CN107376872B - Preparation method of chitosan-soybean protein composite porous microspheres for lead adsorption - Google Patents
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Abstract
The invention discloses a preparation method of chitosan-soybean protein composite porous microspheres for lead adsorption. The chitosan-soybean protein composite porous microspheres are prepared by taking soybean protein and chitosan as raw materials and crosslinking through glutaraldehyde, and are taken as adsorbing materials to carry out micro-column adsorption on lead in a solution, and the adsorption capacity of the chitosan-soybean protein composite porous microspheres on the lead is 42.8 mg/g. The invention overcomes the defects of complex preparation and high price of the existing material, and the defects of complex static adsorption operation, complex steps and the like, reduces the material preparation cost, reduces the manual operation steps, simplifies the operation flow and improves the lead adsorption efficiency.
Description
Technical Field
The invention relates to a preparation method of chitosan-soybean protein composite porous microspheres for lead adsorption.
Background
With the development of global industry, lead pollution has caused great threat to the environment and human health, and the research and development of a rapid and convenient lead adsorption material is urgently needed to meet the requirements of environmental detection and the like.
At present, methods for separating and enriching cadmium in water include precipitation, ion exchange, adsorption and the like. Among them, the adsorption method is widely used because it is simple and efficient and the adsorbent can be recycled.
At present, the preparation of the chitosan-soy protein composite porous microspheres for lead adsorption has not been researched.
Disclosure of Invention
The invention provides a preparation method of chitosan-soybean protein composite porous microspheres for lead adsorption.
The concept is as follows: although various adsorbing materials are used for adsorbing lead at present, the preparation is complicated and the cost is high. The soybean protein has abundant amide groups in the molecular structure, and the chitosan molecule contains a large amount of amino groups, so that the adsorption material prepared from the soybean protein and the chitosan has low price and is used for adsorbing lead, the material is simple to prepare, and the material has practical application value. In the experiment, the chitosan-soybean protein composite porous microspheres are used as the micro-column adsorption material to dynamically adsorb and separate lead in a sample solution, so that manual operation is reduced, and the operation process is simplified.
The invention relates to chitosan-soy protein composite porous microspheres and dynamic microcolumn adsorption of lead. When lead in a sample solution passes through a microcolumn loaded with chitosan-soybean protein composite porous microspheres, the lead is adsorbed by the action of groups on a microsphere material, then the lead is eluted by eluent and subjected to atomic absorption spectrometry, and the adsorption capacity of the material on the lead is tested.
The method comprises the following specific steps:
(1) preparing chitosan-soybean protein composite porous microspheres:
weighing 4g of chitosan, putting the chitosan into a 100mL beaker, adding 50mL of 2% acetic acid solution by mass, stirring for dissolving, standing for 12 hours, and removing bubbles in the solution to obtain a chitosan solution for later use; adding 2.0g of soybean protein and 40mL of secondary water into a 100mL beaker, and stirring until the soybean protein is completely dissolved to obtain a soybean protein solution for later use; and mixing 40mL of the chitosan solution and 40mL of the soybean protein solution, adding 2.0g of nano-silica, and uniformly stirring to obtain a chitosan-soybean protein-silica mixed solution for later use.
Taking 140mL of liquid paraffin into a 250mL three-neck flask, dropwise adding 4 drops of analytically pure active agent span 80, mechanically stirring (300r/min) for 30 minutes, heating the liquid paraffin to 60 ℃ in a water bath, dropwise adding 60mL of chitosan-soybean protein-silicon dioxide mixed solution into the three-neck flask, continuously stirring for two hours until uniform oil bead particles are formed, then adjusting the pH of the mixed solution to 9.5 by using analytically pure sodium hydroxide solution, heating the water bath to 90 ℃, then adding 20mL of analytically pure glutaraldehyde solution, reacting for 3 hours, standing, cooling, filtering to obtain solid microsphere particles, alternately cleaning each of the solid microsphere particles by using water and absolute ethyl alcohol for 3-5 times, and extracting for 24 hours by using ethyl alcohol with the mass percentage concentration of 95% in a Soxhlet extractor; soaking the solid microsphere particles in 5.0mol/L sodium hydroxide solution for 24 hours, washing with secondary water to be neutral, filtering, drying at 40 ℃, and sieving to obtain the chitosan-soybean protein composite porous microspheres with the particle size of 40-60 meshes.
