JPH032187A - Production of aluminoxane - Google Patents

Abstract

PURPOSE:To readily obtain the highly active and highly pure subject compound useful as a catalyst for producing olefin-based polymers, etc., by reacting an organoaluminum compound with water in a specific solvent and concentrating the resultant solution under a normal pressure or reduced pressure. CONSTITUTION:For example, an organoaluminum compound (preferably trimethylaluminum) is reacted with water (example, usual water or water saturated with a solvent) in a solvent (example; benzene) containing a solvent having a higher boiling point than that of the organoaluminum compound [xylene, etc., in an amount of preferably 30-100% (wt.) based on the total amount of solvent is contained] and the resultant solution, at it is or after filtration of a solid residue, is concentrated under a normal pressure or reduced pressure (760-0.01mmHg) at -30 to 200 deg.C to afford the objective compound. The aminoxane concentration of the aminoxane-containing solution is preferably 5-50%.

Description

[Detailed Description of the Invention] [Industrial Application Field] The present invention relates to a method for producing aluminoxane, and more specifically, it is a highly pure and highly active aluminoxane that can be suitably used as a catalyst component for producing olefin polymers, styrene polymers, etc. The present invention relates to a method for easily producing aluminoxane.

(Prior Art and Problems to be Solved by the Invention) Conventionally, when producing an olefin polymer or styrenic polymer by polymerizing olefin or styrene in the presence of a catalyst, (A) a transition metal compound has been used as a catalyst. and (B)
A method using aluminoxane is widely known (JP-A-62-36390, JP-A-599).
5292, etc.).

However, in the method disclosed in JP-A-62-36390, the filtrate obtained by filtering solid matter from the condensation reaction mixture of organoaluminum and water is left as is when preparing the above-mentioned aluminoxane. Further, in the method disclosed in JP-A-59-95292, a solvent (for example, toluene or heptane) having a boiling point lower than that of the raw organic aluminum is simply distilled off at room temperature.

By the way, the above reaction mixture contains unreacted organoaluminum compounds that are not effective as catalyst components, as well as chain and cyclic aluminoxanes, but when aluminoxane is prepared in a low boiling point solvent as described above, the solvent Even after removing the organic aluminum, unreacted organoaluminum cannot be distilled out, resulting in a drawback that highly pure aluminoxane cannot be obtained.

On the other hand, the present inventors have already developed a method for obtaining pure aluminoxane by removing unreacted organoaluminum by concentrating the filtrate after the reaction between organoaluminum and water and then heat-treating it under normal pressure or reduced pressure. (Japanese Unexamined Patent Publication No. 1-240504).

However, in this method, aluminoxane is obtained as a viscous liquid or a glass-like heterogeneous solid during the reduced pressure heat treatment, so it is difficult to perform uniform heat treatment on an industrial scale, and unreacted organic aluminum The problem is that it cannot be completely removed.

Furthermore, in order to utilize the aluminoxane obtained by this method as a catalyst, there are practical disadvantages such as the necessity of dissolving it in an appropriate hydrocarbon solvent or making it into a slurry.

As mentioned above, although aluminoxane is expensive as a catalyst component, it has not been known to be of high purity. In the case where the catalyst was used, there was a drawback that the catalytic activity was not sufficient.

The second object of the present invention is to solve the above-mentioned conventional drawbacks and to easily produce a highly pure and highly active aluminoxane that can be suitably used as a catalyst component for producing olefin polymers and styrene polymers. be.

[Means for solving the problem] That is, the present invention provides an organic aluminum compound and water,
A method for producing aluminoxane (hereinafter referred to as production method I), which comprises concentrating a solution obtained by reacting in a solvent containing a solvent having a boiling point higher than that of the organoaluminum compound under normal pressure or reduced pressure. The method is characterized in that a solution obtained by reacting an organoaluminum compound and water with a solvent containing a solvent having a boiling point higher than that of the organoaluminum compound is concentrated under normal pressure or reduced pressure. The present invention provides a method for producing aluminoxane (hereinafter referred to as production method ①).

In production method I, an organoaluminum compound and water are used as raw materials.

Here, the organoaluminum compound is usually a trialkylaluminum compound represented by the general formula A IlR' (wherein R+ represents an alkyl group having 1 to 8 carbon atoms), specifically trimethylaluminum, triethylaluminum , triisobutylaluminum, etc., and trimethylaluminum is particularly preferred.

