CN103007894A - Soybean protein micro sphere material and preparation method and application of material in treating waste water containing heavy metal ion - Google Patents
Soybean protein micro sphere material and preparation method and application of material in treating waste water containing heavy metal ion Download PDFInfo
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- CN103007894A CN103007894A CN2012105382713A CN201210538271A CN103007894A CN 103007894 A CN103007894 A CN 103007894A CN 2012105382713 A CN2012105382713 A CN 2012105382713A CN 201210538271 A CN201210538271 A CN 201210538271A CN 103007894 A CN103007894 A CN 103007894A
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Abstract
The invention relates to a soybean protein micro sphere material and a preparation method and application of the soybean protein micro sphere material in treating waste water containing heavy metal ion. The method comprises the following steps of: adding soybean protein into water to be swelled; stirring for 10-30min and preparing soybean protein water suspension liquid of which the concentration is 2-10%; conditioning by using a physical method; finally carrying out vacuum defoamation and cooling and drying at 0-5 DEG C so as to obtain the soybean protein micro sphere material of which the micro sphere particle size is 0.1-200micon. The soybean protein micro sphere is prepared by using the soybean protein as the raw material and by using the method of thermotropic conversion, ultrasonic, ultraviolet irradiation, homogeneity by using a homogenizer and the like. The soybean protein micro sphere material has the advantages of simple production process and low raw material cost. The micro sphere material can be used for absorbing free state heavy metals such as lead, chromium, copper, nickel, zinc, mercury and the like in sewage water in a feeding and stirring mode, has the advantages of convenience in implementation, good absorption effect, high absorption capacity, recycling and treatment easiness and secondary pollution freeness, and has wide application prospect.
Description
Technical field
The present invention relates to a kind of soybean protein micro-sphere material, and its preparation method, also relate to it and contain application aspect the heavy metal ion sewage in processing, belong to material and technical field of sewage.
Background technology
Because science and technology and industrial expansion, water pollution problems has been subjected to great concern, and in the water pollution problems, comparatively serious surely belong to heavy metal pollution, be present in heavy metal in the waste water in discharge process, be not only a kind of waste of resource, a kind of serious environmental problem especially, these heavy metals enter human body by food chain and also can damage human body.For the angle of economic benefit and ecological protection, it is very necessary and significant that the heavy metal in the waste water is processed.
In the processing to the pollutant of heavy metal, absorption method is a heavy metal species treatment technology that is most widely used at present, even the heavy metal ion of dissolved state changes the insoluble compound precipitation into.Up to the present, absorption method has been applied to the fields such as chemical industry, environmental protection, medical and health and bioengineering, but the industrial adsorbent that generally uses is expensive, and the application of absorption method is restricted.Therefore, we need to develop a kind of economical and efficient, and environment amenable adsorbent, to replace traditional heavy metal treatment product.
Soybean protein is the byproduct of soya-bean oil industry, is comprised of 18 seed amino acids, and strand is rich in amine, carboxylic acid, and hydroxyl and mercaptan isopolarity functional group have good biologically active and biodegradability.As adsorbent, soybean protein has significant advantage, such as the relatively low processing etc. that is easy to of viscosity.So recently the exploitation of phytoprotein adsorbent has been subject to the energetically support of environmental protection organization.
Patent CN1094611 discloses a kind of method for preparing the soybean protein microballoon that realizes by adding the steps such as modifier and injection deionized water, patent CN10455645 discloses a kind of method for preparing the soybean protein microballoon by realizing with methods such as buffer solution and emulsifying agents, but the reaction that these methods relate to is more, and technique is also complicated.
In sum, existing heavy metal treatment technology cost is expensive, be badly in need of a kind of with low cost, simple preparation method of technique and process heavy metal pollution in the water, and existing property of medicine soybean protein microsphere preparation technology is comparatively loaded down with trivial details, and finds no the soybean protein microballoon as the report of heavy metal ion adsorbing material.
Summary of the invention
The present invention is directed to the prior art above shortcomings, a kind of preparation method of soybean protein micro-sphere material is provided, the method technique is simple, and production cost is low, is suitable for suitability for industrialized production.
