CN106673038B - A kind of preparation method of aluminium-alcohol salt - Google Patents
A kind of preparation method of aluminium-alcohol salt Download PDFInfo
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- CN106673038B CN106673038B CN201510761588.7A CN201510761588A CN106673038B CN 106673038 B CN106673038 B CN 106673038B CN 201510761588 A CN201510761588 A CN 201510761588A CN 106673038 B CN106673038 B CN 106673038B
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Abstract
The invention discloses a kind of preparation method of aluminium-alcohol salt, including alcohol and aluminium to carry out reaction and generate corresponding aluminium-alcohol salt, and wherein alcohol and reactive aluminum is carried out under conditions of externally-applied magnetic field, and applied field strengths are 5~100 kA/m, preferably 10~50 kA/m.Compared with prior art, the present invention is under additional magnetic fields, when alcohol and reactive aluminum, can effectively reduce the content of iron tramp in product aluminium alcoholates, and then can produce high purity aluminium oxide with the aluminium containing certain impurity iron, reduces cost of material, improves product competitiveness.
Description
Technical field
The present invention relates to a kind of preparation method of high purity aluminium oxide, specifically using Organic Alcohol and reactive aluminum, reaction
The method that product hydrolysis prepares high purity aluminium oxide.
Background technology
High purity aluminium oxide has the incomparable light of common alumina powder, electricity, magnetic, heat, machinery and catalytic performance, mainly
Applied to fields such as catalysis, information industries.In catalytic field, SB aluminum oxide is one kind of high purity aluminium oxide, for a variety of catalysis
The carrier of agent, but it is higher to produce more difficulty, cost.
SB aluminum oxide is produced using alkoxide hydrolysis, and main process is produced by the aluminium isopropoxide that fine aluminium is prepared in hydrolysis
Aluminum oxide.According to the similitude of alcohol, isopropanol can be replaced to prepare n-hexyl alcohol aluminium with n-hexyl alcohol and hydrolyze generation aluminum oxide again.It is but pure
Aluminium cost is higher, and the impurity in aluminium can enter in alumina product, influence the performance of product.For example, the impurity iron meeting of aluminium
Into 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 one kind is to use high-purity raw material
Aluminium, another kind of is that the alkoxide of aluminium carries out de- impurity treatment.Research in document to latter class discloses 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, which has simultaneously participated in reaction and formed, contains Fe organic compound.Mainly it have studied reaction
The influence of thing ratio, environment, catalyst, alcohol species to iron tramp content in aluminium alcoholates.Experiment proves：Reactant ratio, urge
Agent does not have too much influence to the iron tramp content in the aluminium alcoholates of synthesis；Environment be influence iron tramp generation it is important because
Element, oxygen can suppress the generation of Fe organic compound.This rule is suitable for various aluminium-alcohol salt building-up processes to iron tramp content
Research.
Have much for the edulcoration purification process of alkoxide, such as：Distillation under vacuum, crystallisation, extraction etc..Decompression is steamed
The characteristics of method of evaporating make use of metal alkoxide boiling point in a heated condition and be easy to decompose, so as to realize purifying alkoxide, because
Its is simple to operate, takes less, quick, so being widely used in the industrial production.The process of crystallisation is by alcohol
Salt is dissolved in certain organic solvent, then the different solubility according to alkoxide in the organic solvent under condition of different temperatures,
Metal alkoxide is crystallized out finally by cooling.This method has that energy consumption is low, and equipment volume is small for vacuum distillation,
The advantages of cost is not high, but due to very time-consuming, so it is difficult to promoting in the industrial production.The cardinal principle of extraction be by
Metal alkoxide dissolves in organic solvent so that insoluble substance is deposited to reactor bottom and then obtains purer material
So as to come realize alkoxide and impurity separation, this method, which can mainly make up the alkoxide such as isooctanol aluminium, can not be depressurized distillation
Feature, because this method is equally time-consuming thus can not produce in batches in the industrial production.
The content of the invention
In view of the shortcomings of the prior art, the invention provides a kind of preparation method of aluminium-alcohol salt, purity can be used relatively low
Raw material aluminium, using simple technique, the relatively low aluminium-alcohol salt of impurity content can be obtained, can be used for urging after the alfol salt hydrolysis
Agent carrier.
