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Method for evaluating rare earth isoprene rubber production materials by bottle polymerization with neodymium n-valerate

A technology of rare earth isoprene rubber and neodymium n-valerate, which is applied in the preparation of organic compounds, chemical instruments and methods, and preparation of carboxylate, which can solve the problems that dissolved oxygen is not suitable for removal, oxygen content is difficult to measure, and is difficult to take. , to achieve the effect of great market promotion and application value, stable quality, convenient storage, transportation and use

Active Publication Date: 2019-03-19
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When used as the main catalyst of the catalyst used in bottle polymerization evaluation, the neodymium carboxylate hexane solution has the following disadvantages: (1) the concentration is easily changed due to solvent volatilization during storage; (2) the moisture content is increased due to moisture absorption Distillation and dehydration are required, and the test concentration should be re-analyzed, which is complicated to operate; (3) Dissolved oxygen should not be removed, and the oxygen content is not easy to measure; (4) The danger of transportation and storage is high
[0007] The neodymium carboxylate hexane solution in the above papers and patents is a viscous solid after drying and removing the solvent, which is difficult to take
U.S. Patent No. 5,783,676 discloses a synthetic method of solid powdery neodymium carboxylate, which requires that the carboxylic acid ligand is preferably a branched carboxylic acid, and controls the pH of the reaction solution to be greater than 7.5, in order to ensure that the obtained carboxylic acid Neodymium products are in the form of fine powder, which is convenient for preparing diolefin coordination polymerization catalysts and improving the activity of the catalysts, but it is not the best choice as the main catalyst of the catalyst used in the bottle polymerization evaluation of rare earth isoprene rubber production materials

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] A. Synthesis of neodymium n-valerate

[0030] Under normal temperature and stirring state, add 1.0g n-valeric acid into 99mL deionized water to prepare n-valeric acid aqueous solution, then add 1.3g 30% sodium hydroxide aqueous solution, then add 2.7g 30% neodymium chloride aqueous solution, use pH The pH of the reaction product was measured by test paper to be 5. After stirring and reacting for 30 minutes, the generated neodymium n-valerate was precipitated and filtered, and the filter cake was washed twice with deionized water. Dry 2h in oven, be ground into powder, then dry 2h, product weighs 1.31g, records moisture with Karl Fischer moisture analyzer and is 1.0%, records neodymium element content with EDTA complexometric titration method and is 0.00221g / mol, And sealed and stored in a glass desiccator for later use.

[0031] B. Bottle polymerization evaluation

[0032] Draw 10mL of triisobutylaluminum (2mol / L) and 2mL of diethylaluminum chloride (2mol / L) into an a...

Embodiment 2

[0037] A. Synthesis of neodymium n-valerate

[0038] Under normal temperature and stirring state, add 3.0g n-valeric acid into 97mL deionized water to prepare n-valeric acid aqueous solution, then add 2.93g 40% sodium hydroxide aqueous solution, then add 5.8g 40% neodymium chloride aqueous solution, use pH The PH value of the reaction product measured by the test paper is 7. After stirring and reacting for 30 minutes, the generated neodymium n-valerate is precipitated and filtered, and the filter cake is washed twice with deionized water. Dry in a vacuum oven for 2h, then grind into powder, then dry for 2h, the product weighs 3.90g, the moisture is 2.0% as measured by the Karl Fischer moisture analyzer, and the neodymium element content is 0.00225g / mol as measured by the EDTA complexometric titration method , and sealed and stored in a glass desiccator for later use.

[0039] B. Bottle polymerization evaluation

[0040] Draw 9mL of triisobutylaluminum (2mol / L) and 3mL of die...

Embodiment 3

[0045] A. Synthesis of neodymium n-valerate

[0046] Under normal temperature and stirring state, add 2.0g n-valeric acid into 98mL deionized water to prepare n-valeric acid aqueous solution, then add 2.24g 35% sodium hydroxide aqueous solution, then add 4.60g 35% neodymium chloride aqueous solution, use pH The pH of the reaction product was measured by test paper to be 6. After stirring and reacting for 30 minutes, the resulting neodymium n-valerate was precipitated and filtered, and the filter cake was washed twice with deionized water. Dry it in an oven for 2 hours, grind it into powder, and dry it for another 2 hours. The product weighs 2.72g, and the moisture is 1.5% as measured by Karl Fischer moisture analyzer, and the content of neodymium element is 0.00223g / mol as measured by EDTA complexometric titration, and is sealed and stored in a glass desiccator for subsequent use.

[0047] B. Bottle polymerization evaluation

[0048] Draw 10mL of triisobutylaluminum (2mol / L)...

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PUM

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Abstract

The invention discloses a method for synthesizing n-pentanoic acid neodymium and evaluating rare earth isoprene rubber production material through bottle polymerization with n-pentanoic acid neodymium. The method for synthesizing the n-pentanoic acid neodymium includes raw material, feed proportion, reaction control condition and product purification, and the purity of products of the n-pentanoic acid neodymium is in 0.0021-0.0025mol / g in neodymium content and 1.0%-2.0% in water content; the method for evaluating the rare earth isoprene rubber production material includes the process for preparation a polymerization catalyst of the n-pentanoic acid neodymium, polymerization material treatment and bottle polymerization. The synthesizing process is simple, high in product purity, stable in quality and convenient and safe in store transportation and use; the method for evaluating the bottle polymerization on the basis of the synthesized n-pentanoic acid neodymium is simple and easy to implement as compared with a traditional method, the evaluation results are good in repeatability, standard methods are easy to form, and high market promotion application value is achieved.

Description

technical field [0001] The invention belongs to the technical field of synthetic polymer material production, and more specifically relates to a synthesis method of neodymium n-valerate and a method for evaluating rare earth isoprene rubber production materials through bottle polymerization using a catalyst prepared from the neodymium n-valerate. Background technique [0002] Cis-1,4-polyisoprene rubber (referred to as isoprene rubber) is an important synthetic rubber obtained by directional polymerization of isoprene. It has excellent comprehensive properties because of its molecular structure and natural rubber The same, the performance is close to natural rubber, so it is also commonly known as synthetic natural rubber. It can be used alone or in combination with natural rubber or other synthetic rubber to replace or partially replace natural rubber. [0003] The production of isoprene rubber in foreign countries originated in the 6C of the last century. According to dif...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F136/08C08F4/52C07C51/41C07C53/126
CPCC07C51/412C08F136/08C08F4/52C07C53/126
Inventor 项曙光王继叶孙晓岩夏力
Owner QINGDAO UNIV OF SCI & TECH