Another purpose of the present invention provides the soybean protein micro-sphere material by the method preparation.
The present invention also provides the application of the soybean protein micro-sphere material that makes in processing heavy metal ion-containing waste water.
The objective of the invention is to realize in the following manner:
A kind of preparation method of soybean protein micro-sphere material, the method comprises the steps:
Soybean protein is added to the water swelling, stirs 10-30min, making concentration is the soybean protein water slurry of 2-10%; Adopt again the physical method modulation, carry out at last vacuum defoamation and 0-5 ℃ cool drying, make the soybean protein micro-sphere material of microspherulite diameter between 0.1-200 μ m.
The solid content of the soybean protein microballoon that wherein, makes is 2.5-15%.
Wherein, the multistep of any step or random order during described physical method may further comprise the steps:
1) thermotropic denaturalization: the soybean protein water slurry that makes is stirred 1-10h at 30-100 ℃ of lower heating water bath, and stir speed (S.S.) is 100-3000r/min;
2) ultrasonic: the soybean protein water slurry is carried out ultrasonic processing under 0-20 ℃ of constant temperature, ultrasonic power is 200-600W, and the time is 0.5-2h;
3) ultraviolet ray irradiation: the soybean protein water slurry is shone 10-240min through the 190-300nm ultraviolet ray, is the magnetic stirrer of 100-3000r/min simultaneously with rotating speed;
4) homogenizer homogeneous: by 5-10 circulation of homogenizer homogeneous, the pressure of homogenizer is 10-200 bar with the soybean protein water slurry.
The soybean protein micro-sphere material that said method makes.
The application of above-mentioned soybean protein micro-sphere material in processing heavy metal ion-containing waste water.Concrete grammar is as follows:
Adjusting contains the wastewater pH of heavy metal ion to 2-6, the control wastewater temperature is 20-80 ℃, the soybean protein micro-sphere material is dropped in the waste water, wherein the mass ratio of heavy metal ion and soybean protein microballoon is 1/10-1/1, under the stirring condition of 60-1000r/min, stirring and adsorbing 10-480 min filters or centrifugation after having adsorbed, and carries out Separation of Solid and Liquid and gets final product.
Described heavy metal ion be Cr (
), Cu (
), Cd (
), Ni (II), Pb (
) and Zn (
) in one or more mixing.
In the situation of pH=5.0, the soybean protein micro-sphere material to contain heavy metal Cr (
), Cu (
), Cd (
), Ni (II), Pb (
) and Zn (
) saturated extent of adsorption of solution: under 20 ℃, be respectively 42.60,92.43,106.37,130.05,169.18 and 174.71 mg/g; Under 70 ℃, be respectively 52.94,115.01,120.83,177.11,235.56 and 254.95mg/g.
The present invention compared with prior art has following beneficial effect:
(1) preparation method of soybean protein microballoon of the present invention makes through certain physical method take soybean protein as the basis.It is easy to have production technology, and the advantage that cost of material is low is suitable for industrial processing in enormous quantities.
(2) the soybean protein micro-sphere material of the present invention's preparation, the counterweight metal has stronger suction-operated.Thereby it can be applicable to process the waste water that contains heavy metal ion.The inventor is through measuring, the soybean protein micro-sphere material that this method makes to heavy metal ion Cr (
), Cu (
), Cd (
), Ni (II), Pb (
) and Zn (
) saturated extent of adsorption under 20 ℃, be respectively 42.60,92.43,106.37,130.05,169.18 and 174.71mg/g, be respectively 52.94,115.01,120.83,177.11,235.56 and 254.95mg/g under 70 ℃.Its cost performance is far above parallel material.
(3) this soybean protein micro-sphere material can by the mode that adds and stir adsorb Cr in the sewage (
), Cu (
), Cd (
), Ni (II), Pb (
) and Zn (
) etc. the free state heavy metal, have and use conveniently, the advantage of non-secondary pollution is with a wide range of applications.
Description of drawings
Accompanying drawing 1 be the soybean protein micro-sphere material in the electron microscope picture of 70 ℃ of lower saturated adsorption Cu (II), can find out that the particle diameter of soybean protein micro-sphere material is between 0.1-200 μ m.
