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Method for preparing catalysts for manufacturing polycarbonate diols

A technology of polycarbonate and diol, which is applied in the field of catalyst preparation to achieve the effects of high catalytic efficiency, high purity and simple operation

Inactive Publication Date: 2015-11-25
宁波诺尔丽化学科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, these catalysts have many disadvantages

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] The preparation method of the catalyst for producing polycarbonate diol includes the following steps,

[0025] A. Prepare a mixed solution of divalent metal ion solution and trivalent metal ion solution;

[0026] B. Titrate the mixed solution of divalent metal ion solution and trivalent metal ion solution, sodium hydroxide and sodium carbonate at the same time, the temperature is controlled at 60℃, the PH value is controlled at 8, and stirred for 4 hours;

[0027] C. Wash with water to pH 7, dry, grind, calcinate, and after cooling, mix with Lewis base and calcinate again to obtain the catalyst for producing polycarbonate diol.

[0028] The divalent metal ion solution is one of magnesium chloride solution, magnesium nitrate solution, copper sulfuric acid solution, calcium chloride solution, and zinc nitrate. The trivalent metal ion solution is one of aluminum chloride solution, aluminum nitrate, and ferric chloride.

Embodiment 2

[0030] The preparation method of the catalyst for producing polycarbonate diol includes the following steps,

[0031] A. 0.06mol of divalent metal ion solution and 0.02mol of trivalent metal ion solution are dissolved in 80ml of deionized water to prepare a mixture of divalent metal ion solution and trivalent metal ion solution.

[0032] In step B, 0.16mol NaOH and 0.04mol Na 2 CO 3 Dissolve in 80ml of deionized water to obtain a mixture of sodium hydroxide and sodium carbonate; titrate the mixture of divalent metal ion solution and trivalent metal ion solution, sodium hydroxide and sodium carbonate at the same time, and the temperature is controlled at 50℃ , PH value is controlled at 8, and white slurry is obtained to stop the reaction. C. Washed with water to pH 7, dried at 60°C for 12h, then dried at 120°C for 3h, ground, calcined, cooled, mixed with Lewis base and calcined again to obtain a catalyst for producing polycarbonate diol .

[0033] The divalent metal ion solution is ...

Embodiment 3

[0035] The preparation method of the catalyst for producing polycarbonate diol includes the following steps,

[0036] A. 0.06mol of divalent metal ion solution and 0.02mol of trivalent metal ion solution are dissolved in 80ml of deionized water to prepare a mixture of divalent metal ion solution and trivalent metal ion solution.

[0037] In step B, 0.16mol NaOH and 0.04mol Na 2 CO 3 Dissolve in 80ml of deionized water to obtain a mixture of sodium hydroxide and sodium carbonate; titrate the mixture of divalent metal ion solution and trivalent metal ion solution, sodium hydroxide and sodium carbonate at the same time, and the temperature is controlled at 65℃ , PH value is controlled at 10, get white slurry to stop the reaction. C. Wash with water to pH 7, dry, grind, and calcinate in a muffle furnace at 500°C for 5 hours. After cooling, mix with Lewis base. Add 1 g of Lewis base to every 10 g of calcined product, and then It is calcined in a muffle furnace at 500°C for 5 hours to o...

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PUM

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Abstract

The invention relates to the field of organic synthesis, and discloses a method for preparing catalysts for manufacturing polycarbonate diols. The method includes steps of preparation phases, hydrotalcite preparation and Lewis base loading. The method has the advantages that Lewis base is immobilized on the basis of hydrotalcite, and accordingly the catalysts can be applied to generating the polycarbonate diols by the aid of a small-molecule carbonate ester exchange process and are high in catalytic efficiency, good in reaction selectivity and free of oligomerization; the catalysts prepared by the aid of the method can be applied to generating the polycarbonate diols, obtained products are high in purity, and accordingly the technical problem that generation of polycarbonate diols can be affected by other impurities in catalysts produced in the prior art can be solved; the products are free of mixed colors, and accordingly the technical problem of discoloration (such as yellow discoloration) of products in the prior art can be solved; the obtained products do not need to be further treated, and the catalysts remain in polyols without affecting follow-up reaction.

Description

Technical field [0001] The invention relates to the field of organic synthesis, in particular to a preparation method of a catalyst for producing polycarbonate diols. Background technique [0002] The synthesis methods of polycarbonate diols include phosgene method, carbon dioxide epoxide adjustment copolymerization method, ring-opening polymerization method of cyclic carbonate, and small molecule carbonate exchange method. The catalyst of the present invention is applied to the small molecule carbonate ester exchange method. [0003] The catalysts used in the transesterification method to synthesize polycarbonate diols are mostly homogeneous catalysts, such as alkali metals or alkaline earth metals and their alkoxides, tin or organotin compounds, and titanium compounds. However, these catalysts have many disadvantages. When using strong bases such as alkali metals or alkaline earth metals or their alkoxides, once the oligomerization reaction occurs, additional process steps must...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G64/20
Inventor 郁之义
Owner 宁波诺尔丽化学科技有限公司
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