Preparation method and application of solution type rear earth catalyst

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

Inactive Publication Date: 2014-12-17
LIAONING HEYUN SYNTHETIC RUBBER RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] 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 WO 02 / 38635 and WO 02 / 38636 that after dissolving the solid catalyst at high temperature, various components are added to prepare the catalyst to polymerize isoprene, but the obtained catalytic system is a viscous, unstable suspension. The stability of the polymer has some influence
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)

Method used

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  • Preparation method and application of solution type rear earth catalyst
  • Preparation method and application of solution type rear earth catalyst
  • Preparation method and application of solution type rear earth catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Embodiment 1: the preparation of solution type rare earth catalyst, this method comprises the following steps:

[0024] 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

[0025] Embodiment 2: the preparation of solution type rare earth catalyst, this method comprises the following steps:

[0026] 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

[0027] Embodiment 3: the preparation of solution type rare earth catalyst, this method comprises the following steps:

[0028] 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 rear earth catalyst and application of the solution type rear earth catalyst to diolefin polymerization. The preparation method comprises the following steps of adding alcohol chemical compounds into rear earth compounds; after reaction is completed, adding the reactants into organophosphorus ester; after the reaction happens for a period of time, adding rear earth compounds and performing dilution through organic solvent; after the reaction is completed, sealing the solution type rear earth catalyst for standby. The solution type rear earth catalyst can achieve dual/ternary aging modes to obtain a homogeneous phase rear earth catalysis system, avoid the problem of control difficulty of molecular weight and molecular weight distribution of polymers prepared through heterogeneous rear earth catalysts and bring convenience to technological design of industrial production. Meanwhile, the solution type rear earth catalyst can avoid generating water solution and omit multiple washing and drying of products, is simple in process and low in cost, avoids layered alkali washing and achieves simple post-processing and environmental protection. Correspondingly, the invention also provides the application of preparation of homogeneous phase catalysis systems through the solution type rear earth catalyst to catalysis of diolefin polymerization.

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] [0003] 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 d...

Claims

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Application Information

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