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Preparation method of multifunction organic metal initiator for anionic polymerization

An organic alkali metal and anionic polymerization technology, which is applied in the field of preparation of multifunctional organic alkali metal initiators for anionic polymerization, can solve problems affecting polymer quality, unfavorable long-term maintenance of initiator activity, and affecting initiator functionality. The effect of low production cost, less equipment demand, and less waste

Inactive Publication Date: 2011-01-12
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0016] (2) If you do not use aromatic hydrocarbons but only use alkanes as solvents, it will affect the control of the initiator functionality due to the inhomogeneity of the first step reaction, thereby affecting the quality of the polymer
[0017] (3) The presence of aromatic hydrocarbons is not conducive to the long-term maintenance of initiator activity

Method used

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  • Preparation method of multifunction organic metal initiator for anionic polymerization

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] Add 22 mmoles of lithium naphthalene to a purified 250 mL polymerization bottle with electromagnetic stirring. Add 100 mL of butadiene-cyclohexane solution with a concentration of 60 g / L in four times, and react at 25° C. for half an hour after each addition. After the reaction was completed, 2.7 mmoles of tin tetrachloride solution was added, and the reaction was stopped at 25° C. for another 1 hour. The product is a polyfunctional organolithium initiator with an average functionality of 3.7.

Embodiment 2

[0054] Add 25mL of cyclohexane solution of butadiene to the purified 250mL polymerization bottle with electromagnetic stirring, the monomer concentration is 60 g / L, add 22 mmoles of lithium naphthalene, react at 25°C for half an hour, and then keep the reaction temperature at At 25°C, 75 mL of isoprene-cyclohexane solution was added dropwise within 1 hour, and reacted at 25°C for half an hour after all the addition was completed. Add 2.5 mmol tin tetrachloride solution, and stop the reaction after reacting at 25°C for 1 hour. The product is a polyfunctional organolithium initiator with an average functionality of 2.5.

Embodiment 3

[0056] Add 13mL of butadiene-cyclohexane-hexane solution to the purified 250mL polymerization bottle with electromagnetic stirring, the monomer concentration is 80 g / L, cyclohexane: hexane is 80:20, add naphthalene lithium 20 Millimole, react at 25°C for half an hour; then add butadiene solution 13mL, 14mL, and 14mL in three batches, and react at 25°C for half an hour after each addition. After the reaction was completed, 2.5 mmoles of tin tetrachloride solution was added, and the reaction was stopped at 25°C for another 1 hour. The product is a polyfunctional organolithium initiator with an average functionality of 3.8.

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Abstract

This invention relates to the preparation method of a multifunctional group organic alkali metal initiator used for anionic polymerization. First aryl alkali metals and conjugated diene hydrocarbon or vinyl monomer takes reaction, then by stage add monomeric alkane solution, finally after reaction adds halide. The initiator can be expressed as follow general expression: Ma (RMe). M element includes Sn, Ti, Al, Si, B; R is alkyl, a is one to three, b is 2.5 to 6.5, Me is alkali metals, includes Na nad Li. This synthetic craft produce less three wastes, functionality lend itself to regulative, and obtained initiator solution not contain aromatic solvent, activating could keep 1 mouth.

Description

technical field [0001] The invention relates to a preparation method of a multifunctional organic alkali metal initiator for anionic polymerization. Background technique [0002] Organolithium initiators are widely used in anionic polymerization. According to the number of active centers contained in each molecule after initiation, it can be divided into single lithium initiators, such as RLi; dilithium initiators, such as naphthalene lithium; and multifunctional organic lithium initiators (number of active centers per molecule ≥ 3) Several kinds. [0003] Multifunctional organolithium initiators are mainly used in the synthesis of star-shaped polymers. Compared with linear polymers, star-shaped polymers have their own characteristics. For example, compared with linear solution-polymerized styrene-butadiene, star-shaped solution-polymerized styrene-butadiene has better comprehensive mechanical properties, mainly in low rolling resistance and good wet skid resistance. It is...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F4/46C08F297/04C08F236/06C08F210/02
Inventor 姚明张兴英赵素合吴友平
Owner BEIJING UNIV OF CHEM TECH
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