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Preparation method of chitosan/nanometer oxycellulose/nanometer quaternary ammonium salt cellulose ether blended membrane

A nano-oxidation and cellulose ether technology, applied in chemical instruments and methods, alkali metal oxides/hydroxides, water/sludge/sewage treatment, etc., can solve the problems of dissolution, low mechanical strength, and easy adsorption of heavy metal ions Affected by the pH of the water body and other issues, to achieve good adsorption performance and good environmental friendliness

Active Publication Date: 2017-02-15
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, chitosan's mechanical strength is not high, it is easy to dissolve in acidic medium, and the adsorption of heavy metal ions is easily affected by the pH of water, which limits the application of chitosan.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment １

[0031] Embodiment 1: the preparation method of chitosan / nano oxidized cellulose / nano quaternary ammonium cellulose ether blend film, specific operations are as follows:

[0032] (1) Preparation process of nano-oxidized cellulose

[0033] Add 50 mL of 4-amino-2,2,6,6-tetramethylpiperidine-1-oxyl radical containing 17.1 mg (0.1 mmol×171.26 g / mol=17.1 mg) to 1 g of dry microcrystalline cellulose and 102.9mg (1.0mmol×102.89g / mol=102.9mg) of sodium bromide in deionized water, then placed in an ultrasonic water bath at 25°C, stirred evenly, and then added 0.85mL of sodium hypochlorite solution with a concentration of 8% by mass ([(1mmol×74.442g / mol) / (8%×1000)] / 1.10g / mL=0.85mL), and dropwise add 0.1mol / L sodium hydroxide to pH 9.0, turn on the ultrasonic device, adjust to output The power is 300w, the ultrasonic wave acts for 1min every 5min, and oxidizes for 24h; after the reaction is over, the sample is mixed uniformly, centrifuged at 5000rpm for 10min, the upper layer liquid is c...

Embodiment 2

[0041] Embodiment 2: the preparation method of chitosan / nano oxidized cellulose / nano quaternary ammonium salt cellulose ether blend film, concrete operations are as follows:

[0042] (1) Preparation process of nano-oxidized cellulose

[0043] Add 100 mL of 4-amino-2,2,6,6-tetramethylpiperidine-1-oxyl radical containing 85.6 mg (0.5 mmol×171.26 g / mol=85.6 mg) to 1 g of dry microcrystalline cellulose and 514.5mg (5.0mmol×102.89g / mol=514.5mg) of sodium bromide in deionized water, then placed in an ultrasonic water bath at 50°C, stirred evenly, and then added 6.8mL of sodium hypochlorite solution with a concentration of 10% by mass ([(10mmol×74.442g / mol) / (10%×1000)] / 1.10g / mL=6.8mL), and dropwise add 0.5mol / L sodium hydroxide to pH 10.0, turn on the ultrasonic device, adjust to output The power is 900w, the ultrasonic wave is applied for 6 minutes every 15 minutes, and the oxidation is 120 hours; after the reaction is completed, the sample is mixed uniformly, centrifuged at 8000rp...

Embodiment 3

[0051] Embodiment 3: the preparation method of chitosan / nano oxidized cellulose / nano quaternary ammonium salt cellulose ether blend film, concrete operations are as follows:

[0052] (1) Preparation process of nano-oxidized cellulose

[0053] Add 200 mL of 4-amino-2,2,6,6-tetramethylpiperidine-1-oxyl radical containing 171.3 mg (1.00 mmol×171.26 g / mol=171.3 mg) to 1 g of dry microcrystalline cellulose and 1028.9mg (10.0mmol×102.89g / mol=1028.9mg) of sodium bromide in deionized water, then placed in an ultrasonic water bath at 75°C, stirred evenly, and then added 11.3mL of sodium hypochlorite solution with a concentration of 12% by mass ([(20.0mmol×74.442g / mol) / (12%×1000)] / 1.10g / mL=11.3mL), and dropwise add 1.0mol / L sodium hydroxide to pH 11.0, turn on the ultrasonic device, adjust to The output power is 1200w, the ultrasonic wave is applied every 30 minutes for 10 minutes, and the oxidation is 240 hours; after the reaction is completed, the sample is centrifuged at 10,000 rpm ...

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Abstract

The invention discloses a preparation method of a chitosan / nanometer oxycellulose / nanometer quaternary ammonium salt cellulose ether blended membrane capable of adsorbing heavy metal salts. According to the preparation method, chitosan and microcrystalline cellulose are taken as the main raw materials, the ultrasonic wave concerted piperidine nitrogen oxide free radical / cooxidation system method is adopted to realize selective oxidation of microcrystalline cellulose and obtain nanometer oxidized microcrystalline cellulose; and at the same time, a cationic etherifying agent and microcrystalline cellulose are subjected to etherification reaction in ultrasound bath so as to obtain nanometer cationic microcrystalline cellulose ether; the above two nanometer modified cellulose products are mixed with an acetic acid solution, chitosan, and glycerinum, and alkali neutralization, gel forming, and drying are carried out so as to obtain the chitosan / nanometer modified cellulose blended membrane. The chitosan / nanometer oxycellulose / nanometer quaternary ammonium salt cellulose ether blended gel membrane prepared via the preparation method is a transparent sheet, and possesses relatively absorption capacity on heavy metal ions and negative ions such as CuSO4, ZnSO4, Pb(NO3)2, and Fe(NO3)2.

Description

technical field [0001] The invention relates to a preparation technology of a natural polymer adsorption membrane for efficiently treating heavy metal ion waste liquid, and belongs to the technical field of natural polymer modified materials. Background technique [0002] Heavy metal pollution in the water environment means that the heavy metal pollutants discharged into the water body exceed the self-purification capacity of the water body, which changes the composition and properties of the water, thereby deteriorating the growth conditions of organisms in the water environment and causing serious damage to human life and health. bad influence behavior [1] . Every year, my country's petrochemical industry, electronic production, leather manufacturing, electroplating and electrolysis and other industrial production processes will produce a large amount of waste water and waste residue containing heavy metal ions. According to the data from the Ministry of Environmental Pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/26B01J20/28C02F1/28B01J20/30C02F101/20
CPCB01J20/24C02F1/288B01J20/265B01J20/28033C02F2101/20
Inventor 高欣张恒陈克利
Owner KUNMING UNIV OF SCI & TECH
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