On the other hand, the water to be reacted with the above-mentioned organoaluminum compound may include, in addition to ordinary water, various hydrous compounds, solvent-saturated water, water adsorbed by inorganic substances or organic substances, and copper sulfate natural water salt (C
It contains crystal water containing metal salts such as uSOs・5H,O). In addition, water in item F contains amines such as ammonia and ethylamine.

Sulfur compounds such as hydrogen sulfide, phosphorus compounds such as phosphorous esters, etc. may be contained up to about 20%.

In production method I, the above-mentioned organoaluminum compound and water are first reacted in a solvent containing a solvent having a boiling point higher than that of the 31W aluminum compound.

Here, as the solvent having a boiling point higher than that of the organoaluminum compound, various solvents can be used as long as they have a boiling point higher at atmospheric pressure than the above-mentioned organoaluminum compound.

Specifically, there are aromatic hydrocarbons such as xylene, ethylbenzene, propylbenzene, and cumene, and aliphatic hydrocarbons such as octane, nonane, and decane. Preferably, aromatic hydrocarbons have a higher content than the above-mentioned organoaluminum compounds. Examples include those that have a boiling point.

The solvent used in the production method (1) of the present invention contains a solvent having a boiling point higher than that of the above-mentioned organoaluminum compound. The content of (sometimes referred to as "solvent") is 10 to 100% by weight, preferably 30 to 100% by weight, based on the total amount of the solvent. If the content of this high-boiling point solvent is less than 10% by weight, that is, if a solvent containing a solvent with a boiling point lower than that of the organoaluminum compound (hereinafter sometimes referred to as a low-boiling point solvent) is used in a proportion exceeding 90% by weight, High purity aluminoxane cannot be obtained by concentration in the next step.

Note that low-boiling point solvents that can be used together with high-boiling point solvents include aromatic hydrocarbons such as benzene and toluene;
Alternatively, aliphatic hydrocarbons such as hexane and heptane can be used. Further, the amount of the solvent used, including a solvent having a boiling point higher than that of the organoaluminum compound, is not limited, but is preferably 0.1 to 102% per mole of the organoaluminum compound.

Regarding the high boiling point solvent used in the above manufacturing method (1), specifically, when trimethylaluminum is used as an organoaluminum compound, ethylbenzene, p-xylene, m-xylene, 0-xylene,
A mixture of the above xylenes, propylbenzene, cumene, etc. may be used.

The reaction in the above production method I is not particularly limited, and may be carried out according to a known method. For example, ■ A method in which an organoaluminum compound is dissolved in a solvent and brought into contact with water; ■ Crystal water contained in metal salts, etc., or water adsorbed on inorganic or organic substances is reacted with an organoaluminum compound in a solvent. There are ways to do this.

Further, the reaction conditions are not particularly limited, and may be the conditions used in ordinary aluminoxane production methods.

In production method I, the solution obtained by such a reaction is concentrated under normal pressure or reduced pressure, but if a hydrous compound is used, the solid residue may be filtered out in advance if necessary. good.

In this way, in production method I, the solution obtained by the reaction (
The reaction mixture) as it is, or the solution from which the solid residue has been filtered off in advance as described above, is heated under normal pressure or reduced pressure until the weight of the solution is 1/1.5 to 1/100, preferably 1/2 of the original weight.
Concentrate until the volume is about 1/10. The processing temperature and pressure at this time depend on the type of organoaluminum compound and solvent, but the temperature is in the range of -30 to 200°C, and the pressure is in the range of 760 to 0.01 nn11g. preferable.

Please note that this process is only a concentration process,
If the solvent is completely distilled off to dryness, it will be necessary to crush and dissolve it before use, making the process complicated and undesirable. The aluminoxane concentration of the resulting aluminoxane-containing solution is not particularly limited, but is preferably 5 to 50% by weight.

Through this concentration step, the unreacted organoaluminum compound, which is not effective as a catalyst component, has a lower boiling point than the high-boiling point solvent, so it is distilled off at the beginning of the concentration step. Therefore, as a result of concentration, a highly pure aluminoxane solution is obtained.

Next, in production method H, a solution obtained by reacting an organoaluminum compound and water is used as a raw material solution.

This raw material solution may be prepared by any method using the same organic aluminum compound and water as described above,
Usually, it is a mixed solution of aluminoxane and an unreacted organoaluminum compound. The reaction between the organoaluminum compound and water can be carried out in a solvent, but the solvent used in this reaction is not particularly limited and may be any solvent commonly used in the production of aluminoxane.

