CN107486185B - Method for preparing selective adsorption material by using phosphorus-rich biomass - Google Patents
Method for preparing selective adsorption material by using phosphorus-rich biomass Download PDFInfo
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- CN107486185B CN107486185B CN201710964546.2A CN201710964546A CN107486185B CN 107486185 B CN107486185 B CN 107486185B CN 201710964546 A CN201710964546 A CN 201710964546A CN 107486185 B CN107486185 B CN 107486185B
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/265—Synthetic macromolecular compounds modified or post-treated polymers
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
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- C02F2101/101—Sulfur compounds
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
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- C02F2101/105—Phosphorus compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/007—Contaminated open waterways, rivers, lakes or ponds
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Abstract
A method for preparing a selective adsorption material by using phosphorus-rich biomass relates to the technical field of molecular imprinting, biomass materials and water treatment application. Firstly, glutaraldehyde solution is utilized to crosslink and fix collagen of the phosphorus-rich biomass, and then citric acid is utilized to remove XO combined with the collagen in the phosphorus-rich biomass4 n‑A conformational molecule, thereby making it specific for XO4 n‑A selective adsorbent material in molecular configuration. The invention only needs two steps of fixing and acid washing to successfully obtain the selective adsorbing material of phosphate radical and sulfate radical. The characterization of an electron microscope and the like proves that the phosphate radical and sulfate radical selective binding property is achieved. The selective adsorption material prepared by using the phosphorus-rich biological wastes such as fish scales and the like as raw materials can be recycled, so that the cost is low, the technical route is extremely simple, and phosphate radicals in secondary sedimentation tank effluent and eutrophic lakes of domestic urban sewage treatment plants and sulfate radicals in acid mine wastewater and the like can be effectively removed.
Description
Technical Field
The invention relates to the technical field of molecular imprinting, biomass material and water treatment application, in particular to a method for preparing a selective adsorption material by using phosphorus-rich biomass.
Background
At present, the total phosphorus in effluent is less than or equal to 0.5mg/L along with the upgrading and upgrading of the effluent of more and more urban sewage treatment plants to primary A. In order to achieve the discharge standard, chemical phosphorus removal is added after the biological nitrogen and phosphorus removal process. But the chemical phosphorus removal method needs to add a large amount of phosphorus removal agent, so that the phosphorus removal cost is greatly increased, and the addition of the phosphorus removal agent can produce a large amount of sludge, so that the sludge treatment cost is increased; in addition, the added phosphorus removal agent cannot be reused.
China is the country with the largest aquatic product yield in the world, and the total aquatic product yield in the country is about 4500 ten thousand tons in recent years, wherein the aquaculture yield accounts for 58% of the total yield. Most of leftovers produced in the processing process of aquatic products are discarded as raw materials or waste materials of feed fish meal, so that the environment is polluted and economic loss is caused. The fish scale is one of the main components in the leftovers, and has the characteristics of wide source and low cost.
The invention provides a method for preparing a selective adsorption material by using phosphorus-rich biomass, which is characterized in that glutaraldehyde and citric acid are firstly adopted to treat the phosphorus-rich biomass (such as fish scales, animal bones and the like) to prepare the selective adsorption material capable of being used for sewage treatment, and the prepared adsorption material can be recycled and has low cost.
Disclosure of Invention
Aiming at the technical problems, the invention provides a method for preparing a selective adsorption material by using phosphorus-rich biomass, which has simple process and low cost and is suitable for industrial scale production.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: a method for preparing selective adsorption material by using phosphorus-rich biomass comprises the steps of firstly utilizing glutaraldehyde solution to crosslink and fix collagen of the phosphorus-rich biomass, and then utilizing citric acid to wash and remove XO combined with the collagen in the phosphorus-rich biomass4 n-A conformational molecule, thereby making it specific for XO4 n-A selective adsorbent material in molecular configuration.
