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Coprecipitation Cd/Al (Cadmium / Aluminum) catalyst and application of catalyst for catalyzing and synthesizing 2,6-naphthalenedicarboxylic acid

A naphthalene dicarboxylic acid and co-precipitation technology, which is applied in the direction of physical/chemical process catalysts, carboxylate preparation, chemical instruments and methods, etc., can solve the problems of low catalytic activity and small specific surface area, and achieve high natural purity and specific surface area. The effect of large surface area and low production cost

Inactive Publication Date: 2011-06-15
WENZHOU UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The first technical problem to be solved by the present invention is to overcome the defects of small specific surface area and low catalytic activity of general cadmium-based catalysts, and provide a new type of co-precipitated Cd / Al catalyst

Method used

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  • Coprecipitation Cd/Al (Cadmium / Aluminum) catalyst and application of catalyst for catalyzing and synthesizing 2,6-naphthalenedicarboxylic acid
  • Coprecipitation Cd/Al (Cadmium / Aluminum) catalyst and application of catalyst for catalyzing and synthesizing 2,6-naphthalenedicarboxylic acid
  • Coprecipitation Cd/Al (Cadmium / Aluminum) catalyst and application of catalyst for catalyzing and synthesizing 2,6-naphthalenedicarboxylic acid

Examples

Experimental program
Comparison scheme
Effect test

experiment example 1

[0033] At 80°C, add dropwise a mixed solution of 300 mL of 0.8 mol / L cadmium nitrate aqueous solution and 0.8 mol / L aluminum nitrate aqueous solution in 200 mL of 1.0 mol / L sodium carbonate aqueous solution (wherein the cadmium nitrate aqueous solution and the aluminum nitrate aqueous solution The volume ratio is 19:1), stir quickly, add dropwise to pH = 4, then back drop sodium carbonate solution to pH = 9, and age at 80°C for 30min, filter, wash, dry the filter residue at 120°C for 12h, cool to room temperature, then raised from room temperature to 500 °C at 2 °C / min, after calcination for 3 hours, cooled naturally to room temperature, taken out and kept dry. Obtain coprecipitation Cd / Al=95 / 5 catalyzer 26.3g at last, do XRD characterization to the catalyzer after drying, the peak position that obtains is consistent with the peak position of standard cadmium oxide, aluminum oxide (see attachment figure 1 ).

experiment example 2

[0035] At 80°C, add dropwise a mixed solution of 300 mL of 0.8 mol / L cadmium nitrate aqueous solution and 0.8 mol / L aluminum nitrate aqueous solution in 200 mL of 1.0 mol / L sodium carbonate aqueous solution (wherein the cadmium nitrate aqueous solution and the aluminum nitrate aqueous solution The volume ratio is 7:3), stirring quickly, adding dropwise to pH=4, then back-dropping 1.0mol / L sodium carbonate solution to pH=9, aging at 80°C for 30min, filtering, washing, and filtering the filter residue at 120 Dry at ℃ for 12 hours, cool to room temperature, then raise from room temperature to 550℃ at 2℃ / min, after calcining for 3h, cool to room temperature naturally, take it out and keep it dry. Finally, 18.5 g of the co-precipitated Cd / Al=70 / 30 catalyst was obtained, and XRD was performed on the dried catalyst, and the peak positions obtained were consistent with those of standard cadmium oxide and aluminum oxide.

experiment example 3

[0037]At 80°C, add dropwise a mixed solution of 300 mL of 0.8 mol / L cadmium nitrate aqueous solution and 0.8 mol / L aluminum nitrate aqueous solution in 200 mL of 1.0 mol / L sodium carbonate aqueous solution (wherein the cadmium nitrate aqueous solution and the aluminum nitrate aqueous solution The volume ratio is 19:1), stir quickly, add dropwise to pH = 4, then back drop sodium carbonate solution to pH = 9, and age at 80°C for 30min, filter, wash, dry the filter residue at 120°C for 12h, cool to room temperature, and then raised from room temperature to 650 °C at 2 °C / min, after calcination for 3 hours, naturally cooled to room temperature, taken out and kept dry. Finally, 25.5 g of the co-precipitated Cd / Al=95 / 5 catalyst was obtained, and XRD was performed on the dried catalyst, and the peak positions obtained were consistent with those of standard cadmium oxide and aluminum oxide.

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Abstract

The invention discloses a coprecipitation Cd / Al (Cadmium / Aluminum) catalyst which is prepared by the following steps of: under 80 DEG C, dripping mixed solution which is mixed by cadmium nitrate water solution and aluminum nitrate water solution in sodium carbonate water solution, dripping until the pH value is 3.5-4.5; then dripping the sodium carbonate water solution until the pH is 8.5-9.5, standing under 70-80 DEG C, filtering, washing, drying, heating up to 400-650 at the speed of 2 DEG C / min to calcine, and cooling to obtain the coprecipitation Cd / Al catalyst. The invention further discloses the application of the catalyst for catalyzing and synthesizing 2,6-naphthalenedicarboxylic acid. The Cd / Al catalyst disclosed by the invention is large in specific surface area, excellent in catalyzing effect and simple in preparation, wherein Al element and Cd element are both doped so as to improve the catalytic activity of the catalyst. The method for synthesizing the 2,6-naphthalenedicarboxylic acid by the coprecipitation Cd / Al catalyst can obtain the product by one step; and the product is high in purity, high in productive rate and simple in process route.

Description

(1) Technical field [0001] The invention relates to a co-precipitated Cd / Al catalyst and its application in catalytically synthesizing 2,6-naphthalene dicarboxylic acid. (2) Background technology [0002] 2,6-Naphthalene dicarboxylic acid and its derivatives are important monomers for the preparation of various polyesters, polyurethane materials and liquid crystal polyester resins. [0003] There are many kinds of synthetic methods for 2,6-naphthalene dicarboxylic acid, (1) Heinkel method, including disproportionation method and isomerization method; (2) 2,6-dialkylnaphthalene oxidation method (alkyl can be methyl, ethyl and isopropyl, etc.), wherein the oxidation of 2,6-diisopropylnaphthalene to prepare 2,6-naphthalene dicarboxylic acid is the most common, and the reaction of this method to synthesize 2,6-naphthalene dicarboxylic acid is Liquid-phase exothermic reaction, using Co-Mn-Br catalyst system, with C 2 ~C 6 The organic acid is the solvent, the reaction temperatu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/06B01J35/10C07C63/38C07C51/02
Inventor 唐天地吴国强乔迁赵倩文王如国
Owner WENZHOU UNIVERSITY
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