(2) Adsorbing lead by using the chitosan-soybean protein composite porous microspheres:
the separation and enrichment device comprises a peristaltic pump, a self-made mini column ((7cm multiplied by 0.5mm i.d.), a polytetrafluoroethylene tube (0.8mm i.d.) and a connecting joint, wherein a small amount of glass wool is plugged at one end of the mini column, the crosslinked soybean protein microspheres prepared in the step (1) are filled in the mini column by a wet method, then a small amount of glass wool is plugged in the mini column, the mini column is compacted and connected, secondary distilled water is pumped into the mini column by the peristaltic pump, and the mini column is washed for standby application, the separation and enrichment step of Pb (II) comprises the steps of enabling a Pb (II) solution with the pH of 5.0 to pass through the mini column at the flow rate of 3.0mL/min, then washing the unadsorbed ions in the mini column by 5.0mL of distilled water at the flow rate of 3.0mL/min, and using 10.0mL of HNO with the concentration of 0.3Reversely eluting the adsorbed Pb (II) at the flow rate of 3.6 mL/min; the elution solution was used for subsequent atomic absorption spectroscopy.
(3) The detection method comprises the following steps:
the measuring instrument: atomic absorption spectrophotometer (beijing general analytical instruments ltd); the instrument conditions for measuring Pb by graphite furnace atomic absorption spectrometry are as follows: the wavelength is 283.3nm, the slit is 0.5nm, the lamp current is 2.0mA, and the height of the atomizer is-0.2 mm; the procedure for measuring atomic absorption spectroscopy in a graphite furnace is shown in Table 1. And (3) measuring the concentration of Pb (II) in the eluent obtained in the step (2) by utilizing graphite furnace atomic absorption spectrometry.
Table 1: graphite furnace atomic absorption spectrometry program
| Procedure for measuring the movement of a moving object | Temperature (. degree.C.) | Temperature rise rate (DEG C/s) | Retention time(s) |
| Drying | 80 | 5 | 5 |
| Drying | 100 | 10 | 10 |
| Ashing | 600 | 10 | 10 |
| Atomization of | 1900 | 0 | 4 |
| Purification | 1950 | 1 | 1 |
(4) The adsorption capacity of the chitosan-soybean protein composite porous microspheres to lead is determined:
conditions for flame atomic absorption spectrometry determination of lead: the wavelength is 283.3nm, the slit is 0.5nm, the lamp current is 2.0mA, the height of the burner is 5.0mm, the acetylene flow is 1500mL/min, and the air flow is 5000 mL/min. Adsorbing 20.0 mu g/mL of Pb (II) solution according to the step (2), collecting effluent every 10mL, stopping the experiment until the concentration of lead in the effluent is the same as the original solution concentration, measuring the concentration of Pb (II) in each effluent by using a flame atomic absorption spectrometry, and calculating the adsorption capacity of the chitosan-soybean protein composite porous microspheres on lead.
The invention overcomes the defects of complex preparation and high price of the existing material, and the defects of complex static adsorption operation, complex steps and the like, reduces the material preparation cost, reduces the manual operation steps, simplifies the operation flow and improves the lead adsorption efficiency.
Drawings
Fig. 1 is a scanning electron microscope photograph of chitosan-soy protein composite porous microspheres prepared in the example of the present invention.
Detailed Description
Example (b):
(1) preparing chitosan-soybean protein composite porous microspheres:
weighing 4g of chitosan in a 100mL beaker, adding 50mL of 2% acetic acid solution by mass, stirring to dissolve, standing for 12 hours, and removing bubbles in the solution to obtain a chitosan solution for later use. Adding 2.0g of soybean protein and 40mL of secondary water into a 100mL beaker, and stirring until the soybean protein is completely dissolved to obtain a soybean protein solution for later use; and mixing 40mL of the chitosan solution and 40mL of the soybean protein solution, adding 2.0g of nano-silica, and uniformly stirring to obtain a chitosan-soybean protein-silica mixed solution for later use.
