A kind of preparation method of bacterial cellulose supported nanometer palladium catalyst

A technology of bacterial cellulose and nano-palladium, which is applied in chemical instruments and methods, preparation of organic compounds, catalysts for physical/chemical processes, etc., can solve the problems of high cost, complicated preparation process, etc. Easy-to-use effects

Active Publication Date: 2011-12-14
NANJING UNIV OF SCI & TECH
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The carrier preparation process used in many loaded palladium catalysts reported before is complicated and expensive, such as the preparation of PADC-Pd catalyst reported in 2006 and its The catalytic performance of the Heck reaction, the carrier used in this article is polyacrylamide (PAAM) undergoes Hofmann degradation reaction to generate intermediate polyvinylamine (PVAm), and PVAm reacts with CS2 at 50°C 36h, finally generate side chain type carbamate chelating resin (PADC)

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  • A kind of preparation method of bacterial cellulose supported nanometer palladium catalyst
  • A kind of preparation method of bacterial cellulose supported nanometer palladium catalyst
  • A kind of preparation method of bacterial cellulose supported nanometer palladium catalyst

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Embodiment 1

[0034] Implementation example 1: the preparation method of bacterial cellulose supported palladium catalyst of the present invention may further comprise the steps:

[0035] In the first step, 0.5% NaOH solution was added to 3 g of wet bacterial cellulose, boiled for 2 hours, then treated with 1.0% acetic acid solution for 50 minutes, and then washed with deionized water until neutral;

[0036] In the second step, the product obtained in the first step is added into 50 mL of ultrapure water, and fully stirred;

[0037] The 3rd step, the 2nd step product is added 0.17g palladium chloride, fully stirs;

[0038] In the fourth step, the system of the third step is ventilated with nitrogen to remove oxygen;

[0039] In the fifth step, the temperature is raised to 135°C, and the reaction is carried out under reflux and nitrogen atmosphere for 6 hours;

[0040] In the sixth step, slowly add 50 mL of 0.035 g / mL potassium borohydride solution to the product in the fifth step;

[004...

Embodiment 2

[0043] Implementation example 2: the preparation method of bacterial cellulose supported nano palladium catalyst of the present invention may further comprise the steps:

[0044] In the first step, add 1.0% NaOH solution to 3 g of wet bacterial cellulose, boil for 1 hour, then treat with 1.5% acetic acid solution for 30 minutes, and finally wash with deionized water until neutral;

[0045] In the second step, the product obtained in the first step is added into 50 mL of ultrapure water, and fully stirred;

[0046] The 3rd step, the 2nd step product is added 0.26g palladium chloride, fully stirs;

[0047] In the fourth step, the system of the third step is ventilated with nitrogen to remove oxygen;

[0048] In the fifth step, the temperature is raised to 140° C., and the reaction is carried out under reflux and nitrogen atmosphere for 5 hours;

[0049] In the sixth step, slowly add 30 mL of 0.040 g / mL potassium borohydride solution to the product in the fifth step;

[0050] ...

Embodiment 3

[0052] Implementation example 3: the preparation method of bacterial cellulose supported palladium catalyst of the present invention may further comprise the steps:

[0053] In the first step, add 2.0% NaOH solution to 3 g of wet bacterial cellulose, boil for 0.5 hours, then treat with 2.0% acetic acid solution for 20 minutes, and then wash with deionized water until neutral;

[0054] In the second step, the product obtained in the first step is added into 50 mL of ultrapure water, and fully stirred;

[0055] The 3rd step, the 2nd step product is added 0.51g palladium chloride, carry out thorough stirring;

[0056] In the fourth step, the system of the third step is ventilated with nitrogen to remove oxygen;

[0057] In the fifth step, the temperature is raised to 145°C, and the reaction is carried out under reflux and nitrogen atmosphere for 5 hours;

[0058] In the sixth step, slowly add 50 mL of 0.045 g / mL potassium borohydride solution to the product in the fifth step; ...

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Abstract

The invention discloses a method for preparing a bacterial cellulose loaded nanometer palladium catalyst. The method comprises the following steps of: pretreating bacterial cellulose, stirring the pretreated bacterial cellulose in ultrapure water, and dispersing; adding palladium chloride or palladium nitrate, dispersing fully, removing oxygen, and heating; adding potassium borohydride solution; and after reaction is finished, blanching and centrifugal separation repeatedly to obtain the bacterial cellulose loaded nanometer palladium catalyst. In the method, divalent potassium ions are reduced by using the potassium borohydride solution under the hydrothermal condition to form the zero-valent palladium catalyst with small grain diameters and uniform distribution; and the preparation process is simple, the prepared catalyst is high in catalytic efficiency, and the method can be applied in the fields of organic synthesis and the like.

Description

technical field [0001] The invention belongs to the technical field of depositing nanoparticles on the surface of nanofibers, in particular to a method for preparing palladium supported on bacterial cellulose. Background technique [0002] Bacterial cellulose (BC) is one of the hot spots in the research of biomaterials at home and abroad. It is a kind of polymer compound produced by some bacteria. It was first discovered by British scientist Brown in 1886. Bacterial cellulose fibers are composed of microfibrils with a diameter of 3-4 nm to form 40-60 nm thick fiber bundles, and interweave to form a developed ultra-fine network structure. The elastic modulus of bacterial cellulose is several times to that of ordinary plant fibers. More than ten times, it has a strong water holding capacity, and has high biocompatibility, adaptability and good biodegradability. [0003] Transition metal-catalyzed cross-coupling reaction is an effective method widely used in organic synthesis,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/06B01J23/44C07C67/343C07C69/618C07C15/52C07C2/88
Inventor 唐卫华唐键周培培王欢欢孙东平
Owner NANJING UNIV OF SCI & TECH
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