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Microwave assisted method for synthesizing polysaccharide monohydrate selenium dioxide ester

A technology for synthesizing selenite and polysaccharide, which is applied in the field of microwave-assisted synthesis and achieves the effects of short reaction time, controllable reaction conditions and low pollution

Active Publication Date: 2009-08-12
NORTHWEST NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Patent CN1281629C discloses selenic acid polysaccharide and its preparation method. This method is to first synthesize selenous acid, then reduce selenous acid to selenic acid, and then introduce selenate into polysaccharide; patent CN1560088A discloses a selenized glucomannan The preparation method of making a Se 6+ Reaction solution, add glucomannan in selenization reaction solution, make selenide mannan; Patent CN1284509A discloses chitosan selenite and preparation method thereof, and this method is to use the amine group of chitosan and Selenous acid is reacted; domestic and foreign patents all do not relate to the method for synthesizing Bracken polysaccharide and Artemisia polysaccharide selenite with microwave-assisted conditions

Method used

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  • Microwave assisted method for synthesizing polysaccharide monohydrate selenium dioxide ester
  • Microwave assisted method for synthesizing polysaccharide monohydrate selenium dioxide ester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] The preparation method of a kind of fern polysaccharide selenite product of the present invention comprises the following steps:

[0022] (1) select the fern polysaccharide as raw material;

[0023] (2) Weighing 0.5g of P. japonica polysaccharide with a purity of more than 90% and adding it to a 250ml three-necked flask, adding 100ml of 1.2% nitric acid solution at a concentration of 1.2% by weight, stirring on a magnetic stirrer at room temperature for 10min, and standing for 12 hours. Obtain the Junaca polysaccharide suspension A;

[0024] (3) Put the Juna polysaccharide suspension A in a microwave reactor, add 1.65g of barium chloride and 0.5g of selenous acid into a three-necked flask, raise the temperature to 70°C, and set the microwave power at 300W and the frequency at 2450MHz The reaction was carried out for 0.5h, and after cooling to room temperature, a suspension B was obtained;

[0025](4) After the suspension B was filtered under reduced pressure at 0.06Mp...

Embodiment 2

[0028] The preparation method of a kind of fern polysaccharide selenite product of the present invention comprises the following steps:

[0029] (1) select the fern polysaccharide as raw material;

[0030] (2) Weighing 0.4g of the polysaccharides of Zernia japonica with a purity of more than 90% and adding it to a 250ml three-necked flask, adding 100ml of 0.6% nitric acid solution at a concentration of 0.6% by weight, stirring for 15min on a magnetic stirrer at room temperature, and standing for 15 hours, Obtain the Junaca polysaccharide suspension A;

[0031] (3) Put the suspension A of the fern polysaccharides in a microwave reactor, add 1.65g of barium chloride and 0.8g of selenous acid into a three-necked flask, heat up to 60°C, and react at a microwave power of 200W and a frequency of 2450MHz After 1.5h, after cooling to room temperature, suspension B was obtained;

[0032] (4) After the suspension B was filtered under reduced pressure at 0.07Mpa, 26ml of 3.0mol / L sulfu...

Embodiment 3

[0035] The preparation method of a kind of fern polysaccharide selenite product of the present invention comprises the following steps:

[0036] (1) select the fern polysaccharide as raw material;

[0037] (2) Weighing 1.0g of P. japonicus polysaccharide with a purity of more than 90% is added to a 250ml three-necked flask, and the concentration by weight is 100ml of 0.8% nitric acid solution, stirred on a magnetic stirrer at room temperature for 20min, and left to stand for 18 hours. Obtain the Junaca polysaccharide suspension A;

[0038] (3) Put the suspension A of the fern polysaccharide in a microwave reactor, add 1.65g of barium chloride and 2.0g of selenous acid into a three-necked flask, heat up to 45°C, and react at a microwave power of 100W and a frequency of 2450MHz 4h, after cooling to room temperature, suspension B was obtained;

[0039] (4) After the suspension B was filtered under reduced pressure at 0.08Mpa, 30ml of 3.0mol / L sulfuric acid was added to the filt...

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Abstract

The invention relates to a method for synthesizing polysaccharide selenious acid ester by microwave assistance, which comprises the following steps of adding potentilla anserina polysaccharide or sand sagebrush polysaccharide with the purity of more than 90 percent into a vessel, adding saltpeter solution, stirring at the room temperature and setting aside overnight to obtain potentilla anserina polysaccharide or sand sagebrush polysaccharide suspension liquid A; putting the suspension liquid A into a microwave reaction instrument, adding barium chloride and selenious acid, heating up and reacting for 0.5-4h under the microwave condition and cooling to the room temperature to obtain suspension liquid B; decompressing and filtering the suspension liquid B, adding sulphuric acid in the filtrate to generate white precipitate, removing the white precipitate and regulating pH of supernatant fluid by sodium hydroxide to obtain a matter C; putting the matter C in a dialyzing bag to be dialyzed, decompressing and concentrating the solution in the dialyzing bag after the solution is detected to have no red by ascorbic acid solution, adding ethanol, precipitating, setting aside, centrifugating, collecting precipitate at the lower layer, freezing and drying to obtain potentilla anserina polysaccharide selenious acid ester or sand sagebrush polysaccharide selenious acid ester. The invention has the advantages of controllable reaction conditions, good repeatability, short reaction time consumption and low energy consumption.

Description

technical field [0001] The invention relates to a microwave-assisted synthesis method, in particular to a method for microwave-assisted synthesis of polysaccharide selenite by using artemisia polysaccharides or pterophyll polysaccharides as raw materials. Background technique [0002] As a selenium source, selenium polysaccharides have the characteristics of high absorption rate and biological activity, low toxicity, and low environmental pollution compared with inorganic selenium. It is a hot spot in selenium chemistry research. As an organic selenium compound, selenium polysaccharides maintain the basic configuration and physiological functions of polysaccharides, while effectively improving the bioavailability of selenium and its physiological function as an essential trace element for biology. The toxicity and side effects are greatly reduced compared with inorganic selenium. Studies have proved that selenium polysaccharides have significant biological activities such as...

Claims

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Application Information

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IPC IPC(8): C08B37/00
Inventor 张继赵保堂王俊龙王小芳王云普姚健梁俊玉马君义赵美荣许乐王邦
Owner NORTHWEST NORMAL UNIVERSITY
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