Table 1 be the soybean protein micro-sphere material of embodiment 1 under 20 ℃ and 70 ℃ to the saturated extent of adsorption of each ion, compare with similar macromolecular material adsorbent, have better adsorption effect.
The soybean protein micro-sphere material that table 2 makes for embodiment 2,3,4 is 15
oC, 25
oC and 50
oTo the saturated extent of adsorption of each ion, compare with similar macromolecular material adsorbent under the C, have better adsorption effect.
Table 3 is that the soybean protein micro-sphere material of embodiment 1 is 20
oTo the adsorbance of different heavy metal ion in the solution, find the adsorption effect of Cu (II) better than Ni (II) and Pb (II) under the C.
The specific embodiment
Embodiment 1:The preparation method of soybean protein microballoon may further comprise the steps successively:
The 5g soybean protein is added swelling in the 100mL water, stir 10min, make concentration and be 5% soybean protein water slurry;
Gained suspension is stirred 2h at 70 ℃ of lower heating water baths, and speed of agitator is 500r/min;
Suspension after the heat treatment is mixed well, and is that the Ultrasound Instrument of 200W is carried out ultrasonic processing 1h to suspension with power, and the ultrasonic procedure system temperature is constant in 0-10 ℃;
Suspension after ultrasonic is placed on cool drying in 0-5 ℃ the refrigerator, makes the soybean protein micro-sphere material.Its particle diameter of surveying by electron microscope is between 10-200 μ m.
Embodiment 2:The preparation method of soybean protein microballoon may further comprise the steps successively:
The 2g soybean protein is added swelling in the 100mL water, stir 10min, make concentration and be 2% soybean protein water slurry;
It is ultrasonic with power to be that the Ultrasound Instrument of 400W is carried out it, and the ultrasonic procedure system temperature is constant in 0-10 ℃, and ultrasonic time is 0.5h;
Product after ultrasonic is carried out vacuum defoamation, behind the cold hydrazine cool drying, make the soybean protein micro-sphere material in subzero 40 ℃.Its particle diameter of surveying by electron microscope is between 1-100 μ m.
Embodiment 3:The preparation method of soybean protein microballoon may further comprise the steps successively:
The 5g soybean protein is added swelling in the 100mL water, stir 20min, make concentration and be 5% soybean protein water slurry;
Be 10 circulations of high pressure homogenizing device of 100bar by pressure with gained suspension;
Product after the HIGH PRESSURE TREATMENT is cooled off deaeration, can be made into the soybean protein micro-sphere material after the drying.
Embodiment 4:The preparation method of soybean protein microballoon may further comprise the steps successively:
The 8g soybean protein is added swelling in the 100 mL water, stir 30 min, make concentration and be 8% soybean protein water slurry;
With gained suspension radiation 120 min under the strong ultraviolet lamp line of 253.7nm, be the magnetic stirrer of 500 r/min simultaneously with rotating speed;
Soybean protein microballoon after crosslinked is obtained the soybean protein micro-sphere material through vacuum drying.
Embodiment 5:The preparation method of soybean protein microballoon may further comprise the steps successively:
The 10g soybean protein is added swelling in the 100 mL water, stir 30 min, make concentration and be 10% soybean protein water slurry;
With gained suspension radiation 60min under the strong ultraviolet lamp line of 253.7nm, be the magnetic stirrer of 1000 r/min simultaneously with rotating speed.
Gained suspension is stirred 2h at 80 ℃ of lower heating water baths, and speed of agitator is 500r/min;
Suspension after the heat treatment is mixed well, and is that the Ultrasound Instrument of 400W is carried out ultrasonic processing 1h to suspension with power, and the ultrasonic procedure system temperature is constant in 10-15 ℃;
Be 6 circulations of high pressure homogenizing device of 50bar by pressure with gained suspension;
High pressure homogenizing is processed rear product cool off deaeration, can be made into the soybean protein micro-sphere material after the drying.