As a preferred technical scheme of the invention, the preparation steps are as follows:
firstly, putting the cleaned phosphorus-rich biomass into a container, and then adding a proper amount of glutaraldehyde solution into the container, wherein the addition amount of the glutaraldehyde solution is at least based on the complete immersion of the phosphorus-rich biomass;
② soaking at room temperature, then removing supernatant, washing solid with water;
thirdly, adding citric acid into the solid, adding a proper amount of water, and stirring and soaking at room temperature;
and fourthly, removing supernatant, washing residues with water, and drying to obtain the selective adsorption material.
As a preferable technical scheme of the invention, the phosphorus-rich biomass is selected from fish scales which need to be washed till no blood water exists.
As another preferred embodiment of the present invention, the phosphorus-rich biomass is selected from animal bones, which are first pulverized and then the animal bone powder is washed to be bloodless water.
As a further preferable technical scheme of the invention, in the preparation method, the volume percentage of the glutaraldehyde solution in the step (i) is 5-15%. The soaking time in the step II and the stirring and soaking time in the step III are both 5 to 15 hours. In the third step, the mass ratio of the solid to the citric acid is 1: 0.8-1.2. In the step IV, the drying temperature is 70-80 ℃.
According to the invention, the solid waste phosphorus-rich biomass and the conventional glutaraldehyde solution are used as reaction raw materials, and the selective adsorption material for phosphate radicals and sulfate radicals can be successfully obtained only through two steps of reaction of fixation and acid washing. The characteristics of electron microscopy and the like prove that the selective adsorbing material for phosphate radical and sulfate radical prepared by the method has the characteristic of selectively combining phosphate radical and sulfate radical. The preparation method provided by the invention adopts the phosphorus-rich biological wastes such as fish scales and the like as raw materials, the prepared selective adsorption material can be recycled, the cost is low, the technical route is extremely simple, and phosphate radicals in secondary sedimentation tank effluent of a domestic town sewage treatment plant and eutrophicated lakes, acid radicals in acid mine wastewater and the like can be effectively removed. Compared with the prior art, the invention also has the following advantages:
1. the invention realizes that the waste phosphorus-rich biomass (including but not limited to fish scales, bones and the like) is used as a raw material, and XO such as phosphate and the like can be quickly obtained4 n-The selective adsorption material with molecular configuration provides a new way for the phosphorus-rich biomass waste.
2. The method has the advantages of simple process, few steps, simple and convenient operation, easy construction of the whole preparation system, easy control of conditions, low cost and easy control of product composition, and is suitable for large-scale industrial production.
3. The invention adopts phosphorus-rich biomass, glutaraldehyde and citric acid as reactants, produces few byproducts in the preparation process, has little pollution to the environment and is an environment-friendly synthesis process.
4. The product of the present invention is XO4 n-Selective adsorption material of structural configuration for XO4 n-The ions have better selective adsorption. Is environment-friendly and can be applied to the effluent PO of the municipal domestic sewage secondary sedimentation tank4 3-Upgrading and transforming for upgrading and removing PO of eutrophic lake4 3-And removing SO from acid mine wastewater4 2-And the like, thereby having wider application prospect.
Drawings
The method for preparing selective adsorption material with phosphorus-rich biomass according to the present invention is further described in detail with reference to the following examples and the accompanying drawings.
Fig. 1 is a photograph of a process of treating fish scales directly with citric acid in comparative example 1.
Fig. 2 is a photograph of the process of treating fish scales using glutaraldehyde-citric acid in example 1 and a photograph of comparison with the method of treating with citric acid and then fixing with glutaraldehyde in comparative example 2.
FIG. 3 is a comparative microscopic electron micrograph of 3 sets of experiments (untreated, fixed with glutaraldehyde and then citric acid, and treated with citric acid and then glutaraldehyde).
FIG. 4 is an electron micrograph of comparative Ca and P distributions from 3 experiments (untreated, fixed with glutaraldehyde and then treated with citric acid, treated directly with citric acid).
FIG. 5 shows the selective adsorption material prepared in example 1 for K2HPO4Electron micrographs of P distribution before and after adsorption.
FIG. 6 shows that the selective adsorbing material prepared in example 1 is for Na2SO4Electron micrographs of S distribution before and after adsorption.
Fig. 7 is a SEM scanning elemental content graph for P, S, Cl and before and after Br adsorption for the selective adsorbent material prepared in example 1.
