CN103007894B - 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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- CN103007894B CN103007894B CN201210538271.3A CN201210538271A CN103007894B CN 103007894 B CN103007894 B CN 103007894B CN 201210538271 A CN201210538271 A CN 201210538271A CN 103007894 B CN103007894 B CN 103007894B
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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 processing containing the application aspect heavy metal ion sewage, belong to material and technical field of sewage.
background technology
Due to science and technology and industrial expansion, water pollution problems has been subjected to great concern, and in water pollution problems, comparatively serious surely belong to heavy metal pollution, be present in heavy metal in 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 waste water is processed.
In the processing of the pollutant to heavy metal, absorption method is the heavy metal species treatment technology being most widely used at present, even if the heavy metal ion of dissolved state changes 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 generally using 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 made up 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, is easy to processing etc. as viscosity is relatively low.So recently the exploitation of phytoprotein adsorbent has been subject to the support energetically of environmental protection organization.
Patent CN1094611 discloses a kind of by adding modifier and injecting the method for preparing soybean protein microballoon that the steps such as deionized water realize, patent CN10455645 discloses a kind of by the method for preparing soybean protein microballoon realizing with the method such as buffer solution and emulsifying agent, but the reaction that these methods relate to is more, technique is also more complicated.
In sum, existing heavy metal treatment technology cost costliness, urgent need one is with low cost, the simple preparation method of technique processes heavy metal pollution in water, and existing property of medicine soybean protein microsphere preparation technology is comparatively loaded down with trivial details, and find no the report of soybean protein microballoon as heavy metal ion adsorbing material.
summary of the invention
The present invention is directed to 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 object of the present invention is to provide the soybean protein micro-sphere material of being prepared by the method.
The present invention also provides the soybean protein micro-sphere material making in the application of processing in heavy metal ion-containing waste water.
the object of the invention is to realize in the following manner:
A preparation method for soybean protein micro-sphere material, the method comprises the steps:
Soybean protein is added to the water swelling, stir 10-30min, making concentration is the soybean protein water slurry of 2-10%; Adopt again physical method modulation, finally carry out vacuum defoamation and 0-5 DEG C 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 wherein, making is 2.5-15%.
Wherein, the multistep of described physical method any step or random order in comprising the following steps:
1) thermotropic denaturalization: the soybean protein water slurry making heating water bath at 30-100 DEG C is stirred to 1-10h, and stir speed (S.S.) is 100-3000r/min;
2) ultrasonic: soybean protein water slurry is carried out to ultrasonic processing under 0-20 DEG C of constant temperature, and ultrasonic power is 200-600W, and the time is 0.5-2h;
3) ultraviolet ray is irradiated: soybean protein water slurry is irradiated to 10-240min, the magnetic stirrer that is simultaneously 100-3000r/min with rotating speed through 190-300nm ultraviolet ray;
4) homogenizer homogeneous: by 5-10 circulation of homogenizer homogeneous, the pressure of homogenizer is 10-200 bar by soybean protein water slurry.
The soybean protein micro-sphere material that said method makes.
Above-mentioned soybean protein micro-sphere material is in the application of processing in heavy metal ion-containing waste water.Concrete grammar is as follows:
Regulate the wastewater pH that contains heavy metal ion to 2-6, control wastewater temperature is 20-80 DEG C, soybean protein micro-sphere material is dropped in 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.
Described heavy metal ion be Cr (
), Cu (
), Cd (
), Ni (II), Pb (
) and Zn (
) in one or more mixing.
The in the situation that of pH=5.0, soybean protein micro-sphere material to containing heavy metal Cr (
), Cu (
), Cd (
), Ni (II), Pb (
) and Zn (
) saturated extent of adsorption of solution: at 20 DEG C, be respectively 42.60,92.43,106.37,130.05,169.18 and 174.71 mg/g; At 70 DEG C, 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, taking soybean protein as basis, makes through certain physical method.Have production technology easy, the advantage that cost of material is low, is suitable for industrial processing in enormous quantities.
(2) the soybean protein micro-sphere material that prepared by the present invention, counterweight metal has stronger suction-operated.Thereby it can be applicable to process the waste water containing heavy metal ion.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 at 20 DEG C, 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 at 70 DEG C.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 sewage (
), Cu (
), Cd (
), Ni (II), Pb (
) and Zn (
) etc. free state heavy metal, have and use conveniently, the advantage of non-secondary pollution, is with a wide range of applications.
brief description of the drawings
Accompanying drawing 1 is the electron microscope picture of soybean protein micro-sphere material saturated adsorption Cu (II) at 70 DEG C, can find out that the particle diameter of soybean protein micro-sphere material is between 0.1-200 μ m.