Embodiment 6:
Take by weighing 6 parts of the soybean protein micro-sphere materials that 0.1g embodiment 1 makes; Add respectively 100mL 200mg/L Cr (
), Cu (
), Cd (
), Ni (II), Pb (
) and Zn (
) in the solution, pH is adjusted to 5.0, at 20 ℃ of lower 4h that stir; Utilize centrifuge under the condition of 12000r/min, it is carried out Separation of Solid and Liquid, and join the accurate solution of label taking; Survey its concentration by flame atomic absorption spectrophotometer, and calculate respectively adsorbance (seeing Table 1).
Embodiment 7:
Take by weighing 6 parts of the soybean protein micro-sphere materials that 0.1g embodiment 1 makes; Add respectively 100mL 200mg/L Cr (
), Cu (
), Cd (
), Ni (II), Pb (
) and Zn (
) in the solution, pH is adjusted to 5.0, at 70 ℃ of lower 4h that stir; Utilize centrifuge under the condition of 12000r/min, it is carried out Separation of Solid and Liquid, and join the accurate solution of label taking; Survey its concentration by flame atomic absorption spectrophotometer, and calculate respectively adsorbance (seeing Table 1).Utilize electron microscope to Adsorption of Cu (
) the soybean protein micro-sphere material characterize (seeing accompanying drawing 1).
Embodiment 8:
Take by weighing 6 parts of the soybean protein micro-sphere materials that 0.2g embodiment 2 makes; Add respectively 200mL 200mg/L Cr (
), Cu (
), Cd (
), Ni (II), Pb (
) and Zn (
) in the solution, pH is adjusted to 5.0, at 15 ℃ of lower 5h that stir; Utilize Buchner funnel that it is filtered, make Separation of Solid and Liquid, and join the accurate solution of label taking; Survey its concentration by flame atomic absorption spectrophotometer, and calculate adsorbance (seeing Table 2).
Embodiment 9:
Take by weighing 6 parts of the soybean protein micro-sphere materials that 0.1g embodiment 3 makes; Add respectively 100mL 100mg/L Cr (
), Cu (
), Cd (
), Ni (II), Pb (
) and Zn (
) in the solution, pH is adjusted to 5.0, at 25 ℃ of lower 4h that stir; Utilize Buchner funnel that it is filtered, make Separation of Solid and Liquid, and join the accurate solution of label taking; Survey its concentration by flame atomic absorption spectrophotometer, and calculate adsorbance (seeing Table 2).
Embodiment 10:
Take by weighing 6 parts of the soybean protein micro-sphere materials that 0.1g embodiment 4 makes; Add respectively 100mL 200mg/L Cr (
), Cu (
), Cd (
), Ni (II), Pb (
) and Zn (
) in the solution, pH is adjusted to 5.0, at 50 ℃ of lower 3h that stir; Utilize Buchner funnel that it is filtered, make Separation of Solid and Liquid, and join the accurate solution of label taking; Survey its concentration by flame atomic absorption spectrophotometer, and calculate adsorbance (seeing Table 2).
Embodiment 11:
Take by weighing 1 part of the soybean protein micro-sphere material that 0.1g embodiment 1 makes; Add 100mL contain Cu (
) and the solution of each 50mg/L of Ni (II) in, pH is adjusted to 5.0, at 20 ℃ of lower 4h that stir; Utilize centrifuge under the condition of 12000r/min, it is carried out Separation of Solid and Liquid, and join the accurate solution of label taking; Survey its concentration by flame atomic absorption spectrophotometer, calculate the adsorbance (seeing Table 3) to these two kinds of ions.
Embodiment 12:
Take by weighing 1 part of the soybean protein micro-sphere material that 0.1g embodiment 1 makes; Add 100mL contain Cu (
) and the solution of each 50mg/L of Cd (II) in, pH is adjusted to 5.0, at 20 ℃ of lower 4h that stir; Utilize centrifuge under the condition of 12000r/min, it is carried out Separation of Solid and Liquid, and join the accurate solution of label taking; Survey its concentration by flame atomic absorption spectrophotometer, calculate the adsorbance (seeing Table 3) to these two kinds of ions.
