Method for preparing modification aluminoxane

A modification technology of alkyl aluminoxane, which is applied in the field of preparation of modified alkyl aluminoxane, which can solve the problem of affecting the storage stability and use effect of aluminoxane, the content of active ingredients of target products caused by local overheating, and the effect of catalytic effect and other problems, to achieve good catalytic effect, improve storage stability and use effect, and improve production flexibility

Inactive Publication Date: 2011-09-21
NORTHEAST GASOLINEEUM UNIV
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AI Technical Summary

Problems solved by technology

In the above two methods, controlling the reaction rate is still a difficult problem
[0007] Due to the formation of molecular clusters between water molecules through the action of hydrogen bonds, it is easy to cause local overheating and a decrease in the content of active ingredients in the target product due to excessive local water concentration during the process of hydrolysis. Water dispersion is still not a good solution to this problem
In addition, the inhomogeneity of the reaction resulted in about 10% residual aluminum alkyl in the product
Ineffective ingredients in aluminoxane will not only affect the catalytic effect, but also lead to the formation of polymers with relatively large molecular weight, that is, gel, which will affect the storage stability and use effect of aluminoxane

Method used

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  • Method for preparing modification aluminoxane

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Effect test

Embodiment 1

[0030] Under the protection of high-purity nitrogen, make triethylaluminum into 500mL of 2.5mol / L toluene solution, transfer it to the storage tank of alkylaluminum solution; , the modifier (methanol) and toluene were mixed and stirred at high speed for 10 minutes to form a mixture of 350 mL of hydrolyzing agent, which was transferred to the hydrolyzing agent storage tank and kept stirring at a speed of 1000 rpm.

[0031] After the reaction device equipped with nitrogen, venting system and cooling system is fully vacuumed-nitrogen replacement operation, two feed pumps are turned on, the flow rate of triethylaluminum solution is 4mL / min, and the flow rate of hydrolyzing agent is 2.8mL / min. material. The two feeds are cooled to -15°C through the cooling coil immersed in the cold bath, and then enter the T-shaped tube reactor for mixing and then flow into the reactor 1. The reaction liquid enters the continuously stirred reactor 1 from the upper part for degassing and further Re...

Embodiment 2

[0036] Under the protection of high-purity nitrogen, make triethylaluminum into 500mL of 2.5mol / L toluene solution, and transfer it to the storage tank of alkylaluminum solution; : After mixing in the ratio of 75 (V / V / V), high-speed stirring was carried out for 10 minutes, and the formed mixture was 850 mL of hydrolyzing agent, which was transferred to the hydrolyzing agent storage tank, kept stirring, and the stirring speed was 600 rpm.

[0037] After the reaction device equipped with nitrogen, venting system and cooling system is fully deoxygenated-nitrogen replacement operation, two feed pumps are turned on, the flow rate of triethylaluminum solution is 5mL / min, and the flow rate of hydrolyzing agent is 8.4mL / min. material. The two feeds are cooled to -10°C through the cooling coil immersed in the cold bath, and then enter the T-shaped tube reactor for mixing and then flow into the reactor 1. The reaction liquid enters the continuously stirred reactor 1 from the upper part ...

Embodiment 3

[0042] Under the protection of high-purity nitrogen, make triisobutylaluminum into 500mL of 4.0mol / L toluene solution, and transfer it to the storage tank of alkylaluminum solution; Mix at a ratio of 0.25:113 (V / V / V) and then stir at high speed for 10 minutes. The resulting mixture is 910 mL of hydrolyzing agent, which is transferred to the storage tank of hydrolyzing agent and kept stirring at a stirring speed of 1000 rpm.

[0043] After the reaction device equipped with nitrogen, venting system and cooling system is fully deoxygenated-nitrogen replacement operation, two feed pumps are turned on, the flow rate of triethylaluminum solution is 5mL / min, and the flow rate of hydrolyzing agent is 9.1mL / min. material. The two feeds are cooled to -20°C through the cooling coil immersed in the cold bath, and then enter the T-shaped tube reactor for mixing and then flow into the reactor 1. The reaction liquid enters the continuously stirred reactor 1 from the upper part for degassing an...

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Abstract

The invention discloses a preparation method for modification aluminoxane, comprising the following steps: a) preparing an inertia solvent solution of aluminium alkyl under the protection of an inert gas; b) mixing water, a modifier and an inertia solvent to prepare a hydrolysis agent under the protection of an inert gas; c) mixing the inertia solvent solution of aluminium alkyl and the hydrolysis agent in a T-type pipe reactor at a temperature of between -10 DEG C and -50 DEG C, flowing the mixture into a kettle reactor, heating the mixture to a temperature of between 10 to 100 DEG C and reacting for 1 to 10 hours; d) obtaining a reaction solution by filtering, reducing pressure to remove the solvent to obtain alkylauminoxane. According to the method of the invention, the interacting effect of the modifier and water is utilized to control the local concentration of water and the composition and concentration of the modifier are used to influence the composition of the generated aluminoxane so as to improve the storage stability and usage effect of the alkylauminoxane.

Description

technical field [0001] The invention relates to a preparation method of a modified alkyl aluminoxane, in particular to a method for preparing an alkyl aluminoxane by a direct hydrolysis process. Background technique [0002] At present, the main preparation method of alkylaluminoxane is the hydration method, which is divided into two categories: direct hydration and indirect water hydration according to the state of the reaction water. Among them, the direct hydration method usually uses free gaseous, liquid or solid water, while the indirect hydration method mainly uses the crystal water of the compound and the water adsorbed on the surface of the porous material. [0003] In the indirect water process, the reaction between crystalline hydrate and alkylaluminum is mostly used. Usually, the crystalline hydrate and the solvent are pre-prepared into a suspension in the reactor, and the alkylaluminum solution is gradually added to the suspension (positive addition method) or t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F5/06B01J31/14C07C11/02C07C2/32C07C2/30
Inventor 毛国梁姜涛宁英男罗明检吴韦陈洪侠张海燕
Owner NORTHEAST GASOLINEEUM UNIV
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