Taking 140mL of liquid paraffin into a 250mL three-neck flask, dropwise adding 4 drops of analytically pure active agent span 80, mechanically stirring (300r/min) for 30 minutes, heating the liquid paraffin to 60 ℃ in a water bath, dropwise adding 60mL of chitosan-soybean protein-silicon dioxide mixed solution into the three-neck flask, continuously stirring for two hours until uniform oil bead particles are formed, then adjusting the pH of the mixed solution to 9.5 by using analytically pure sodium hydroxide solution, heating the water bath to 90 ℃, then adding 20mL of analytically pure glutaraldehyde solution, reacting for 3 hours, standing, cooling, filtering to obtain solid microsphere particles, alternately cleaning each by using water and absolute ethyl alcohol for 3 times, and extracting for 24 hours by using ethyl alcohol with the mass percentage concentration of 95% in a Soxhlet extractor. Soaking the solid microsphere particles in 5.0mol/L sodium hydroxide solution for 24 hours, washing with secondary water to be neutral, filtering, drying at 40 ℃, and sieving to obtain the chitosan-soybean protein composite porous microspheres with the particle size of 40-60 meshes. The scanning electron micrograph of the chitosan-soy protein composite porous microsphere is shown in figure 1.
(2) Adsorbing lead by using the chitosan-soybean protein composite porous microspheres:
the separation and enrichment device consists of a peristaltic pump, a self-made micro column (7cm multiplied by 0.5mm i.d.), a polytetrafluoroethylene tube (0.8mm i.d.) and a connecting joint. Plugging a small amount of glass wool at one end of the microcolumn, filling the crosslinked soybean protein microspheres prepared in the step (1) into the microcolumn by a wet process, filling a small amount of glass wool, compacting and connecting, pumping secondary distilled water into the microcolumn by a peristaltic pump, and washing for later use; the Pb (II) separation and enrichment steps are as follows: passing Pb (II) solution with pH of 5.0 through the micro column at flow rate of 3.0mL/min, washing off unadsorbed ions in the micro column with 5.0mL distilled water at flow rate of 3.0mL/min, and adding 10.0mL HNO with concentration of 0.1mol/L3Reversely eluting the adsorbed Pb (II) at the flow rate of 3.6 mL/min; the elution solution was used for subsequent atomic absorption spectroscopy.
(3) The detection method comprises the following steps:
the measuring instrument: atomic absorption spectrophotometer (beijing general analytical instruments ltd); the instrument conditions for measuring Pb by graphite furnace atomic absorption spectrometry are as follows: the wavelength is 283.3nm, the slit is 0.5nm, the lamp current is 2.0mA, and the height of the atomizer is-0.2 mm; the procedure for measuring atomic absorption spectroscopy in a graphite furnace is shown in Table 1. And (3) measuring the concentration of Pb (II) in the eluent obtained in the step (2) by utilizing graphite furnace atomic absorption spectrometry.
Table 1: graphite furnace atomic absorption spectrometry program
| Procedure for measuring the movement of a moving object | Temperature (. degree.C.) | Temperature rise rate (DEG C/s) | Retention time(s) |
| Drying | 80 | 5 | 5 |
| Drying | 100 | 10 | 10 |
| Ashing | 600 | 10 | 10 |
| Atomization of | 1900 | 0 | 4 |
| Purification | 1950 | 1 | 1 |
(4) The adsorption capacity of the chitosan-soybean protein composite porous microspheres to lead is determined:
conditions for flame atomic absorption spectrometry determination of lead: the wavelength is 283.3nm, the slit is 0.5nm, the lamp current is 2.0mA, the height of the burner is 5.0mm, the acetylene flow is 1500mL/min, and the air flow is 5000 mL/min. Adsorbing 20.0 mu g/mL of Pb (II) solution according to the step (2), collecting effluent every 10mL, stopping the experiment until the concentration of lead in the effluent is the same as the original solution concentration, measuring the concentration of Pb (II) in the effluent by using a flame atomic absorption spectrometry, and calculating the adsorption capacity of the chitosan-soybean protein composite porous microspheres to lead to be 42.8 mg/g.