Table 1 is soybean protein micro-sphere material saturated extent of adsorption to each ion at 20 DEG C and 70 DEG C of embodiment 1, compares with similar macromolecular material adsorbent, has 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
osaturated extent of adsorption to each ion under C, compares with similar macromolecular material adsorbent, has better adsorption effect.
Table 3 is that the soybean protein micro-sphere material of embodiment 1 is 20
oadsorbance to different heavy metal ion in solution under C, finds the adsorption effect of Cu (II) better than Ni (II) and Pb (II).
detailed description of the invention
embodiment 1:the preparation method of soybean protein microballoon comprises the following steps successively:
5g soybean protein is added in 100mL water swelling, stir 10min, make concentration and be 5% soybean protein water slurry;
Gained suspension heating water bath at 70 DEG C is stirred to 2h, and speed of agitator is 500r/min;
Suspension after heat treatment is mixed well, and the Ultrasound Instrument that is 200W with power is carried out ultrasonic processing 1h to suspension, and ultrasonic procedure system temperature is constant in 0-10 DEG C;
Suspension after ultrasonic is placed on to cool drying in the refrigerator of 0-5 DEG C, makes 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 comprises the following steps successively:
2g soybean protein is added in 100mL water swelling, stir 10min, make concentration and be 2% soybean protein water slurry;
The Ultrasound Instrument that is 400W with power is carried out ultrasonic to it, ultrasonic procedure system temperature is constant in 0-10 DEG C, and ultrasonic time is 0.5h;
Product after ultrasonic is carried out to vacuum defoamation, after cold hydrazine cool drying, make soybean protein micro-sphere material in subzero 40 DEG C.Its particle diameter of surveying by electron microscope is between 1-100 μ m.
embodiment 3:the preparation method of soybean protein microballoon comprises the following steps successively:
5g soybean protein is added in 100mL water swelling, stir 20min, make concentration and be 5% soybean protein water slurry;
10 circulations of the high pressure homogenizing device that is 100bar by pressure by gained suspension;
Product after HIGH PRESSURE TREATMENT is carried out to cooling deaeration, after being dried, can be made into soybean protein micro-sphere material.
embodiment 4:the preparation method of soybean protein microballoon comprises the following steps successively:
8g soybean protein is added in 100 mL water swelling, stir 30 min, make concentration and be 8% soybean protein water slurry;
By gained suspension radiation 120 min under the strong ultraviolet lamp line of 253.7nm, be the magnetic stirrer of 500 r/min with rotating speed simultaneously;
Soybean protein microballoon after crosslinked is obtained to soybean protein micro-sphere material through vacuum drying.
embodiment 5:the preparation method of soybean protein microballoon comprises the following steps successively:
10g soybean protein is added in 100 mL water swelling, stir 30 min, make concentration and be 10% soybean protein water slurry;
By gained suspension radiation 60min under the strong ultraviolet lamp line of 253.7nm, be the magnetic stirrer of 1000 r/min with rotating speed simultaneously.
Gained suspension heating water bath at 80 DEG C is stirred to 2h, and speed of agitator is 500r/min;
Suspension after heat treatment is mixed well, and the Ultrasound Instrument that is 400W with power is carried out ultrasonic processing 1h to suspension, and ultrasonic procedure system temperature is constant in 10-15 DEG C;
6 circulations of the high pressure homogenizing device that is 50bar by pressure by gained suspension;
After high pressure homogenizing is processed, product carries out cooling deaeration, after being dried, can be made into soybean protein micro-sphere material.
embodiment 6:
Take 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 solution, pH is adjusted to 5.0, at 20 DEG C, stirs 4h; Utilize centrifuge under the condition of 12000r/min, carried out Separation of Solid and Liquid, and join and get standard liquid; Survey its concentration by flame atomic absorption spectrophotometer, and calculate respectively adsorbance (in table 1).
embodiment 7:
Take 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 solution, pH is adjusted to 5.0, at 70 DEG C, stirs 4h; Utilize centrifuge under the condition of 12000r/min, carried out Separation of Solid and Liquid, and join and get standard liquid; Survey its concentration by flame atomic absorption spectrophotometer, and calculate respectively adsorbance (in table 1).Utilize electron microscope to Adsorption of Cu (
) soybean protein micro-sphere material characterize (seeing accompanying drawing 1).