Detailed Description
Comparative example 1
The fish scales are directly soaked by citric acid.
Fig. 1 is a photograph showing the procedure of directly treating fish scales with citric acid in comparative example, fig. 1A is a photograph of untreated fish scales (as a control), fig. 1B is a photograph of fish scales directly treated with citric acid, and fig. 1C is a photograph of the supernatant of fig. 1B taken and placed in another beaker. Citric acid was added directly to the fish scales and the solids were found to dissolve and still be in a precipitated state (fig. 1B), whereupon the supernatant was poured out into another beaker and was found to quickly become jelly (fig. 1C).
Comparative example 2
Firstly, soaking the fish scales by using citric acid, and then curing collagen by using a glutaraldehyde solution.
Example 1
Glutaraldehyde and citric acid are sequentially utilized to treat fish scales to prepare the selective adsorption material, and the method comprises the following steps:
firstly, putting fish scales (which need to be washed till no blood water) into a container, and then adding a proper amount of 10 volume percent glutaraldehyde solution into the fish scales, wherein the addition amount of the glutaraldehyde solution is at least based on completely immersing the phosphorus-rich biomass;
② soaking for 10 hours at room temperature, then removing supernatant, washing solid with water;
③ adding the solid into the solid according to the mass ratio of the solid to the citric acid of 1: 1 adding citric acid, adding a proper amount of water, stirring and soaking for 10 hours at room temperature;
fourthly, removing supernatant, washing residues with water, and drying at 75 ℃ to obtain the selective adsorption material.
Fig. 2 is a photograph of the process of treating fish scales using glutaraldehyde-citric acid in example 1 and a photograph of comparison with the method of treating with citric acid and then fixing with glutaraldehyde in comparative example 2. Glutaraldehyde is added into the fish scales to directly crosslink and fix the collagen on the sheet-shaped plates on the inner sides of the fish scales (shown in figure 2A); adding citric acid into the A beaker to soak the precipitate (shown in FIG. 2B); the fish scale solids are not obviously dissolved and the fish scale forms are consistent as can be seen from the beakers in fig. 2A and 2B. Fig. 2C shows that the morphology of the fish scales precipitated in the beakers of fig. 2C and fig. 2A and 2B, as well as the supernatant solution, are clearly different when the fish scales are treated with glutaraldehyde (collagen fixation) after the supernatant is discarded after the fish scales are directly treated with citric acid.
For several methods described above, the fish scales are processed, and the associated microstructure morphology is now characterized using electron microscopy, as shown in fig. 3. FIG. 3 is a comparative microscopic electron micrograph of 3 sets of experiments (untreated, fixed with glutaraldehyde and then citric acid, and treated with citric acid and then glutaraldehyde). FIG. 3A is a microscopic electron microscope picture of fish scales without being treated by glutaraldehyde and citric acid; fig. 3B is a microscopic electron microscope picture sequentially treated with glutaraldehyde-citric acid, and fig. 3C is a microscopic electron microscope picture sequentially treated with citric acid and then fixed with glutaraldehyde. As can be seen by comparing fig. 3B and 3C, the scale of fig. 3B has larger and thicker wrinkled corrugations (collagen) than fig. 3C, and fig. 3C shows that collagen fails to fix to the scale after pickling with citric acid and glutaraldehyde fixation.
FIG. 4 is an electron micrograph of comparative Ca and P distributions from 3 experiments (untreated, fixed with glutaraldehyde and then treated with citric acid, treated directly with citric acid). Fig. 4A and 4D are distribution electron micrographs of fish scales themselves, i.e., Ca and P without (glutaraldehyde and citric acid) treatment, respectively, fig. 4B and 4E are distribution pictures of Ca and P after fixing proteins with glutaraldehyde and eluting with citric acid, and fig. 4C and 4F are distribution pictures of Ca and P after directly pickling fish scales with citric acid. The Ca, P content is significantly reduced in FIGS. 4B, 4C compared to FIG. 4A, indicating its removal; and the contents of fig. 4B and 4C are the same, which shows that the effect of removing Ca and P from the fish scales by directly treating with citric acid and treating with glutaraldehyde and then citric acid is the same.