Table 1: the soybean protein micro-sphere material is 20
oC and 70
oUnder the C to the adsorbance (mg/g) of different heavy metal ion
| Metal ion | 20 oSaturated extent of adsorption under the C (mg/g) | 70 oSaturated extent of adsorption under the C (mg/g) |
| Zn(II) | 174.71 | 254.95 |
| Cr(II) | 42.60 | 52.94 |
| Pb(II) | 169.18 | 235.56 |
| Cd(II) | 106.37 | 120.83 |
| Cu(II) | 92.43 | 115.01 |
| Ni(II) | 130.05 | 177.11 |
Table 2: the soybean protein micro-sphere material is 15
oC, 25
oC and 70
oUnder the C to the adsorbance (mg/g) of different heavy metal ion
| Metal ion | 15 oSaturated extent of adsorption under the C (mg/g) | 25 oSaturated extent of adsorption under the C (mg/g) | 50 oSaturated extent of adsorption under the C (mg/g) |
| Zn(II) | 167.79 | 183.33 | 235.46 |
| Cr(II) | 40.56 | 45.62 | 50.04 |
| Pb(II) | 164.48 | 176.68 | 224.54 |
| Cd(II) | 103.35 | 108.88 | 108.68 |
| Cu(II) | 89.56 | 94.46 | 110.30 |
| Ni(II) | 127.75 | 136.67 | 169.74 |
Table 3: the soybean protein micro-sphere material is 20
oUnder the C to the adsorbance (mg/g) of different heavy metal ion in the solution
| Metal ion | 20 oSaturated extent of adsorption under the C (mg/g) | 20 oSaturated extent of adsorption under the C (mg/g) |
| Cu(II) | 50.21 | 54.69 |
| Ni(II) | 30.86 | — |
| Pb(II) | — | 63.44 |
Claims (8)
1. the preparation method of a soybean protein micro-sphere material, the method comprises the steps:
Soybean protein is added to the water swelling, stirs 10-30min, making concentration is the soybean protein water slurry of 2-10%; Adopt again the physical method modulation, carry out at last vacuum defoamation and 0-5 ℃ cool drying, make the soybean protein micro-sphere material of microspherulite diameter between 0.1-200 μ m.
2. preparation method according to claim 1, wherein, the solid content of the soybean protein microballoon that makes is 2.5-15%.
3. preparation method according to claim 1 and 2, wherein, the multistep of any step or random order during described physical method may further comprise the steps:
1) thermotropic denaturalization: the soybean protein water slurry that makes is stirred 1-10h at 30-100 ℃ of lower heating water bath, and stir speed (S.S.) is 100-3000r/min;
2) ultrasonic: the soybean protein water slurry is carried out ultrasonic processing under 0-20 ℃ of constant temperature, ultrasonic power is 200-600W, and the time is 0.5-2h;
3) ultraviolet ray irradiation: the soybean protein water slurry is shone 10-240min through the 190-300nm ultraviolet ray, is the magnetic stirrer of 100-3000r/min simultaneously with rotating speed;
4) homogenizer homogeneous: by 5-10 circulation of homogenizer homogeneous, the pressure of homogenizer is 10-200 bar with the soybean protein water slurry.
4. the soybean protein micro-sphere material that makes of claim 1,2 or 3 described preparation methods.
5. the application of the described soybean protein micro-sphere material of claim 4 in processing heavy metal ion-containing waste water.
6. application according to claim 5, it is characterized in that: concrete grammar is as follows:
Adjusting contains the wastewater pH of heavy metal ion to 2-6, the control wastewater temperature is 20-80 ℃, the soybean protein micro-sphere material is dropped in the waste water, wherein the mass ratio of heavy metal ion and soybean protein microballoon is 1/10-1/1, under the stirring condition of 60-1000r/min, stirring and adsorbing 10-480 min filters or centrifugation after having adsorbed, and carries out Separation of Solid and Liquid and gets final product.
7. application according to claim 6 is characterized in that; Described heavy metal ion be Cr (
), Cu (
), Cd (
), Ni (II), Pb (
) and Zn (
) in one or more mixing.