In production method (2), a solvent containing the above-mentioned high boiling point solvent is added to the mixed solution of the aluminoxane thus obtained and the unreacted organoaluminum compound.

Such a solvent (hereinafter sometimes referred to as an additional solvent).

) is the same as that described in the above-mentioned production method I, that is, the above-mentioned high boiling point solvent is used at 10 to 100%
Examples include solvents containing % by weight, preferably 30 to 100% by weight. Further, the amount of this high boiling point solvent to be used is not particularly limited as in Production Method I, but is 0.1 to 10 I per mole of organoaluminum compound! , is preferable.

In production method H, a solution to which the above-mentioned solvent is added is concentrated under normal pressure or reduced pressure.

? The degree of shrinkage is the same as described in the production method ① above, and the weight of the solution is 1/1 of the original weight under normal pressure or reduced pressure.
．． 5-1/100. Preferably, it is concentrated to about 1/2 to 1/1O. The processing temperature and pressure at this time are as follows:
Depending on the type of organoaluminum compound and solvent, the temperature ranges from -30 to 200°C and the pressure is 76°C.
A range of 0 to 0.01 myaHg is preferred.

In addition, in manufacturing method I! As mentioned in the case of the line treatment, if the solvent is completely distilled off to dryness, the process will become complicated because it will have to be crushed and dissolved before use. In addition, since unreacted organoaluminum compounds that are not effective as catalyst components are distilled out at the beginning of the concentration process, the degree of concentration is determined by the type of solvent of the raw material solution and additional solvent, as described above.
All you have to do is take the amount into consideration and do it to the extent that it does not completely dry out. The aluminoxane concentration of the resulting aluminoxane-containing solution is not particularly limited, but is between 5 and 5.
50% by weight is preferred.

This concentration process yields a highly pure aluminoxane solution.

The aluminoxane obtained as described above is combined with a transition metal compound such as titanium or zirconium to form an olefin polymer such as polyethylene, acid polypropylene, isotactic polypropylene, polybutene-1, poly-4-methyl. Pentene-1 etc. and ethylene-
Propylene copolymers etc. or styrene polymers, specifically styrene polymers having a syndiotactic structure,
Furthermore, it can be used as it is in the form of a solution as a catalyst component for low polymerization of propylene. Note that the transition metal compound may be selected from transition metals in group 1 VB of the periodic table according to the type of the desired polymer.

[Examples] Next, the present invention will be explained in more detail with reference to Examples and Comparative Examples.

Example 1 (1) 8-circle aluminoxane vent line equipped with a wet flow meter, internal capacity 1000F
Copper sulfate pentahydrate (
Add 47.4-g (190 mmol) of CuSO4.5HzO) and 300 ml of ethylbenzene (boiling point 136"C), cool to 0°C, and add trimethylaluminum (boiling point 1
A solution of 48d (0.50 mol) dissolved in 52d of ethylbenzene was added dropwise over 10 minutes. Next, the temperature was raised to 40°C over 20 minutes, and the methane gas was
6.811.10 moles.

The reaction was allowed to occur until the reaction occurred (24°C). Total reaction time was 8 hours and 33 minutes.

After the reaction was completed, the solid residue was filtered off, and 310 g of the obtained filtrate
The mixture was placed in a 500 d glass container capable of being depressurized, and concentrated to 100 g under a reduced pressure of 4 torr while stirring. At this time, elemental analysis and proton nuclear magnetic resonance ('H-N
Confirmed with MR). Furthermore, the concentration of methylaluminoxane contained in the concentrated liquid was 1.6 g atoms/l in terms of aluminum concentration.

This was directly used as a catalyst solution in the following polymerization reaction.

(2) Content volume l of ethylene replaced with polymerized nitrogen! 400 d of toluene, 1 mmol of the methylaluminoxane obtained in (1) above as an aluminum atom, and 5 micromol of biscyclopentagenylzirconium dichloride were sequentially added to the autoclave, and the temperature was raised to 80°C. Next, ethylene was continuously introduced into the autoclave at a rate of 8 kg/cIl.
The polymerization reaction was carried out at 1G for 1 hour. After the reaction was completed, methanol was added to decompose the catalyst, followed by drying to obtain 121 g of polyethylene. Polymerization activity is 265kg/g-Zr
Met.

(3) Polymerization of styrene In a nitrogen-substituted autoclave with contents 11f, 400 ml of styrene, 4 mmol of triisobutylaluminum 11, 4 mmol of the methylaluminoxane obtained in (1) above as an aluminum atom, and pentamethylcyclopentadienyl titanium. 20 micromoles of trimethoxide was added, and a polymerization reaction was carried out at 70°C for 1 hour.