embodiment 8:
Take 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 solution, pH is adjusted to 5.0, at 15 DEG C, stirs 5h; Utilize Buchner funnel to be filtered, make Separation of Solid and Liquid, and join and get standard liquid; Survey its concentration by flame atomic absorption spectrophotometer, and calculate adsorbance (in table 2).
embodiment 9:
Take 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 solution, pH is adjusted to 5.0, at 25 DEG C, stirs 4h; Utilize Buchner funnel to be filtered, make Separation of Solid and Liquid, and join and get standard liquid; Survey its concentration by flame atomic absorption spectrophotometer, and calculate adsorbance (in table 2).
embodiment 10:
Take 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 solution, pH is adjusted to 5.0, at 50 DEG C, stirs 3h; Utilize Buchner funnel to be filtered, make Separation of Solid and Liquid, and join and get standard liquid; Survey its concentration by flame atomic absorption spectrophotometer, and calculate adsorbance (in table 2).
embodiment 11:
Take 1 part of the soybean protein micro-sphere material that 0.1g embodiment 1 makes; Add 100mL contain Cu (
) and the solution of the each 50mg/L of Ni (II) in, pH is adjusted to 5.0, at 20 DEG C, stirs 4h; Utilize centrifuge under the condition of 12000r/min, carried out Separation of Solid and Liquid, and join and get standard liquid; Survey its concentration by flame atomic absorption spectrophotometer, calculate the adsorbance (in table 3) to these two kinds of ions.
embodiment 12:
Take 1 part of the soybean protein micro-sphere material that 0.1g embodiment 1 makes; Add 100mL contain Cu (
) and the solution of the each 50mg/L of Cd (II) in, pH is adjusted to 5.0, at 20 DEG C, stirs 4h; Utilize centrifuge under the condition of 12000r/min, carried out Separation of Solid and Liquid, and join and get standard liquid; Survey its concentration by flame atomic absorption spectrophotometer, calculate the adsorbance (in table 3) to these two kinds of ions.
Table 1: soybean protein micro-sphere material is 20
oc and 70
oadsorbance (mg/g) to different heavy metal ion under C
| Metal ion | 20 oSaturated extent of adsorption under C (mg/g) | 70 oSaturated extent of adsorption under 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: soybean protein micro-sphere material is 15
oc, 25
oc and 70
oadsorbance (mg/g) to different heavy metal ion under C
| Metal ion | 15 oSaturated extent of adsorption under C (mg/g) | 25 oSaturated extent of adsorption under C (mg/g) | 50 oSaturated extent of adsorption under 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: soybean protein micro-sphere material is 20
oadsorbance (mg/g) to different heavy metal ion in solution under C
| Metal ion | 20 oSaturated extent of adsorption under C (mg/g) | 20 oSaturated extent of adsorption under C (mg/g) |
| Cu(II) | 50.21 | 54.69 |
| Ni(II) | 30.86 | — |
| Pb(II) | — | 63.44 |
Claims (2)
1. a preparation method for soybean protein micro-sphere material, the method comprises the steps:
Soybean protein is added to the water swelling, stir 10-30min, making concentration is the soybean protein water slurry of 2-10%; Adopt again physical method modulation, finally carry out vacuum defoamation and 0-5 DEG C 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 wherein, making is 2.5-15%; Wherein, the multistep of described physical method any step or random order in comprising the following steps:
1) thermotropic denaturalization: the soybean protein water slurry making heating water bath at 30-100 DEG C is stirred to 1-10h, and stir speed (S.S.) is 100-3000r/min;
2) ultrasonic: soybean protein water slurry is carried out to ultrasonic processing under 0-20 DEG C of constant temperature, and ultrasonic power is 200-600W, and the time is 0.5-2h;
3) ultraviolet ray is irradiated: soybean protein water slurry is irradiated to 10-240min, the magnetic stirrer that is simultaneously 100-3000r/min with rotating speed through 190-300nm ultraviolet ray;
4) homogenizer homogeneous: by 5-10 circulation of homogenizer homogeneous, the pressure of homogenizer is 10-200 bar by soybean protein water slurry.
2. the soybean protein micro-sphere material that described in claim 1, preparation method makes.
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| 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 |
| CN107376872B (en) * | 2017-08-06 | 2020-01-21 | 桂林理工大学 | Preparation method of chitosan-soybean protein composite porous microspheres for lead adsorption |
| 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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