Configuration K2HPO4、Na2SO4KCl, KBr solution, concentration 1% (m/v), soaked in the scale selective adsorption material (prepared in example 1) for 24 hours, then washed with distilled water, dried at 75 ℃, and SEM scanned. FIG. 5 shows the selective adsorption material prepared in example 1 for K2HPO4Electron micrographs of P distribution before and after adsorption. FIG. 6 shows that the selective adsorbing material prepared in example 1 is for Na2SO4Before and after adsorptionS distribution electron micrograph. As can be seen from the electron microscope distribution photographs of FIG. 5 and FIG. 6, the P, S content after adsorption is greatly increased, which illustrates that the selective adsorption material prepared in example 1 can adsorb PO4 3-And SO4 2-Ions.
Fig. 7 is a SEM scanning elemental content graph for P, S, Cl and before and after Br adsorption for the selective adsorbent material prepared in example 1. As can be seen from fig. 7, after 24 hours of soaking, the Cl and Br contents before adsorption (background values) were extremely low, and no significant increase was observed after 24 hours of soaking; like the previous fig. 5 and 6, the P, S content in fish scales is greatly increased. It can be seen that the selective adsorbent material prepared in example 1 is selective for P, S.
And soaking the adsorption material which is adsorbed to saturation with citric acid, and removing phosphate radicals and sulfate radicals by acid washing to regenerate the molecular imprinting material. Therefore, the selective adsorption material can be used for repeatedly adsorbing and desorbing (phosphate radical and sulfate radical ions), so that the selective adsorption material can be circularly and repeatedly utilized, and the phosphate radical and the sulfate radical ions in water can be removed at low cost and high efficiency.
Example 2
Firstly, putting fish scales (which need to be washed till no blood water) into a container, and then adding a proper amount of 5 volume percent glutaraldehyde solution into the fish scales, wherein the addition amount of the glutaraldehyde solution is at least based on completely immersing the phosphorus-rich biomass;
② soaking for 15 hours at room temperature, then removing supernatant, washing solid with water;
③ adding the solid into the solid according to the mass ratio of the solid to the citric acid of 1: 1.2 adding citric acid, adding a proper amount of water, stirring and soaking for 15 hours at room temperature;
fourthly, removing supernatant, washing residues with water, and drying at 80 ℃ to obtain the selective adsorption material.
Example 3
Firstly, putting fish scales (which need to be washed till no blood water) into a container, and then adding a proper amount of 15 volume percent glutaraldehyde solution into the fish scales, wherein the addition amount of the glutaraldehyde solution is at least based on completely immersing the phosphorus-rich biomass;
② soaking for 5 hours at room temperature, then removing supernatant, washing solid with water;
③ adding the solid into the solid according to the mass ratio of the solid to the citric acid of 1: 0.8 adding citric acid, adding a proper amount of water, stirring and soaking for 5 hours at room temperature;
fourthly, removing supernatant, washing residues with water, and drying at 70 ℃ to obtain the selective adsorption material.
Example 4
Firstly, taking animal bones (firstly, crushing the animal bones, then, washing the animal bones until no blood exists) and putting the animal bones into a container, and then, adding a proper amount of glutaraldehyde solution with the volume percentage of 15% into the animal bones, wherein the addition amount of the glutaraldehyde solution is at least based on the complete immersion of the phosphorus-rich biomass;
② soaking for 5 hours at room temperature, then removing supernatant, washing solid with water;
③ adding the solid into the solid according to the mass ratio of the solid to the citric acid of 1: 1.2 adding citric acid, adding a proper amount of water, stirring and soaking for 5 hours at room temperature;
fourthly, removing supernatant, washing residues with water, and drying at 80 ℃ to obtain the selective adsorption material.
