CN106673038A - Aluminum alkoxide preparation method - Google Patents
Aluminum alkoxide preparation method Download PDFInfo
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Abstract
The present invention discloses an aluminum alkoxide preparation method, which comprises that an alcohol and aluminum are subjected to a reaction under an external magnetic field to produce a corresponding aluminum alkoxide, wherein the intensity of the external magnetic field is 5-100 kA/m, preferably 10-50 kA/m. Compared to the preparation method in the prior art, the preparation method of the present invention has the following characteristics that the alcohol and the aluminum are subjected to the reaction under the action of the external magnetic field, such that the iron impurity content in the product aluminum alkoxide can be effectively reduced so as to produce the high-purity alumina by using the aluminum containing a certain impurity iron, such that the raw material cost is reduced, and the product competitiveness is increased.
Description
Technical field
The present invention relates to a kind of preparation method of high purity aluminium oxide, the method for specifically preparing high purity aluminium oxide using Organic Alcohol and reactive aluminum, product hydrolysis.
Background technology
High purity aluminium oxide has common alumina powder jointed incomparable light, electricity, magnetic, heat, machinery and catalytic performance, is mainly used in the fields such as catalysis, information industry.In catalytic field, SB aluminum oxide is one kind of high purity aluminium oxide, for the carrier of multiple catalysts, but produces more difficult, relatively costly.
SB aluminum oxide is produced using alkoxide hydrolysis, and main process produces aluminum oxide by the aluminium isopropoxide that fine aluminium is prepared in hydrolysis.According to the similitude of alcohol, isopropanol can be replaced with n-hexyl alcohol to prepare n-hexyl alcohol aluminium and to hydrolyze generation aluminum oxide again.But fine aluminium is relatively costly, the impurity in aluminium can enter the performance that product is affected in alumina product.For example, the impurity iron of aluminium can be entered in aluminum oxide.Therefore the impurity of aluminum oxide how is controlled, is this area important research direction.
In general, controlling the method for impurity content in alumina mainly includes two classes, and a class is to use high-purity raw material aluminium, and another kind of is that the alkoxide of aluminium carries out de- impurity treatment.The research of latter class disclosed in document more.Such as《Inorganic chemicals industry》" Study on influencing factors of iron tramp content in aluminium-alcohol salt synthesis " of the introductions such as 06 phase Chu's big waves in 2013, is disclosed directly below content：In aluminium-alcohol salt building-up process, the iron tramp in aluminium skimmings has simultaneously participated in reaction and has been formed containing Fe organic compound.Mainly have studied the impact of reactant ratio, environment, catalyst, alcohol species to iron tramp content in aluminium alcoholates.Experiment is proved：Reactant ratio, catalyst do not have too much influence to the iron tramp content in the aluminium alcoholates of synthesis；Environment is the key factor for affecting iron tramp to generate, and oxygen can suppress the generation of Fe organic compound.This rule contains quantifier elimination suitable for various aluminium-alcohol salt building-up processes to iron tramp.
For the edulcoration purification process of alkoxide has a lot, for example：Distillation under vacuum, crystallisation, extraction etc..Distillation under vacuum make use of metal alkoxide boiling point in a heated condition and be easy to the characteristics of decomposing, so as to realizing purifying alkoxide, because its is simple to operate, take few, instant effect, so being widely used in the industrial production.The process of crystallisation is that alkoxide is dissolved in certain organic solvent, and then the different solubility according to alkoxide in the organic solvent under condition of different temperatures, finally by cooling metal alkoxide is crystallized out.This method has that energy consumption is low for vacuum distillation, and equipment volume is little, the not high advantage of cost, but due to taking very much, so it is difficult to promoting in the industrial production.The cardinal principle of extraction is to dissolve metal alkoxide in organic solvent, so that insoluble substance is deposited to reactor bottom and then obtains the pure material of comparison so as to detached to realize alkoxide and impurity, the characteristics of this method mainly can make up the alkoxide such as isooctanol aluminium and can not be depressurized distillation, because the method equally takes thus can not produce in batches in the industrial production.
The content of the invention
For the deficiencies in the prior art, the invention provides a kind of preparation method of aluminium-alcohol salt, can adopt the relatively low raw material aluminium of purity, using simple technique, it is possible to obtain the relatively low aluminium-alcohol salt of impurity content, after the alfol salt hydrolysis catalyst carrier is can be used for.
The inventive method includes that alcohol and aluminium carry out reaction and generates corresponding aluminium-alcohol salt, it is characterised in that：Alcohol and reactive aluminum are carried out under conditions of externally-applied magnetic field, and applied field strengths are 5～100 kA/m, preferably 10～50 kA/m.
In the inventive method, externally-applied magnetic field can be produced by electromagnetic induction device, can be the dynamic magnetic fields such as magnetostatic field, or rotating excitation field.Magnetic field can certainly be produced by permanent magnet.
In the inventive method, alcohol is isopropanol or n-hexyl alcohol, preferably n-hexyl alcohol.Alcohol and reactive aluminum can adopt state of the art, specially：Reaction temperature is 140～170 DEG C, with aluminium chloride or aluminium isopropoxide as initiator, after reaction causes, leads to the speeds control reaction speed for adding alcohol.Trimethylbenzene can be added in reactant system, to improve the rate of filtration of product.Trimethylbenzene consumption is the 20%～60% of alcohol（Quality）.
