Method for synthesizing neodymium phosphate solution and synthesized neodymium phosphate solution

A neodymium phosphate and solution technology, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve the problems of single composition of neodymium phosphate solution, inability to effectively reduce the viscosity of glue, and improve processing performance and reduce glue viscosity. , the effect of reducing energy loss

Active Publication Date: 2016-11-23
PETROCHINA CO LTD
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Problems solved by technology

[0007] The object of the present invention is to provide a kind of preparation method of neodymium phosphate solution and the prepared neodymium phosphate solution, to solve the single composition of neodymium phosphate solution prepared by the prior art method, can not effectively reduce in the polymerization catalytic process as synthetic rubber Defects in Glue Viscosity

Method used

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  • Method for synthesizing neodymium phosphate solution and synthesized neodymium phosphate solution

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Effect test

Embodiment 1

[0057] The present embodiment provides a kind of method for synthesizing neodymium phosphate solution, it is to adopt figure 1 The production device shown is carried out, and the method comprises the following steps:

[0058] 1, nickel chloride hexahydrate is mixed with saturated nickel chloride aqueous solution in nickel chloride solution kettle 2;

[0059] 2. Add 840 kg of C6 oil into the reaction kettle 4 through the first feed port 1, then add 150 kg of 2-ethylhexyl phosphate 2-ethylhexyl ester, 5 kg of molecular sieve, and heat and stir for 5 minutes;

[0060] 3. Add 25 kg of neodymium oxide solid powder into the reaction kettle 4 through the third feed port 6, and stir for 5 minutes;

[0061] 4. Add the saturated nickel chloride aqueous solution in the nickel chloride solution kettle 2 to the reaction kettle 4 through the second feed port 3 for reaction, the amount of the saturated nickel chloride aqueous solution is 5L, and the reaction temperature is controlled at 35-...

Embodiment 2

[0065] The present embodiment verifies saturated nickel chloride solution its catalysis in embodiment 1 synthetic neodymium phosphate solution method, and this verification test comprises the following steps:

[0066] 1. Add 840 kg of C6 oil into the reaction kettle 4 through the first feed port 1, then add 150 kg of 2-ethylhexyl phosphate 2-ethylhexyl ester, add 5 kg of molecular sieves, and heat and stir for 5 minutes;

[0067] 2. Add 25 kg of neodymium oxide solid powder into the reaction kettle 4 through the third feed port 6, and stir for 5 minutes; control the temperature of the mixed solution at 50-55° C., and stir for 60 minutes, and no reaction occurs in the neodymium oxide;

[0068] 3, nickel chloride hexahydrate is mixed with saturated nickel chloride aqueous solution in nickel chloride solution kettle 2;

[0069] 4. Add the saturated nickel chloride aqueous solution in the nickel chloride solution kettle 2 to the reaction kettle 4 through the second feed port 3 for...

Embodiment 3

[0073] The present embodiment provides a kind of method for synthesizing neodymium phosphate solution, it is to adopt figure 1 The production device shown is carried out, and the method comprises the following steps:

[0074] 1. Titanium chloride hexahydrate is mixed with a saturated titanium chloride aqueous solution in the titanium chloride solution kettle 2;

[0075] 2. Add 840 kg of C6 oil into the reaction kettle 4 through the first feed port 1, then add 150 kg of 2-ethylhexyl phosphate 2-ethylhexyl ester, 5 kg of molecular sieve, and heat and stir for 5 minutes;

[0076] 3. Add 25kg of neodymium oxide solid powder into the reaction kettle 4 through the third feed port 6, stir for 5 minutes, control the temperature of the mixed solution to 20-50°C, stir for 60 minutes, and no reaction occurs in the neodymium oxide;

[0077] 4. Add the saturated titanium chloride aqueous solution in the titanium chloride solution kettle 2 to the reaction kettle 4 through the second feed p...

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Abstract

The invention discloses a method for synthesizing a neodymium phosphate solution and the synthesized neodymium phosphate solution. The method comprises steps as follows: a saturated metal halide salt water solution is prepared from metal halide salt; acidic phosphate ester and an organic solvent are mixed, a phosphate ester solution is obtained, and the volume ratio of acidic phosphate ester to the organic solvent is (1:2)-(1:20); neodymium oxide solid powder is added to the phosphate ester solution and stirred, and a turbid liquid is obtained and heated to 20-50 DEG C; the saturated metal halide salt water solution is added to the turbid liquid, heated and stirred, molecular sieves are added, the mixture reacts at the temperature of 20-70 DEG C for 20-90 minutes, is left to stand for layering after the reaction ends and then is separated, an oil phase, namely, the neodymium phosphate solution is obtained, and the mole ratio of metal halide salt to acidic phosphate ester is controlled to range from (1:5) to (1:50). The neodymium phosphate solution contains a little non-rare-earth metal phosphate, can reduce the viscosity of a glue solution in the polymerization catalysis process of synthetic rubber and reduces production loss; the molecular weight distribution of the synthetic rubber is widened, and the processability of the rubber is improved.

Description

technical field [0001] The invention relates to a method for synthesizing a neodymium phosphate solution, in particular to a method for synthesizing a neodymium phosphate solution using a saturated metal halide solution as a catalyst, and 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, Fourth Laboratory of Changchun Institute of Applied Chemistry, Chinese Academy of Sciences) The preparation method of neodymium p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/38
Inventor 齐晓梅张志强梁英超李传光李潇郭中台
Owner PETROCHINA CO LTD
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