Example 5
Firstly, taking animal bones (firstly, crushing the animal bones, then, washing the animal bones until no blood exists) and putting the animal bones into a container, then, taking a proper amount of 5 volume percent glutaraldehyde solution and adding the glutaraldehyde solution into the container, wherein the addition amount of the glutaraldehyde solution is at least based on the complete immersion of the phosphorus-rich biomass;
② soaking for 15 hours at room temperature, then removing supernatant, washing solid with water;
③ adding the solid into the solid according to the mass ratio of the solid to the citric acid of 1: 0.8 adding citric acid, adding a proper amount of water, stirring and soaking for 15 hours at room temperature;
fourthly, removing supernatant, washing residues with water, and drying at 70 ℃ to obtain the selective adsorption material.
The foregoing is merely exemplary and illustrative of the principles of the present invention and various modifications, additions and substitutions of the specific embodiments described herein may be made by those skilled in the art without departing from the principles of the present invention or exceeding the scope of the claims set forth herein.
Claims (8)
1. A method for preparing selective adsorption material by using phosphorus-rich biomass is characterized in that collagen of the phosphorus-rich biomass is fixed by glutaraldehyde solution in a cross-linking mode, and then XO combined with the collagen in the phosphorus-rich biomass is removed by citric acid4 n-A conformational molecule, thereby making it specific for XO4 n-A selective adsorbent material in a molecular configuration;
wherein the phosphorus-rich biomass is selected from fish scales or animal bones, and the XO is4 n-The configurational molecule is phosphate radical PO4 3-Sulfate radical SO4 2-。
2. The method of claim 1, wherein the preparation steps are as follows:
firstly, putting the cleaned phosphorus-rich biomass into a container, and then adding a proper amount of glutaraldehyde solution into the container, wherein the addition amount of the glutaraldehyde solution is at least based on the complete immersion of the phosphorus-rich biomass;
② soaking at room temperature, then removing supernatant, washing solid with water;
thirdly, adding citric acid into the solid, adding a proper amount of water, and stirring and soaking at room temperature;
and fourthly, removing supernatant, washing residues with water, and drying to obtain the selective adsorption material.
3. The method of claim 2, wherein said phosphorus-rich biomass is selected from the group consisting of fish scales that need to be washed to be bloodless.
4. The method of claim 2, wherein the phosphorus-rich biomass is selected from the group consisting of animal bone, which is first comminuted and then the animal bone powder is washed free of blood water.
5. The process according to claim 2, wherein the glutaraldehyde solution in step (i) is present in a percentage by volume of between 5% and 15%.
6. The method of claim 2, wherein the soaking time in step (ii) and the stirring and soaking time in step (iii) are both 5 to 15 hours.
7. The method of claim 2, wherein the mass ratio of the solid to the citric acid in step (c) is 1: 0.8-1.2.
8. The method of claim 2, wherein the drying temperature in step (iv) is 70-80 ℃.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102228824A (en) * | 2011-06-24 | 2011-11-02 | 武汉工业学院 | Preparation method, application and regeneration usage method of freshwater fish scale adsorbent |
| WO2012107022A3 (en) * | 2011-02-08 | 2012-10-11 | Universität Rostock | Method for purifying biogas, flue gas or liquids, adsorbent therefor, filters, and use of the adsorbent |
| CN105968275A (en) * | 2016-04-29 | 2016-09-28 | 江苏大学 | Preparation method and use of phosphate anion surface imprinted polymer |
| CN106219657A (en) * | 2016-08-01 | 2016-12-14 | 华南理工大学 | A kind of modified biomass adsorbent and its preparation method and application |
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| JP2017119230A (en) * | 2015-12-28 | 2017-07-06 | Jnc株式会社 | Adsorbent and method for producing the same |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012107022A3 (en) * | 2011-02-08 | 2012-10-11 | Universität Rostock | Method for purifying biogas, flue gas or liquids, adsorbent therefor, filters, and use of the adsorbent |
| CN102228824A (en) * | 2011-06-24 | 2011-11-02 | 武汉工业学院 | Preparation method, application and regeneration usage method of freshwater fish scale adsorbent |
| CN105968275A (en) * | 2016-04-29 | 2016-09-28 | 江苏大学 | Preparation method and use of phosphate anion surface imprinted polymer |
| CN106219657A (en) * | 2016-08-01 | 2016-12-14 | 华南理工大学 | A kind of modified biomass adsorbent and its preparation method and application |
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