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A kind of preparation method and application of solution type rare earth catalyst

A rare-earth catalyst and solution-type technology, which is applied in the chemical industry, can solve the problems of cumbersome steps, influence on polymer stability, cumbersome extraction steps, etc., and achieve the effects of simple preparation process, realize adjustability, and convenient process design

Inactive Publication Date: 2016-06-29
LIAONING HEYUN SYNTHETIC RUBBER RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Chinese patent CN103224517A provides a method for preparing a solution-type neodymium phosphate complex. In the patent, the preparation of the neodymium phosphate complex requires adding an alkaline solution for saponification reaction, and two separations are required to obtain the second oil phase as a solution-type neodymium phosphate complex. objects, the steps are relatively cumbersome
CN103694378A provides a method for synthesizing a solution-type rare earth rubber catalyst. The method uses alkaline solution for washing, and post-processing the waste water generated during production will increase its industrial cost accordingly
CN101724115A provides a kind of rare earth sulfonate catalyst used for preparing polyisoprene rubber. In its preparation method, it involves the preparation of neodymium sulfonate compounds and complexes, which requires crystallization and purification, and has certain limitations for the specific implementation of industrialized actual production. difficulty
It is mentioned in WO02 / 38635 and WO02 / 38636 that after the solid catalyst is dissolved at high temperature, various components are added to prepare the catalyst to polymerize isoprene, but the obtained catalytic system is a viscous, unstable suspension, which is harmful to the polymer the stability of the
In the existing literature reports, the preparation of neodymium naphthenate catalyst by direct extraction also requires alkali washing and phase separation, and the extraction steps are cumbersome (references: Yang Jihua, Pang Shufen, Gong Zhi, Applied Chemistry, 1996, 13, 117)

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  • A kind of preparation method and application of solution type rare earth catalyst

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Experimental program
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Effect test

Embodiment 1

[0022] Embodiment 1: the preparation of solution type rare earth catalyst, this method comprises the following steps:

[0023] Add 0.25ml of propylene glycol to 0.1g of neodymium trioxide, react at 80°C to obtain a catalyst precursor, add the catalyst precursor to 5ml of diisooctyl phosphate, stir for 30min, add 1g of neodymium trioxide, and use 30ml ring Diluted with hexane, reacted at 80°C for 2 hours, no precipitation after standing still for 10 minutes, the reaction was completed, and the obtained lavender solution was sealed under nitrogen protection for future use.

Embodiment 2

[0024] Embodiment 2: the preparation of solution type rare earth catalyst, this method comprises the following steps:

[0025] Add 0.25ml of propylene glycol to 0.1g of neodymium chloride, react at 90°C to obtain a catalyst precursor, add the catalyst precursor to 5ml of di-isooctyl phosphate, stir for 30 minutes, add 1g of neodymium trioxide, and use 30ml of cyclohexane dilute with alkane, and react at 90°C for 2 hours. After standing still for 10 minutes, there is no precipitation, and the reaction is complete. The obtained lavender solution is sealed under nitrogen protection for future use.

Embodiment 3

[0026] Embodiment 3: the preparation of solution type rare earth catalyst, this method comprises the following steps:

[0027] Add 0.5ml of isopropanol to 0.1g of neodymium chloride, and react at 85°C to obtain a catalyst precursor. Add the catalyst precursor to 5ml of diisooctyl phosphate, stir for 30 minutes, add 1g of neodymium trioxide, and use Dilute with 30ml of cyclohexane, react at 85°C for 2 hours, no precipitation after standing still for 10 minutes, the reaction is complete, and the obtained lavender solution is sealed under nitrogen protection for later use.

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Abstract

The invention relates to a preparation method of a solution type rare earth catalyst and its application in diolefin polymerization. The method comprises the following steps: adding an alcohol compound to the rare earth compound, adding it to the organic phosphate after reacting, adding the rare earth compound again after a period of reaction, diluting with an organic solvent, and sealing it for future use after the reaction is completed. The product can achieve binary / ternary multiple aging methods to obtain a homogeneous rare earth catalyst system, which avoids the problem that the molecular weight and molecular weight distribution of polymers prepared by heterogeneous rare earth catalysts are difficult to control, and brings great benefits to the process design of industrial production. convenient. At the same time, the main catalyst prepared by the method does not produce aqueous solution, does not involve multiple washing and drying of products, has simple process, low cost, does not need layered alkali washing, simple post-treatment, and is environmentally friendly. Correspondingly, the present invention also provides an application of a homogeneous catalytic system prepared from the above main catalyst in catalyzing the polymerization of diolefins.

Description

technical field [0001] The invention relates to a method for preparing a rare earth catalyst, in particular to synthesizing a solution-type rare earth main catalyst, and preparing a homogeneous rare earth catalyst, which is especially suitable for catalyzing the polymerization of diolefins and obtaining highly directional products, and belongs to the technical field of chemical industry . technical background [0002] As the country with the most abundant rare earth resources, China has been committed to research on the application of rare earths. In the 1960s, rare earth catalysts could be used to polymerize olefins after aging with alkyl aluminum and other components, which opened up a new synthesis method for polymer synthesis. The previous research work on rare earth catalysts was all solid catalysts, and the obtained catalytic system was heterogeneous. The heterogeneous catalytic system may have problems such as multiple active centers, poor stability, and difficult c...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F4/54C08F4/52C08F136/08
Inventor 马海芳裴素明高凯
Owner LIAONING HEYUN SYNTHETIC RUBBER RES INST