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Magnetic hydroximated chitosan and its preparation method

A technology of chitosan and chitosan, applied in the field of magnetic hydroxime chitosan and its preparation, can solve the problems of high toxicity and achieve the effects of low toxicity, high selective adsorption performance and high chemical stability

Inactive Publication Date: 2016-01-27
NANHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Currently reported chitosan derivatives mainly include water-soluble chitosan derivatives, carboxymethyl chitosan derivatives, alkyl chitosan derivatives, etc. hydroxime chitosan derivatives are also reported in literature (Document 3 ,KhaledAiedeh,,MutasemO.Taha:Synthesisofiron‐crosslinkedchitosansuccinateandiron‐crosslinkedhydroxamatedchitosansuccinateandtheirinvitroevaluationaspotentialmatrixmaterialsfororaltheophyllinesustained‐releasebeads,EuropeanJournalofPharmaceuticalSciences,13(2001)159–168;文献4,中南大学丁萍2007年博士学位论文“壳聚糖衍生物与金属配合物及药物 Sustained Release Performance of Preparations"), but the catalyst used in the synthesis process is dicyclohexylcarbodiimide (DCCI), which is insoluble in water and highly toxic, and its application is limited to biomedicine. If it is applied to the field of adsorbent , must consider the follow-up solid-liquid separation problem

Method used

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  • Magnetic hydroximated chitosan and its preparation method
  • Magnetic hydroximated chitosan and its preparation method
  • Magnetic hydroximated chitosan and its preparation method

Examples

Experimental program
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Effect test

Embodiment 1

[0022] Weigh 6.25g of chitosan, dissolve it in 167ml of 1% acetic acid solution, let it stand for more than 12h, then add 10g of dissolved α-ketoglutaric acid, adjust the pH to 4-5, and react in a water bath at 37°C for 4 hours , then add 4.67g of sodium borohydride, adjust the pH to 6.5-7, continue to react for 24 hours, finally add 150ml of 95% ethanol, continue to react for 30 minutes, then filter with suction, wash with anhydrous ether and absolute ethanol for 2-3 times , Soxhlet extraction for 8 hours, dried in a constant temperature drying oven at 45° C., and ground to obtain 14.8 g of carboxylated chitosan.

[0023] Weigh 7.2g of carboxylated chitosan, dissolve it in 200ml of 2% acetic acid solution, add 1ml of N-methylpyrrolidone (NMP), react in a water bath at 37°C for 2 hours, then add 7.2g of hydroxylamine hydrochloride, and further react for 1 hour. Adjust the pH to 9, react for 12 to 24 hours, until the mixture appears white flocculent precipitate in 10ml of conce...

Embodiment 2

[0026] Take 100ml of uranium solution whose mass concentration is 2, 5, 10mg / L respectively, adjust the pH to be 5.0~7.0, temperature 30 ℃, rotating speed 150r / min, take by weighing 0.1g of magnetic hydroximated chitosan prepared in Example 1 , carried out the adsorption test, filtered after 45 minutes, and measured the concentration of residual uranium in the aqueous solution by spectrophotometry, which were 0.026, 0.096, and 0.261 mg / L respectively, and calculated the adsorption rate of uranium by the adsorbent. The adsorption rate of sugar to uranium is over 97%.

Embodiment 3

[0028] Refer to the concentration of various anions and cations in the actual wastewater of uranium mining and metallurgy, prepare 28.6mg / LK + , 82mg / LNH 4 + 、300mg / LCa 2+ , 320mg / LMg 2+ , 26mg / LMn 2+ , 1300mg / LSO 4 2‐ The aqueous solution that coexists with the uranium of 10mg / L, carries out adsorption test by the method in embodiment 2, adopts spectrophotometry to measure residual uranium concentration in the aqueous solution, is respectively 0.403,0.198,0.222,0.473,0.081,0.473mg / L, calculates The adsorption rate of uranium by the adsorbent, the results show that under the condition of the coexistence of the above ions, the adsorption rate of magnetic hydroxime chitosan to uranium is over 95%.

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Abstract

The invention discloses a magnetic hydroxamic chitosan and a preparation method thereof. The preparation method comprises the following steps: introducing carboxyl into a chitosan molecule, converting the carboxyl into a hydroxamic group under the action of a catalyst N-methyl-2-pyrrolidinone (NMP), mixing the hydroxamic group with a prefabricated magnetofluid, and carrying out a cross-linking reaction with glutaraldehyde to obtain the magnetic hydroxamic chitosan. The synthetic magnetic hydroxamic chitosan has an extremely-high performance of selective adsorption on uranium. The synthetic method provided by the invention has the advantages of simplicity in operation, mild reaction conditions and high yield, and the used catalyst has the advantages of low toxicity, high heat stability, high chemical stability and the like. The magnetic hydroxamic chitosan can be used as an adsorbent to be used for radioactive waste water treatment and uranium recovery for uranium mining and metallurgy, and is of an important practical significance for cleaning production of uranium mining and metallurgy and environmental protection.

Description

technical field [0001] The invention belongs to the field of environmental functional materials, and relates to a magnetic hydroxime chitosan used for the selective separation of uranium and a preparation method thereof. Background technique [0002] In the uranium-containing wastewater produced by uranium mines, uranium water smelters and other enterprises involving radioactive substances, the uranium-containing mass concentration is about 5mg / L, which is much higher than the national discharge standard (0.05mg / L). If the wastewater is directly Discharge will seriously pollute the environment (Document 1, Wang Xuegang, Wang Guanghui, Xie Zhiying: Cross-linked chitosan adsorption treatment of low-concentration uranium-containing wastewater, Metal Mines, 9 (2010), 133‐136). At the same time, the direct discharge of uranium-containing wastewater also causes a huge waste of uranium resources. It is estimated that by 2020, China's nuclear power demand for natural uranium will re...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/24B01J20/28B01J20/30G21F9/12
Inventor 王劲松贾亮周洁梁俊邹晓亮陈源波林艳
Owner NANHUA UNIV