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Method for preparing load-type zirconium oxide and its using method

An application method and catalyst technology are applied in the field of preparation of supported zirconia catalysts, which can solve the problems of unrecyclable homogeneous catalysts, difficult product separation, unfriendly environment, etc., and achieve easy regeneration and reuse, environmental friendliness and stability. good effect

Inactive Publication Date: 2006-10-25
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] The technical problem to be solved by the present invention is to provide a preparation method of a supported zirconia catalyst and its application in the synthesis of methyl phenylcarbamate. The preparation method of the supported zirconia catalyst of the present invention is simple, easy to operate, and highly repeatable The supported zirconia catalyst is a heterogeneous catalyst with high activity, which is used for the synthesis of methyl phenylcarbamate by the amination method of dimethyl carbonate, which overcomes the disadvantages that the homogeneous catalyst cannot be recycled and is difficult to separate from the product, and The existing heterogeneous catalysts have the disadvantages of being unfriendly to the environment and having low activity

Method used

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  • Method for preparing load-type zirconium oxide and its using method

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Experimental program
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Effect test

Embodiment 1

[0038] (1) The weight percent content of selected zirconia in the whole catalyst is 5%;

[0039] (2) Weigh 5 grams of SiO 2, use deionized water to determine the volume of solution required for equal-volume impregnation to be 10 milliliters;

[0040] (3) Weigh 0.69 grams of ZrOCl 2 ·8H 2 O was dissolved in 10 ml of deionized water to prepare an impregnating solution;

[0041] (4) Add the impregnation solution prepared in step (3) dropwise to 5 grams of SiO taken by (2) 2 On, equal-volume impregnation for 24 hours, and vacuum-dried the impregnated carrier in a constant temperature water bath at 60°C for 2 hours;

[0042] (5) Calcining the impregnated and dried support obtained in step (4) in an air atmosphere at 500° C. in a muffle furnace for 5 hours to obtain the required supported zirconia catalyst of the present invention.

Embodiment 2

[0044] (1) The weight percent content of selected zirconia in the whole catalyst is 3%;

[0045] (2) Take 5 grams of SiO 2 , use deionized water to determine the volume of solution required for equal-volume impregnation to be 10 milliliters;

[0046] (3) Weigh 2 grams of ZrOCl 2 ·8H 2 O was dissolved in 50 ml of deionized water to prepare an impregnating solution;

[0047] (4) with 5 grams of SiO that (2) step claims 2 Place in the impregnating solution prepared in step (3), heat to 90°C, impregnate excessively for 24 hours, obtain the impregnated carrier by vacuum filtration, and vacuum-dry the impregnated carrier at 60°C for 3 hours;

[0048] (5) Calcining the impregnated and dried support obtained in step (4) in an air atmosphere at 500° C. in a muffle furnace for 5 hours to obtain the required supported zirconia catalyst of the present invention.

Embodiment 3-5

[0050] The preparation method is the same as in Example 1, except that the calcination temperatures in step (5) are changed to 400°C, 600°C, and 700°C, respectively, to prepare the respective required supported zirconia catalysts of the present invention.

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Abstract

The present invention relates to a preparation method of loaded type zirconium oxide catalyst and its application. Its preparation method is characterized by that it utilizes equivoluminal impregnation process or overimpregnation process; the weight percentage content of zirconium oxide in catalyst whole body is 0.1-50%; carrier can be silicon oxide, aluminium oxide, titanium oxide, magnesium oxide, molecular sieve, active carbon or montmorillonite; it uses zirconium oxychloride or zirconyl nitrate to prepare impregnation solution and makes impregnation, then makes drying and roasting processes so as to obtain the invented loaded type zirconium oxide catalyst. Said catalyst can be used in methylcarbonate amine decomposition process process to synthesize methyl carbanilate.

Description

technical field [0001] The technical solution of the present invention relates to a catalyst containing zirconia, in particular to a preparation method of a supported zirconia catalyst and an application method thereof. technical background [0002] Methyl phenylcarbamate (MPC for short) is an intermediate for the synthesis of diphenylmethane diisocyanate (MDI for short). MDI is one of the important raw materials for the synthesis of polyurethane. Its polyurethane products are widely used in electromechanical, shipbuilding, aviation, civil engineering, light In industries such as industry. The synthesis methods of MDI are mainly divided into phosgene method and non-phosgene method, and phosgene method is the main method of industrialization at present. Due to the shortcomings of the phosgene method, such as highly toxic raw materials and by-product hydrochloric acid corrosion of equipment, people have paid more attention to the development of non-phosgene methods in recent ...

Claims

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Application Information

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IPC IPC(8): B01J21/06B01J21/04B01J21/08B01J21/10B01J21/16B01J21/18B01J29/00
Inventor 王延吉李芳苗静赵新强
Owner HEBEI UNIV OF TECH
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