In the inventive method, the purity of n-hexyl alcohol is 98%（Quality）More than, preferably 99%（Quality）More than.The water content of n-hexyl alcohol is less than 1000 μ g/g, preferably shorter than 500 μ g/g.The purity of isopropanol is 98%（Quality）More than, preferably 99%（Quality）More than.The water content of isopropanol is less than 100 μ g/g, preferably shorter than 10 μ g/g.Other alcohol can certainly be used.The purity of aluminium is 98%（Quality）More than, preferably 99%（Quality）More than.The impurity iron content of aluminium is 2%（Quality）Hereinafter, preferably 1%（Quality）Below.
Reaction vessel can be the material arbitrarily do not reacted with reaction mass, such as glass, stainless steel, ceramics, lucite.
The present invention is had found by studying, and under additional magnetic fields, when alcohol and reactive aluminum, can effectively reduce the content of iron tramp in product aluminium alcoholates, and then high purity aluminium oxide can be produced with the aluminium containing certain impurity iron, reduces cost of material, improves product competitiveness.
Specific embodiment
The inventive method is described in detail with reference to specific embodiment.The purity of raw material has significantly impact on product purity, and the water content in n-hexyl alcohol can not be too high, typically requires that the iron content in aluminium typically requires 0.2% below 600 μ g/g（Quality）Below.
Feedstock property used by embodiment is as follows：
N-hexyl alcohol：Purity 99%（Quality）, the μ g/g of water content 500.Isopropanol：Purity 99%（Quality）, the μ g/g of water content 3.Aluminium powder 1：Powder degree is less than 0.5 μm, purity 99%（Quality）, iron content 0.15%（Quality）.Aluminium powder 2：Powder degree is less than 0.5 μm, purity 99%（Quality）, iron content 0.09%（Quality）.
Embodiment process is as follows：
Aluminium powder 36g, anhydrous Aluminum chloride 0.5g are added in reaction vessel, 10g alcohol and trimethylbenzene 200g is added, 150 DEG C are heated to, after reaction causes, flow back 15 minutes, alcohol 590g was instilled in 3 hours, after completion of dropwise addition, keeping temperature continues to react 2 hours, and reaction when no hydrogen is released terminates.When being cooled to 90 DEG C, filtered with the ceramic filter that aperture is 1 μm, filtration product carries out iron tramp content analysis（It is scaled iron content in alcohol aluminium salt）.Other conditions and result see the table below.Externally-applied magnetic field is the magnetic field that electromagnetic induction is produced, and applied field strengths are the magnetic field intensity at reaction vessel outer wall.Embodiment 1 and 2 is magnetostatic field, and the rotating speed of embodiment 3 is 30 revs/min of rotation dynamic magnetic field.Specific embodiment and comparative example reaction condition and the results are shown in Table 1.
The embodiment of table 1 and comparative example reaction condition and result.
Claims (10)
1. a kind of preparation method of aluminium-alcohol salt, including alcohol and aluminium carry out reaction and generate corresponding aluminium-alcohol salt, it is characterised in that：Alcohol and reactive aluminum are carried out under conditions of externally-applied magnetic field, and applied field strengths are 5～100 kA/m, preferably 10～50 kA/m.
2. in accordance with the method for claim 1, it is characterised in that：Externally-applied magnetic field is produced by electromagnetic induction device, or produces magnetic field by permanent magnet.
3. the method described in 1 or 2 is sought according to right, it is characterised in that：Externally-applied magnetic field is magnetostatic field, or dynamic magnetic field.
4. in accordance with the method for claim 1, it is characterised in that：Alcohol is isopropanol or n-hexyl alcohol.
5. according to the method described in claim 1 or 4, it is characterised in that：The condition of reaction is：Reaction temperature is 140～170 DEG C, with aluminium chloride or aluminium isopropoxide as initiator, after reaction causes, leads to the speeds control reaction speed for adding alcohol.
6. in accordance with the method for claim 4, it is characterised in that：Trimethylbenzene is added in reactant system, to improve the rate of filtration of product, trimethylbenzene consumption is the 20%～60% of alcohol quality.
7. in accordance with the method for claim 4, it is characterised in that：The purity of n-hexyl alcohol is more than 98 mass %, more than preferably 99 mass %.
8. in accordance with the method for claim 4, it is characterised in that：The water content of n-hexyl alcohol is less than 1000 μ g/g, preferably shorter than 500 μ g/g.
9. in accordance with the method for claim 1, it is characterised in that：The purity of aluminium is more than 98 mass %, more than preferably 99 mass %.
10. in accordance with the method for claim 1, it is characterised in that：The impurity iron content of aluminium is below 2 mass %, below preferably 1 mass %.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111187147A (en) * | 2020-01-13 | 2020-05-22 | 大连理工大学 | Process for continuously synthesizing aluminum alkoxide |
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| CN111187147A (en) * | 2020-01-13 | 2020-05-22 | 大连理工大学 | Process for continuously synthesizing aluminum alkoxide |
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