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Di-amidoxime group containing modified silica gel adsorbent and preparation method thereof

A bisamidoxime and silica gel adsorption technology, which is applied in chemical instruments and methods, adsorption water/sewage treatment, and other chemical processes, can solve problems such as difficult separation, low grafting degree, and insufficient specific surface area, and achieve Improved adsorption performance, high mechanical strength, and good regeneration performance

Inactive Publication Date: 2013-07-31
HOHAI UNIV
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Problems solved by technology

But there are still the following deficiencies: ①The adsorption equilibrium time is long; ②The adsorption effect on low-concentration heavy metals is not good; ③The grafting degree is not high
Chinese patent CN101596449A, a method for preparing an amidoxime-based uranium-extracting adsorbent, in which acrylonitrile powder and titanium dioxide prepared from sol-gel are blended and oximated to obtain a hybrid amidoxime-based uranium-extracting material, but still There are following deficiencies: 1. the mechanical strength of the obtained material is not enough; 2. the adsorption capacity of the material to uranium is not high; Chinese patent CN101357325A, a kind of spherical cellulose chelating adsorbent containing amidoxime group and carboxyl group and its preparation method, the The patent utilizes graft copolymerization of acrylonitrile and cellulose, followed by saponification and oximation to produce a spherical cellulose chelating adsorption material containing amidoxime groups and carboxyl groups, but there are still the following deficiencies: ①The degree of grafting is not high ; ② The adsorption selectivity of the material is not high; ③ The specific surface area of ​​the material is not large enough, resulting in poor adsorption effect
Chinese patent CN101954268A, a method for preparing an adsorbent for heavy metal ions in water. This patent utilizes a mercapto compound to modify nano-titanium dioxide to obtain a nano-titanium dioxide adsorption material containing a mercapto group. However, the following disadvantages still exist: the nano-scale adsorption material is not easy Separation may cause secondary pollution
Tao Tingxian et al. published in "Chemical Research and Application", 2003, 6: 823-825 "Adsorption Kinetics of Amidoxime-based Fibers to Copper (II)" mentioned in the article that amidoxime-based fibers are to copper ions The adsorption capacity is 9.8mg / g, but there are still some deficiencies such as low adsorption capacity for copper ions

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  • Di-amidoxime group containing modified silica gel adsorbent and preparation method thereof
  • Di-amidoxime group containing modified silica gel adsorbent and preparation method thereof
  • Di-amidoxime group containing modified silica gel adsorbent and preparation method thereof

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preparation example Construction

[0032] combine figure 1 , a kind of preparation method that the present invention proposes containing the modified silica gel adsorbent of bisamidoxime group, comprises the following steps:

[0033] Step 1, activation: put 30g of 100-200 mesh column chromatography silica gel in 150mL of 5% methanesulfonic acid solution, reflux at 90°C and keep stirring for 4 hours. After the reaction is completed, rinse with distilled water repeatedly Until the washing liquid is neutral, dry it under vacuum at 50°C for 24 hours;

[0034] Step 2, impregnation: Add 10g of the activated silica gel obtained in Step 1 into 150mL of KH550 in toluene solution, where the volume concentration of KH550 is 10%, reflux at 70°C and keep stirring for 24 hours, filter to get coarse particles, and then use Extract with toluene in a Soxhlet extractor for 24 hours to remove unreacted KH550 on the surface of silica gel to obtain impregnated particles;

[0035] Step 3, drying: vacuum-dry the impregnated granul...

Embodiment 1

[0041] Step 1, activation: put 30g of 100-200 mesh column chromatography silica gel in 150mL of 5% methanesulfonic acid solution, reflux at 90°C and keep stirring for 4 hours. After the reaction is completed, rinse with distilled water repeatedly Until the washing liquid is neutral, dry it under vacuum at 50°C for 24 hours;

[0042] Step 2, impregnation: Add 10g of the activated silica gel obtained in Step 1 into 150mL of KH550 in toluene solution, where the volume concentration of KH550 is 10%, reflux at 70°C and keep stirring for 24 hours, filter to get coarse particles, and then use Extract with toluene in a Soxhlet extractor for 24 hours to remove unreacted KH550 on the surface of silica gel to obtain impregnated particles;

[0043] Step 3, drying: vacuum-dry the impregnated granules obtained in Step 2 at 50° C. for 24 hours to obtain dry granules;

[0044] Step four, modification:

[0045] (1) Add 5g of the dried granules obtained in Step 3 to 100mL of acrylonitrile in ...

Embodiment 2

[0049] Repeat steps one to three in Example 1

[0050] Step four, modification:

[0051] (1) Add 5g of the dried granules obtained in step 3 to 100mL of acrylonitrile in N,N-dimethylformamide (DMF) solution, where the volume concentration of acrylonitrile is 15%, and then blow nitrogen into the bottle to remove Then add 0.1g initiator azobisisobutyronitrile, condense and reflux at 75°C and continue to stir for 5 hours. The agent was extracted in a Soxhlet extractor for 24 hours to remove unreacted acrylonitrile on the surface of the silica gel to obtain impregnated primary modified particles, and vacuum dried at 50°C for 24 hours to obtain dried primary modified particles;

[0052] (2) Mix 20mL of hydroxylamine hydrochloride solution with a concentration of 1mol / L and 20mL of sodium carbonate solution with a concentration of 1mol / L, then add 1g of the modified particles obtained in step 4 (1), and then blow in nitrogen, Remove the air in the bottle, reflux at 70°C and contin...

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Abstract

Belonging to the field of modified silica gel adsorbents, the invention particularly relates to a di-amidoxime group containing modified silica gel adsorbent specific to heavy metal copper ions in an adsorption solution and a preparation method thereof. The preparation method includes: taking silica gel as a starting raw material, conducting activation by a methanesulfonic acid solution, performing impregnation in a toluene solution of KH550, carrying out drying, then adding the obtained dry particles into an N, N-dimethylformamide solution of acrylonitrile to undergo first modification, and carrying out a treatment, then adding the dried first modified particles into a mixed solution of a hydroxylamine hydrochloride solution and a sodium carbonate solution to perform second modification, and conducting a treatment, thus obtaining dried second modified particles, i.e. a di-amidoxime group containing modified silica gel adsorbent finished product. The di-amidoxime group involved in the invention can be chelated with a heavy metal, thus having a strong adsorption effect on heavy metal copper ions. And compared with single-oxime group adsorbents, the di-amidoxime group containing modified silica gel adsorbent disclosed in the invention has substantially improved adsorption performance on copper ions, and the adsorption capacity is increased to 30mg / g.

Description

technical field [0001] The invention belongs to the field of modified silica gel adsorbents, in particular to a modified silica gel adsorbent containing bisamidoxime groups for the adsorption of heavy metal copper ions in solution and a preparation method thereof. [0002] Background technique [0003] As we all know, with the rapid development of my country's national economy, environmental pollution and its derivative economic and social problems are becoming increasingly apparent. The protection, deterioration and treatment of the water environment have attracted more and more attention from all walks of life, especially the treatment of heavy metal polluted water bodies. The research and development of practical new treatment technologies is of great theoretical and practical significance to water resource protection, human life and health, and sustainable economic and social development. [0004] Among many heavy metal water treatment technologies, the adsorption and ...

Claims

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Application Information

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IPC IPC(8): B01J20/22B01J20/30C02F1/28C02F1/62
Inventor 杨汉培俞咪虹吴莎傅小飞张颖超宋双双胡怀金
Owner HOHAI UNIV
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