Prepn process of alkyl aluminoxane
A technology of alkylaluminoxane and alkylaluminum, which is applied in the field of preparation of alkylaluminoxane, can solve problems such as poor fluidity, high sealing requirements for solid feeders, and insufficiently uniform feeding, so as to reduce equipment costs and solve Bridge problem, the effect of improving production capacity
Inactive Publication Date: 2007-04-11
PETROCHINA CO LTD
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Problems solved by technology
Its main disadvantage is: since the alkylaluminum solution is gradually added to the suspension of crystal hydrate, most of the initially added alkylaluminum is converted into Al(OH) by the relatively excess water in the system 3 , only when the concentration of free water in the system is reduced to a certain extent, Al(OH) 3 side effects are reduced to a minor level
[0004] However, the problems in this preparation process are: due to the high sensitivity of alkylaluminum and alkylaluminoxane to moisture and air, the tightness of the solid feeder is high; due to the poor fluidity of crystalline hydrates of salts, Therefore, there is a certain degree of bridge during the operation, the feeding is not uniform enough, and it needs to be cleaned frequently
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Embodiment 1
[0021] After the reaction bottle has been fully vacuum-nitrogen replaced, add 500ml4mol·L -1 TMA toluene solution, started to stir, 92gAl by slurry pump at room temperature 2 (SO 4 ) 3 18H 2 The suspension prepared by O and 500ml of toluene was gradually added into the reaction flask. After the addition, the temperature was gradually raised to 40° C., stirred for 13 hours, and the reaction was stopped. The solid was filtered off, and the solvent was removed under reduced pressure to obtain 59.4 g of white methylaluminoxane solid. The yield of the target product methylaluminoxane was 51.2%.
[0022] Take this methyl aluminoxane 1.7 grams and 0.05g Cp 2 ZrCl 2 , at 60°C and 0.8Mpa, ethylene was polymerized for 1 hour to obtain 732 grams of polyethylene;
[0023] Get this methylaluminoxane 1.7 grams and 0.08g (2,4-diMePh) 2 PBIM 2 FeCl 2 , At 60°C and 0.8Mpa, ethylene was polymerized for 1 hour to obtain 608 grams of polyethylene.
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The present invention provides the preparation process of alkyl aluminoxane as metallocene and post-transition metal co-catalyst. Alkyl aluminoxane is prepared with the suspension of crystallized hydrate and hydrocarbon as organic solvent and alkyl aluminum through continuous reaction, and the target product has high yield and excellent co-catalytic effect.
Description
technical field [0001] The invention relates to a method for preparing metallocene and late transition metal cocatalysts-alkylaluminoxanes for olefin polymerization. Background technique [0002] There are many preparation methods of alkylaluminoxane, but they can be summarized into the following two categories: direct water process and indirect water process. The yield of the target product of the direct water process is relatively high, but the production process is more dangerous. At the same time, in order to solve the production process, it is often necessary to design various special equipment, which greatly increases the investment cost of the device construction ( US4924018, US4772736, US4937363, US4908463, US5087713, US5041585). The indirect water process generally adopts the reaction of crystalline hydrate and alkylaluminum. The preparation process reported in the existing literature is the preparation process in which the crystalline hydrate and the solvent are ...
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IPC IPC(8): C07F5/06
Inventor 韦少义朱博超吴江魏红朱雅杰张长军郝萍刘颖薛蕴玲
Owner PETROCHINA CO LTD