After the reaction was completed, the product was washed with a hydrochloric acid/methanol mixture to separate and remove the catalyst component, and dried to obtain 90.9 g of a polymer. The polymerization activity was 94.9 kg/g-Ti. The syndiotacticity of the racemic pentads of this polymer was determined by nuclear magnetic resonance (13C-NMR) using carbon isotopes.
It was 97% from the measurement. The results are shown in Table 1.

Example 2 (1) Preparation of aluminoxane Aluminoxane (methylaluminoxane ) was prepared.

(2) Polymerization of ethylene In Example 1 (2), the above (
Ethylene polymerization was carried out in the same manner as in Example 1(2) except that the methylaluminoxane obtained in 1) was used. As a result, 129 g of polyethylene was obtained. The polymerization activity was 283 kg/g-Zr.

(3) Polymerization of styrene In Example 1 (3), the above (
Polymerization of styrene was carried out in the same manner as in Example 1 (3) except that the methylaluminoxane obtained in 1) was used. As a result, 93.1 g of polymer was obtained. The polymerization activity was 97.2 kg/g-Ti. The racemic pentad syndiotacticity of this polymer is 13C-
It was 98% according to NMR measurement.

The results are shown in Table 1.

Example 3 (1) Preparation of aluminoxane Aluminoxane (methyl Aluminoxane) was prepared.

(2) Polymerization of ethylene In Example 1 (2), the above (
Ethylene polymerization was carried out in the same manner as in Example 1(2) except that the methylaluminoxane obtained in 1) was used. As a result, 130 g of polyethylene was obtained. The polymerization activity was 2.85 kg/g-Zr.

(3) Polymerization of styrene In Example 1 (3), the above (
Styrene polymerization was carried out in the same manner as in Example 1 (3) except that the methylaminoxane obtained in 1) was used. As a result, 92.6 g of polymer was obtained.

The polymerization activity was 96.7 kg/g-Ti. The racemic pentad syndiotacticity of this polymer was 98% as determined by 13C-NMR measurement. The results are shown in Table 1.

Example 4 (1) Preparation of aluminoxane Aluminoxane (methylaluminoxane (2) Polymerization of ethylene In Example 1 (2), the above (
Ethylene polymerization was carried out in the same manner as in Example 1(2) except that the methylaluminoxane obtained in 1) was used. As a result, 138 g of polyethylene was obtained. Polymerization activity was 303 kg/g-Zr.

(3) Polymerization of styrene In Example 1 (3), the above (
Styrene polymerization was carried out in the same manner as in Example 1 (3) except that the methylaminoxane obtained in 1) was used. As a result, 93.5 g of polymer was obtained.

Polymerization activity is 97. It was 6 kg/g-Ti. The racemic pentad syndiotacticity of this polymer was 98% as determined by l''c-NMR measurement.

The results are shown in Table 1.

Example 5 (1) Preparation of aluminoxane Aluminoxane (
methylaluminoxane) was prepared.

(2) Polymerization of ethylene In Example 1 (2), the above (
Ethylene polymerization was carried out in the same manner as in Example 1 (2) except that the methylaluminoxane obtained in 1) was used. As a result, 132 g of polyethylene was obtained. Polymerization activity was 289 kg/g-Zr.

(3) Polymerization of styrene In Example 1 (3), the above (
Styrene polymerization was carried out in the same manner as in Example 1 (3) except that the methylaminoxane obtained in 1) was used. As a result, 91.4 g of polymer was obtained.

The polymerization activity was 95.4) cg/g-Tt. Syndiotacticity of this polymer in racemic pentads
was 98% according to C-NMR measurement. The results are shown in Table 1.

Comparative Example 1 (1) 8-cycle production of aluminoxane Aluminoxane (methyl Aluminoxane) was prepared.

(2) Polymerization of ethylene In Example 1 (2), the above (
Ethylene polymerization was carried out in the same manner as in Example 1(2) except that the methylaluminoxane obtained in 1) was used. As a result, 90 g of polyethylene was obtained and the zero polymerization activity was 197 kg/g-Zr.

(3) Polymerization of styrene In Example 1 (3), the above (
Styrene polymerization was carried out in the same manner as in Example 1 (3) except that the methylaminoxane obtained in 1) was used. As a result, 17.9 g of polymer was obtained.