8. application according to claim 7 is characterized in that: in the situation of pH=5.0, the soybean protein micro-sphere material to contain heavy metal Cr (
), Cu (
), Cd (
), Ni (II), Pb (
) and Zn (
) saturated extent of adsorption of solution: under 20 ℃, be respectively 42.60,92.43,106.37,130.05,169.18 and 174.71 mg/g; Under 70 ℃, be respectively 52.94,115.01,120.83,177.11,235.56 and 254.95mg/g.
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|---|---|---|---|
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Cited By (9)
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| CN103964536A (en) * | 2014-04-18 | 2014-08-06 | 湖南师范大学 | Method for treating heavy metal cadmium pollution in water |
| CN105293658A (en) * | 2015-10-15 | 2016-02-03 | 顺德职业技术学院 | Water soluble biomass heavy metal capture agent and preparation method of water soluble biomass heavy metal capture agent |
| CN105833847A (en) * | 2016-05-05 | 2016-08-10 | 张小霞 | Heavy metal chelating agent with biological environmental protection property and preparing method thereof |
| CN106000326A (en) * | 2016-06-14 | 2016-10-12 | 常州天地人和生物科技有限公司 | Preparation and application of super tolerance metal chelating affinity packing |
| CN107376872A (en) * | 2017-08-06 | 2017-11-24 | 桂林理工大学 | Preparation method for the chitosan soybean protein composite porous microspheres of lead absorption |
| CN107442073A (en) * | 2017-08-06 | 2017-12-08 | 桂林理工大学 | For the preparation method for the crosslinking soybean protein microballoon for adsorbing cadmium |
| CN107552024A (en) * | 2017-08-06 | 2018-01-09 | 桂林理工大学 | Preparation method for the crosslinking casein porous microsphere of lead absorption |
| CN107683910A (en) * | 2017-07-28 | 2018-02-13 | 含山县长通食品制造有限公司 | A kind of processing method for improving lipid-antioxidant activity during peppery bar stores |
| CN112058241A (en) * | 2020-09-15 | 2020-12-11 | 太原科技大学 | Preparation method of composite adsorption material containing soy protein |
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| CN103964536A (en) * | 2014-04-18 | 2014-08-06 | 湖南师范大学 | Method for treating heavy metal cadmium pollution in water |
| CN105293658A (en) * | 2015-10-15 | 2016-02-03 | 顺德职业技术学院 | Water soluble biomass heavy metal capture agent and preparation method of water soluble biomass heavy metal capture agent |
| CN105833847A (en) * | 2016-05-05 | 2016-08-10 | 张小霞 | Heavy metal chelating agent with biological environmental protection property and preparing method thereof |
| CN106000326A (en) * | 2016-06-14 | 2016-10-12 | 常州天地人和生物科技有限公司 | Preparation and application of super tolerance metal chelating affinity packing |
| CN106000326B (en) * | 2016-06-14 | 2018-11-02 | 常州天地人和生物科技有限公司 | A kind of super metals tolerant chelates the preparation and application of affine filler |
| CN107683910A (en) * | 2017-07-28 | 2018-02-13 | 含山县长通食品制造有限公司 | A kind of processing method for improving lipid-antioxidant activity during peppery bar stores |
| CN107376872A (en) * | 2017-08-06 | 2017-11-24 | 桂林理工大学 | Preparation method for the chitosan soybean protein composite porous microspheres of lead absorption |
| CN107442073A (en) * | 2017-08-06 | 2017-12-08 | 桂林理工大学 | For the preparation method for the crosslinking soybean protein microballoon for adsorbing cadmium |
| CN107552024A (en) * | 2017-08-06 | 2018-01-09 | 桂林理工大学 | Preparation method for the crosslinking casein porous microsphere of lead absorption |
| CN112058241A (en) * | 2020-09-15 | 2020-12-11 | 太原科技大学 | Preparation method of composite adsorption material containing soy protein |
| CN112058241B (en) * | 2020-09-15 | 2022-11-15 | 太原科技大学 | Preparation method of composite adsorption material containing soy protein |
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| CN103007894B (en) | 2014-12-10 |
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