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Preparation and application of marine biological waste oyster shell-supported palladium catalyst

A technology of a palladium catalyst and an oyster shell is applied in the preparation of heterogeneous palladium catalysts and the field of preparation of marine biomass-supported palladium catalysts, and can solve the problems of environmental pollution, high price of homogeneous palladium catalysts, etc., and achieves a wide range of materials and simple processes. Effect

Active Publication Date: 2020-02-04
GUANGDONG OCEAN UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The purpose of the present invention is to provide a kind of modified marine biomass for the problems that the homogeneous palladium catalyst is expensive, it is difficult to separate, recover and recycle from the reaction system under the condition of homogeneous catalysis, and the environment is seriously polluted after the reaction. The preparation method of carrier material supporting transition metal palladium, the obtained heterogeneous palladium catalyst can efficiently (more than 90%) catalyze the Heck reaction of aryl halides such as iodobenzene and bromobenzene and alkenes, and after the catalyst is reused 6 times, there is almost no activity decline, the product yield is still above 90%, and it is found that it also has excellent catalytic ability for Sonogashira coupling

Method used

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  • Preparation and application of marine biological waste oyster shell-supported palladium catalyst
  • Preparation and application of marine biological waste oyster shell-supported palladium catalyst
  • Preparation and application of marine biological waste oyster shell-supported palladium catalyst

Examples

Experimental program
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Effect test

Embodiment 1

[0047] Step 1: Preparation of nano-hydroxyapatite (HAP)

[0048] (1) Fresh oyster shells are cleaned and air-dried naturally, add an appropriate amount of 10% sodium hydroxide solution, and heat at 95°C for 5 hours to fully remove protein;

[0049] (2) Take out the oyster shell, rinse it repeatedly with water, dry it at 100°C, crush it, and pass it through a 100-mesh sieve; the obtained powder is dried at 70-100°C for 24 hours;

[0050] (3) Take oyster shells, (NH4)2HPO4, and cetyltrimethylammonium bromide and add them to the inner tank of the reactor (Ca / P molar ratio n(CaCO3):n((NH4)2HPO4) is 5:6) , adding an appropriate amount of deionized water, adjusting the pH to 6 with phosphoric acid, stirring magnetically at room temperature for 1 hour, sealing the reaction vessel, and stirring and reacting at 140°C for 24 hours;

[0051] (4) After the reaction kettle is cooled to room temperature, centrifuge to obtain a precipitate, and centrifuge and wash the precipitate with deion...

Embodiment 2

[0066] Step 1: Preparation of nano-hydroxyapatite (HAP)

[0067] (1) Fresh oyster shells are cleaned and air-dried naturally, soaked in 5% sodium hypochlorite solution for 1 day to remove protein;

[0068] (2) Take out the oyster shell, rinse it repeatedly with water, dry it at 100°C, crush it, and pass it through a 100-mesh sieve; the obtained powder is dried at 70-100°C for 24 hours;

[0069] (3) Add oyster shells, (NH4)2HPO4, and cetyltrimethylammonium bromide to the inner tank of the reactor (Ca / P molar ratio n(CaCO3):n((NH4)2HPO4) is 1:1) , adding an appropriate amount of deionized water, adjusting the pH to 6 with phosphoric acid, stirring magnetically at room temperature for 1 hour, sealing the reaction vessel, and stirring and reacting at 140°C for 24 hours;

[0070] (4) After the reaction kettle is cooled to room temperature, centrifuge to obtain a precipitate, and centrifuge and wash the precipitate with deionized water for 3 to 6 times until no carbonate ion is det...

Embodiment 3

[0084] Step 1: Preparation of nano-hydroxyapatite (HAP)

[0085] (1) Fresh oyster shells are cleaned and air-dried naturally, add an appropriate amount of 10% sodium hydroxide solution, and heat at 95°C for 5 hours to fully remove protein;

[0086] (2) Take out the oyster shell, rinse it repeatedly with water, dry it at 100°C, crush it, and pass it through a 100-mesh sieve; the obtained powder is dried at 70-100°C for 24 hours;

[0087](3) Take oyster shells, (NH4)2HPO4, and cetyltrimethylammonium bromide and add them to the inner tank of the reactor (Ca / P molar ratio n(CaCO3):n((NH4)2HPO4) is 5:6) , adding an appropriate amount of deionized water, adjusting the pH to 6 with phosphoric acid, stirring magnetically at room temperature for 1 hour, sealing the reaction vessel, and stirring and reacting at 140°C for 24 hours;

[0088] (4) After the reaction kettle is cooled to room temperature, centrifuge to obtain a precipitate, and centrifuge and wash the precipitate with deioni...

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Abstract

The invention discloses preparation and application of a marine biological waste oyster shell-supported palladium catalyst. Oyster shells are used as calcium, cetyltrimethylammonium bromide is used asa porogen to synthesize hydroxyapatite by a hydrothermal method, and a heterogeneous palladium catalyst which can be recycled is prepared. The preparation of the marine biological waste oyster shell-supported palladium catalyst has the following advantages that (1) the oyster shells and phosphate are used as raw materials, the oyster shells and the phosphate are low in cost, easy to obtain, widely available and environmentally friendly, and the process is simple; (2) a Heck reaction of aryl halides such as iodobenzene and bromobenzene with olefin can be can efficiently (90% or above) catalyzed, after repeated six-time use of the catalyst, the activity is almost not reduced, and the product yield is still 90% or above; (3) excellent catalytic ability is achieved on Sonogashira coupling; and (4) compared with other carrier materials, hydroxyapatite carrier materials have the significant advantages that good chemical stability, thermal stability, low solubility and adjustable surface acid and base are achieved, the structure is easy to modify, and ion exchangeability is high.

Description

technical field [0001] The invention relates to a preparation method of a heterogeneous palladium catalyst, in particular to a preparation method of a marine biomass-supported palladium catalyst, and belongs to the technical field of green chemical synthesis. Background technique [0002] With the development of society, people pay more and more attention to physical health and environmental issues. The impact of chemical reactions on the environment cannot be ignored, and the concept of green chemistry came into being. Green chemistry advocates making full use of every atom in the process of obtaining new substances through chemical conversion, which has "atom economy". The goal of green chemistry requires that any chemical activity, including chemical raw materials used, chemical and chemical processes, and final products, should be beneficial to human health and the environment. Therefore, the research results of green chemistry are of fundamental significance for solvi...

Claims

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Application Information

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IPC IPC(8): B01J27/185C07C231/12C07C233/11
CPCB01J27/1856C07C231/12C07C233/11Y02P20/584
Inventor 温燕梅康信煌洪鹏志许晓玲杨俊杰
Owner GUANGDONG OCEAN UNIVERSITY
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