The polymerization activity was 18.7 kg/g-Ti. The racemic pentad syndiotacticity of this polymer was 96% as determined by 13C-NMR measurement. The results are shown in Table 1.

Example 6 (1) Preparation of aluminoxane In an autoclave with an internal capacity of 1000 d equipped with a wet flow meter in the vent line, copper sulfate (Cu) was added under a nitrogen atmosphere.
Add 47.4 g (190 mmol) of SO4.5HzO) and 300 d of toluene, cool to 0°C, and add 48 ml (0,50 mmol) of trimethylaluminum (boiling point 126°C).
A solution prepared by dissolving mol) in 52 ml of toluene was added dropwise over 10 minutes. Then, the temperature was raised to 40 °C over 20 minutes, and 26.811.10 mol of methane gas was added at 24 °C)
The reaction was allowed to occur until it occurred.

After the reaction was completed, the solid residue was filtered off, and the resulting filtrate 340
ml and ethylbenzene as additional solvent (boiling point 136°C
)1020mj! The mixture was placed in a 21 glass container capable of being depressurized and concentrated to 170 d under a reduced pressure of 4 torr while stirring. At this time, it was confirmed by elemental analysis and 'H-NMR that 3.86 g (54 mmol) of trimethylaluminum was dissolved in the distillate.

Also, the concentration of methylaluminoxane contained in the concentrate is 1.2 g atoms/! as aluminum concentration! Met. This was directly used as a catalyst solution in the following polymerization reaction.

(2) Polymerization of ethylene In Example 1 (2), the above (
Ethylene polymerization was carried out in the same manner as in Example 1(2) except that the methylaluminoxane obtained in 1) was used. As a result, 109 g of polyethylene was obtained. The polymerization activity was 239 kg/g-Zr.

(3) Polymerization of styrene In Example 1 (3), the above (
Styrene polymerization was carried out in the same manner as in Example 1 (3) except that the methylaminoxane obtained in 1) was used. As a result, 86.7 g of polymer was obtained.

The polymerization activity was 90.5 kg/g''ri. The racemic pentad syndiotacticity of this polymer was 97% as determined by 13C-NMR measurement. The results are shown in Table 2.

Example 7 (1) Preparation of aluminoxane Aluminoxane was prepared in the same manner as in Example 6(1), except that paraxylene (boiling point 138°C) was used as an additional solvent in place of ethylbenzene. (Methylaluminoxane) was prepared.

(2) Polymerization of ethylene In Example 1 (2), the above (
Ethylene polymerization was carried out in the same manner as in Example 1(2) except that the methylaluminoxane obtained in 1) was used. As a result, 102 g of polyethylene was obtained. The polymerization activity was 224 kg/g-Zr.

(3) Polymerization of styrene In Example 1 (3), the above (
Styrene polymerization was carried out in the same manner as in Example 1 (3) except that the methylaminoxane obtained in 1) was used. As a result, 88.1 g of polymer was obtained.

The polymerization activity was 92.0 kg/g・Ti. The syndiotacticity of this polymer in racemic pentads was 97% according to C-NMR measurement.
Shown in the table.

Example 8 Aluminoxane (methylaluminoxane) was prepared in the same manner as in Example 6(1), except that xylene (boiling point 137-144'c>) was used instead of ethylbenzene as the additional solvent. Prepared.

(2) Polymerization of ethylene In Example 1 (2), ethylene was polymerized in the same manner as in Example 1 (2) except that the methylaluminoxane obtained in (1) was used as aluminoxane. Ta. As a result, 115 g of polyethylene was obtained. Polymerization activity was 252 kg/g-Zr.

(3) Polymerization of styrene In Example 1 (3), the above (
Styrene polymerization was carried out in the same manner as in Example 1 (3) except that the methylaminoxane obtained in 1) was used. As a result, 89.4 g of polymer was obtained.

The polymerization activity was 93.4 kg/g·Ti. The racemic pentad syndiotacticity of this polymer was 98% as determined by C-NMR measurement. The results are shown in Table 2.

Example 9 (1) 8 rounds of aluminoxane Production was carried out in the same manner as in Example 6 (1), except that isopropylbenzene (boiling point 152°C) was used as an additional solvent instead of ethylbenzene in Example 6 (1). Aluminoxane (methylaluminoxane) was prepared.

(2) Polymerization of ethylene In Example 1 (2), the above (
Ethylene polymerization was carried out in the same manner as in Example 1 (2) except that the methylaluminoxane obtained in 1) was used. As a result, polyethylene 11Bg was obtained. Polymerization activity was 259 kg/g-Zr.

