II) |
| WO2023134036A1 (en) * | 2022-01-12 | 2023-07-20 | 广东美亨新材料科技有限公司 | Environment-friendly vinyl ester resin |
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| Publication number | Publication date |
|---|---|
| CN1313473C (en) | 2007-05-02 |
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