Claims (1)
1. A preparation method of chitosan-soy protein composite porous microspheres for lead adsorption is characterized by comprising the following specific steps:
(1) preparing chitosan-soybean protein composite porous microspheres:
weighing 4g of chitosan, putting the chitosan into a 100mL beaker, adding 50mL of 2% acetic acid solution by mass, stirring for dissolving, standing for 12 hours, and removing bubbles in the solution to obtain a chitosan solution for later use; adding 2.0g of soybean protein and 40mL of secondary water into a 100mL beaker, and stirring until the soybean protein is completely dissolved to obtain a soybean protein solution for later use; mixing 40mL of the chitosan solution with 40mL of the soybean protein solution, adding 2.0g of nano-silica, and uniformly stirring to obtain a chitosan-soybean protein-silica mixed solution for later use;
taking 140mL of liquid paraffin into a 250mL three-neck flask, dropwise adding 4 drops of analytically pure active agent span 80, mechanically stirring for 30 minutes at 300r/min, heating the mixture to 60 ℃ in a water bath, dropwise adding 60mL of chitosan-soy protein-silica mixed solution into the three-neck flask, continuously stirring for two hours until uniform oil bead particles are formed, then adjusting the pH of the mixed solution to 9.5 by using analytically pure sodium hydroxide solution, heating the water bath to 90 ℃, then adding 20mL of analytically pure glutaraldehyde solution, reacting for 3 hours, standing, cooling, filtering to obtain solid microsphere particles, alternately washing each of the solid microsphere particles by using water and absolute ethyl alcohol for 3-5 times, and extracting for 24 hours by using ethyl alcohol with the mass percentage concentration of 95% in a Soxhlet extractor; soaking the solid microsphere particles in 5.0mol/L sodium hydroxide solution for 24 hours, washing with secondary water to be neutral, filtering, drying at 40 ℃, and sieving to obtain chitosan-soybean protein composite porous microspheres with the particle size of 40-60 meshes;
(2) adsorbing lead by using the chitosan-soybean protein composite porous microspheres:
the separation and enrichment device consists of a peristaltic pump, a self-made micro column and a connecting joint; a small amount of glass wool is plugged at one end of the microcolumn, the crosslinked soybean protein microspheres prepared in the step (1) are filled in the microcolumn by a wet method, and thenFilling a small amount of glass wool, compacting and connecting, pumping secondary distilled water into a miniature column by using a peristaltic pump, and washing for later use; the Pb (II) separation and enrichment steps are as follows: pb (II) solution with pH =5.0 was passed through the microcolumn at a flow rate of 3.0mL/min, and then non-adsorbed ions in the microcolumn were washed off with 5.0mL of distilled water at a flow rate of 3.0mL/min, followed by 10.0mL of HNO with a concentration of 0.1mol/L3Reversely eluting the adsorbed Pb (II) at the flow rate of 3.6 mL/min; the elution solution is used for subsequent atomic absorption spectrometry;
(3) the detection method comprises the following steps:
the measuring instrument: an atomic absorption spectrophotometer; the instrument conditions for measuring Pb by graphite furnace atomic absorption spectrometry are as follows: the wavelength is 283.3nm, the slit is 0.5nm, the lamp current is 2.0mA, and the height of the atomizer is-0.2 mm; the procedure for measuring atomic absorption spectrum of graphite furnace is shown in Table 1; measuring the concentration of Pb (II) in the eluent obtained in the step (2) by utilizing a graphite furnace atomic absorption spectrometry;
table 1: graphite furnace atomic absorption spectrometry program
(4) The adsorption capacity of the chitosan-soybean protein composite porous microspheres to lead is determined:
conditions for flame atomic absorption spectrometry determination of lead: the wavelength is 283.3nm, the slit is 0.5nm, the lamp current is 2.0mA, the height of a burner is 5.0mm, the acetylene flow is 1500mL/min, and the air flow is 5000 mL/min; adsorbing 20.0 mu g/mL of Pb (II) solution according to the step (2), collecting effluent every 10mL, stopping the experiment until the concentration of lead in the effluent is the same as the original solution concentration, measuring the concentration of Pb (II) in each effluent by using a flame atomic absorption spectrometry, and calculating the adsorption capacity of the chitosan-soybean protein composite porous microspheres on lead.
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