(3) Polymerization of styrene In Example 1 (3), the above (
Styrene polymerization was carried out in the same manner as in Example 1 (3) except that the methylaminoxane obtained in 1) was used. As a result, 90.5 g of polymer was obtained.

The polymerization activity was 94.5 kg/g of Ti. The racemic pentad syndiotacticity of this polymer was 97% as determined by C-NMR measurement. The results are shown in Table 2.

Comparative Example 2 Aluminoxane (methylaluminoxane) was prepared in the same manner as in Example 6(1) except that benzene (boiling point 80°C) was used instead of ethylbenzene as an additional solvent in Example 6(1). .

(2) Polymerization of ethylene In Example 1 (2), the above (
Ethylene polymerization was carried out in the same manner as in Example 1(2) except that the methylaluminoxane obtained in 1) was used. As a result, 90 g of polyethylene was obtained. Polymerization activity was 197 kg/g Zr.

(3) Polymerization of styrene In Example 1 (3), the above (
Styrene polymerization was carried out in the same manner as in Example 1 (3) except that the methylaminoxane obtained in 1) was used. As a result, 15.3 g of polymer was obtained.

Polymerization activity was 16.0 kg/g-Ti. The racemic pentad and σ syndiotacticity of this polymer was 96% as determined by 1''C-NMR measurement. The results are shown in Table 2.

(Left below) Example 10 (Copolymerization of ethylene and propylene) Contents ji
fI! 400 ml of toluene, 1 mmol of the methylaluminoxane obtained in Example 1 (1) as an aluminum atom, and 5 μmol of bis(cyclopentadienyl)zirconium monochloride monohydride were sequentially added to an autoclave at 50°C. The temperature rose. Next, propylene and ethylene were placed in an autoclave at a propylene partial pressure of 8 kg/CIa and an ethylene partial pressure of 1 kg/CIa.
Continuously introduced at a ratio of 40 to 60℃ at 60℃
The copolymerization reaction was carried out for minutes.

After the reaction, the solvent was distilled off, the product was deashed and washed with dilute hydrochloric acid-methanol, and dried under reduced pressure to obtain copolymer 4.
2.7g was obtained. Copolymerization activity is 93.6kg/g-Zr
Met. The copolymer obtained here was an ethylene-propylene copolymer with a propylene content of 41 mol%.

Example 11 (Lower polymerization of propylene) In an autoclave with content 11j2, 400 d of toluene, 6 mmol of methylaluminoxane obtained in Example 1 (1) as an aluminum atom, and 0.5 mmol of bis(pentamethylcyclopentadienyl) hafnium dichloride were added. 0
149 mol were added one after another and the temperature was raised to 50°C. after that,
After introducing hydrogen at 1 kg/ctaG,
Furthermore, propylene is continuously introduced, and the propylene partial pressure is 8
The reaction was carried out at a temperature of 50° C. for 4 hours while maintaining kg/clll. After completion of the reaction, the product was washed with 150 d of 3N hydrochloric acid aqueous solution, and 20 d of propylene low polymer
9.8g was obtained.

The obtained propylene low polymer is distilled to
A dimer fraction consisting of 4-methylpentene-1 (boiling point 53.9°C) with a purity of 99% or more, a trimer fraction consisting of 4,6-dimethylhebutene-1 (boiling point 129°C), 4.6
．． A 41-body fraction consisting of 8-trinothynonene-1 (boiling point 189°C), a 51-body fraction consisting of 4゜6.8.10-tetramethyl-undecene-1 (boiling point 230°C), and a hexamer. It was confirmed that the above ingredients were included.

[Effects of the Invention] According to the method of the present invention, highly pure and highly active aluminoxane can be easily produced.

Moreover, the highly pure aluminoxane solution obtained by the method of the present invention can be used as it is as a catalyst component for the production of olefin polymers and styrene polymers, eliminating the need for dissolving or slurrying steps. .

Therefore, the method of the present invention can be effectively utilized in the field of producing olefin polymers and styrenic polymers.

Claims (2)

[Claims] (1) Production of aluminoxane, which involves concentrating a solution obtained by reacting an organoaluminum compound and water in a solvent containing a solvent having a boiling point higher than that of the organoaluminum compound under normal pressure or reduced pressure. Method. (2) A solution obtained by reacting an organoaluminum compound and water with a solvent containing a solvent having a boiling point higher than that of the organoaluminum compound is concentrated under normal pressure or reduced pressure. A method for producing aluminoxane.