The inventive method includes alcohol and aluminium carries out reaction and generates corresponding aluminium-alcohol salt, it is characterised in that：Alcohol and reactive aluminum are outside
Add and carry out under conditions of magnetic field, 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 magnetostatic field or rotation
The dynamic magnetic fields such as magnetic 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 use this area
Prior art, it is specially：Reaction temperature is 140~170 DEG C, using aluminium chloride or aluminium isopropoxide as initiator, after reaction triggers, is led to
Add the speed control reaction speed of alcohol.Trimethylbenzene can be added in reactant system, to improve the rate of filtration of reaction product.
Trimethylbenzene dosage 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.N-hexyl alcohol
Water content 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%（Matter
Amount）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.Aluminium it is pure
Spend for 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 any not material with reaction mass reaction, such as glass, stainless steel, ceramics, lucite
Deng.
The present invention is had found by studying, and under additional magnetic fields, when alcohol and reactive aluminum, can effectively reduce product aluminium alcoholates
The content of middle iron tramp, and then high purity aluminium oxide can be produced with the aluminium containing certain impurity iron, cost of material is reduced, is improved
Product competitiveness.
Embodiment
The inventive method is described in detail with reference to specific embodiment.The purity of raw material has bright to product purity
Aobvious influence, the water content in n-hexyl alcohol can not be too high, typically requires below 600 μ g/g, the iron content in aluminium typically requires
0.2%（Quality）Below.
Feedstock property used in 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, is heated to
150 DEG C, after reaction triggers, flow back 15 minutes, alcohol 590g was instilled in 3 hours, after completion of dropwise addition, keeping temperature continues reaction 2
Hour, react and terminate when no hydrogen is released.When being cooled to 90 DEG C, filtered with the ceramic filter that aperture is 1 μm, filtering production
Thing 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 electricity
Magnetic field caused by magnetic induction, applied field strengths are the magnetic field intensity at reaction vessel outer wall.Examples 1 and 2 are magnetostatic field, real
Apply the rotation dynamic magnetic field that the rotating speed of example 3 is 30 revs/min.Specific embodiment and comparative example reaction condition and it the results are shown in Table 1.
The embodiment of table 1 and comparative example reaction condition and result.
Claims (15)
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 aluminium
Reaction is carried out under conditions of externally-applied magnetic field, and applied field strengths are 5~100 kA/m.
2. in accordance with the method for claim 1, it is characterised in that：The applied field strengths are 10~50 kA/m.
3. in accordance with the method for claim 1, it is characterised in that：Externally-applied magnetic field is produced by electromagnetic induction device, or by permanent magnetism
Body produces magnetic field.
4. seek any described methods of 1-3 according to right, it is characterised in that：Externally-applied magnetic field is magnetostatic field, or dynamic magnetic field.
5. in accordance with the method for claim 1, it is characterised in that：Alcohol is isopropanol or n-hexyl alcohol.
6. according to the method described in claim 1 or 5, it is characterised in that：The condition of reaction is：Reaction temperature is 140~170
DEG C, using aluminium chloride or aluminium isopropoxide as initiator, after reaction triggers, by the speed control reaction speed for adding alcohol.
7. in accordance with the method for claim 5, it is characterised in that：Trimethylbenzene is added in reactant system, to improve reaction production
The rate of filtration of thing, trimethylbenzene dosage are the 20%~60% of alcohol quality.
8. in accordance with the method for claim 5, it is characterised in that：The purity of n-hexyl alcohol is more than 98 mass %.
9. in accordance with the method for claim 8, it is characterised in that：The purity of n-hexyl alcohol is more than 99 mass %.
10. in accordance with the method for claim 5, it is characterised in that：The water content of n-hexyl alcohol is less than 1000 μ g/g.
11. in accordance with the method for claim 10, it is characterised in that：The water content of n-hexyl alcohol is less than 500 μ g/g.
12. in accordance with the method for claim 1, it is characterised in that：The purity of aluminium is more than 98 mass %.
13. in accordance with the method for claim 12, it is characterised in that：The purity of aluminium is more than 99 mass %.
14. in accordance with the method for claim 1, it is characterised in that：The impurity iron content of aluminium is below 2 mass %.
15. in accordance with the method for claim 14, it is characterised in that：The impurity iron content of aluminium is below 1 mass %.
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