Method for synthesis of solution type neodymium phosphate complex

A complex, neodymium phosphate technology, applied in the field of compound synthesis, can solve the problems of a large amount of ethanol water waste liquid, the product is insoluble in an alkane solvent, and the neodymium phosphate drying process is cumbersome, etc., and achieves low production cost, maintains activity, and is simple in production process. Effect

Active Publication Date: 2013-07-31
PETROCHINA CO LTD
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  • Abstract
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  • Application Information

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Problems solved by technology

The neodymium phosphate catalyst prepared by this method is solid, and the drying process of neodymium phosphate is cumbersome, and a large amount of ethanol water ...

Method used

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  • Method for synthesis of solution type neodymium phosphate complex
  • Method for synthesis of solution type neodymium phosphate complex
  • Method for synthesis of solution type neodymium phosphate complex

Examples

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Embodiment 1

[0037] This embodiment provides a method for synthesizing solution-type neodymium phosphate complexes, which uses figure 1 The production device shown is carried out, and the method comprises the following steps:

[0038] 1, neodymium chloride hexahydrate is mixed with neodymium chloride aqueous solution in neodymium chloride solution still 2, and concentration is 1.31mol / L;

[0039] 2. Add 840 kg of C6 oil into the reactor 4 through the first feed port 1, then add 150 kg of 2-ethylhexyl phosphate, and stir for 5 minutes;

[0040] 3. Add 16kg of sodium hydroxide to 150kg of pure water to prepare an alkaline solution, and then add it to the reaction kettle 4 for reaction. The reaction temperature is controlled at 30-50°C, and the reaction time is controlled at 30 minutes;

[0041] 4. Add the neodymium chloride aqueous solution in the neodymium chloride solution kettle 2 to the reaction kettle 4 through the second feed port 3 for reaction, the addition amount of the neodymium c...

Embodiment 2

[0047] This embodiment provides a method for synthesizing solution-type neodymium phosphate complexes, which uses figure 1 The production device shown is carried out, and the method comprises the following steps:

[0048] 1, neodymium chloride hexahydrate is mixed with neodymium chloride aqueous solution in neodymium chloride solution still 2, and concentration is 1.31mol / L;

[0049] 2. Add 880 kg of C6 oil into the reactor 4 through the first feed port 1, then add 158 kg of bis(2-ethylhexyl) phosphate, and stir for 5 minutes;

[0050] 3. Add 16kg of sodium hydroxide to 150kg of pure water to prepare an alkaline solution, and then add it to the reactor 4 for reaction. The reaction temperature is controlled at 20-40°C, and the reaction time is controlled at 30 minutes;

[0051] 4. Add the neodymium chloride aqueous solution in the neodymium chloride solution kettle 2 into the reaction kettle 4 through the second feed port 3 to react, the addition amount of the neodymium chlori...

Embodiment 3

[0057] Using the solution-type neodymium phosphate complex prepared in Example 1 to mix and age with alkylaluminum hydrides and alkylaluminum chlorides, a rare earth catalyst that can be stored for a long time can be prepared for the polymerization of dienes such as butadiene and isoprene .

[0058] Catalyst: The catalyst is composed of solution-type neodymium phosphate complex, diisobutylaluminum hydride, and sesquiethylaluminum. The molar ratio of the three is: solution-type neodymium phosphate complex: diisobutylaluminum hydride: sesquiethylaluminum Aluminum base=1:10:3.5, wherein, the molar amount of the solution-type neodymium phosphate complex is calculated by neodymium, the molar amount of diisobutylaluminum hydride is calculated by aluminum, and the molar amount of sesquiethylaluminum is calculated by chlorine;

[0059] Preparation method: In the catalyst aging bottle under the protection of nitrogen, first add solution-type neodymium phosphate complex, then add diisob...

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Abstract

The invention relates to a method for synthesis of a solution type neodymium phosphate complex. The method comprises the steps of: preparing neodymium chloride into a neodymium chloride aqueous solution; mixing acidic phosphoric ester with an organic solvent to obtain a phosphoric ester solution, adding an alkaline solution into the phosphoric ester solution to undergo a saponification reaction to obtain a saponified liquid; adding the neodymium chloride aqueous solution into the saponified liquid to undergo a reaction, then performing separation to obtain a first oil phase; adding a complex into the first oil phase, stirring them, and then performing separation to obtain a second oil phase, which is the solution type neodymium phosphate complex. The product of the method provided by the invention is solution type neodymium phosphate, and the product is miscible with alkane, arene and other solvents in arbitrary proportion. In a multicomponent catalyst aging process, more and freer aging modes can be selected. In addition, the method provided in the invention has an obviously simple production process and a low production cost, and the sodium chloride aqueous solution obtained in a layering process can be safely discharged after treatment and does not cause environmental pollution.

Description

technical field [0001] The invention relates to a method for synthesizing neodymium phosphate, in particular to a method for synthesizing a solution-type neodymium phosphate complex, which belongs to the technical field of compound synthesis. Background technique [0002] Neodymium phosphate catalyst and other components are combined and aged in different ways, and can be used as an olefin polymerization catalyst. The research on the use of neodymium phosphate as an olefin polymerization catalyst has been reported in the 1970s, and the neodymium phosphate catalyst used is a solid neodymium phosphate catalyst. [0003] "Catalytic Activity of Rare Earth Compounds with Different Coordinating Groups in Isoprene Polymerization" in "Rare Earth Catalyzed Synthetic Rubber Collection" (Science Press, 1980, the Fourth Laboratory of Changchun Institute of Applied Chemistry, Chinese Academy of Sciences) The preparation method of neodymium phosphate catalyst is disclosed, and the produc...

Claims

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Application Information

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IPC IPC(8): C07F9/11C08F4/52C08F36/06C08F36/08
Inventor 石路颖张志强张凯谷素艳
Owner PETROCHINA CO LTD
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