CN108341459B - Method for removing phosphorus in water body through adsorption of alkali lignin modified by nano lanthanum oxide - Google Patents
Method for removing phosphorus in water body through adsorption of alkali lignin modified by nano lanthanum oxide Download PDFInfo
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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
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- 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
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- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
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Abstract
The invention discloses a method for removing phosphorus in a water body by adsorbing alkali lignin modified by nano lanthanum oxide, which comprises the steps of dissolving the alkali lignin in water, adding polyethyleneimine and a formaldehyde solution, and carrying out a Mannich reaction in an alkaline environment; the obtained product is subjected to hydrothermal reaction in an ethanol water solution by taking lanthanum chloride as a lanthanum source to prepare alkali lignin modified by nano lanthanum oxide; adding the alkali lignin modified by the nano lanthanum oxide into a phosphorus-containing water body, and adsorbing and removing phosphorus in the water body. According to the invention, highly dispersed active lanthanum adsorption sites exist on the surface of lanthanum oxide modified alkali lignin prepared by a hydrothermal method, so that the lanthanum oxide modified alkali lignin has a remarkably excellent phosphorus removal effect and a high cyclic utilization rate; the adsorption time is short, and the treatment efficiency is high; the adopted matrix material alkali lignin is waste residue of the papermaking pulping process, has wide source and low price, and can realize the purpose of treating waste by waste. The method is applied to removing the phosphorus in the water body and has good economic and environmental benefits.
Description
Technical Field
The invention belongs to the technical field of water treatment, relates to a method for removing orthophosphate in a water body, and particularly relates to a method for removing orthophosphate in water by utilizing adsorption of an alkali lignin material modified by nano lanthanum oxide.
Background
Phosphorus is one of the limiting nutrient elements causing eutrophication of various types of surface water bodies. The excessive discharge of phosphorus poses great threats to water quality safety and aquatic organisms on the one hand, and aggravates the shortage of non-renewable resources of phosphorus on the other hand. There are three main forms of phosphorus present in natural waters and wastewater, namely orthophosphates, polymeric phosphates (including pyrophosphates, metaphosphates and polyphosphates) and organically bound phosphates. The three forms of phosphorus have certain conversion, polyphosphate can be hydrolyzed into orthophosphate under acidic condition, and organophosphorus can be mineralized into orthophosphate under the action of biological enzyme secreted by bacterial cells. Therefore, there is much concern about the removal of orthophosphate from bodies of water.
The adsorption method becomes a research hotspot as a water treatment method with high efficiency and low energy consumption, and the adsorption method for removing the phosphorus in the water body has the advantages of low cost, good effect, capability of recycling phosphorus resources and the like. The adsorption dephosphorization process is simple and reliable in operation, and can be used as an advanced treatment method for biological dephosphorization and also can be used as an independent treatment unit. Currently, the common phosphorus removal adsorbents include activated carbon, fly ash, steel slag, metal oxides, composite materials thereof and the like.
Researches find that the rare earth element lanthanum has excellent adsorption selectivity to phosphorus, for example, after zeolite is modified by lanthanum, the adsorption capacity to phosphorus is increased by nearly 10 times, and the phosphorus removal efficiency can reach 99% to the maximum; after the clay mineral is modified by lanthanum oxide, the phosphorus removal effect is greatly improved from 6.75-37.70% before modification to 93.18-99.44%. However, lanthanum oxide has a small diameter and tends to aggregate in water, thereby causing mass transfer resistance and reducing the adsorption capacity.
The alkali lignin is also called lignosulfonate, is a renewable biomass resource and is derived from residues in the pulping industry of a paper-making sulfate method; the lignin molecule surface contains rich oxygen-containing functional groups, which is beneficial to carrying out chemical modification on the surface. About 5000 million tons of industrial lignin byproducts are separated from plants every year in the pulping and papermaking industry, and the resource efficient utilization of the industrial lignin not only provides raw materials for the chemical industry, but also has great significance for promoting the development of resource ecological utilization. Therefore, the resource utilization of the industrial lignin has great economic and environmental benefits.
The alkali lignin is subjected to lanthanum oxide modification treatment and then applied to the adsorption removal of phosphorus in a water body, and no relevant report is found at present. In order to widen the application field of lignin biomass resources, accelerate high-value utilization of lignin which is a main component of papermaking residues, and realize sustainable development and green environmental protection, lanthanum oxide is loaded on the surface of alkali lignin and used for adsorbing and removing orthophosphate in a water body.
Disclosure of Invention
1. Technical problem to be solved
Aiming at the defects of limited available effective active adsorption sites, long adsorption time and low phosphorus removal adsorption amount of lanthanum oxide, the invention aims to provide a method for removing phosphorus in a water body by using nano lanthanum oxide modified alkali lignin as an adsorbent.
2. Technical scheme
The method for removing phosphorus in the water body by adsorbing the alkali lignin modified by the nano lanthanum oxide takes the alkali lignin modified by the nano lanthanum oxide as an adsorbent, and can quickly and efficiently adsorb and remove orthophosphate in the water body.
The method for removing phosphorus in the water body by adsorbing the alkali lignin modified by the nano lanthanum oxide comprises the following steps:
step 1, grafting alkali lignin on polyethyleneimine:
alkali lignin is added into the mixture according to the mass volume ratio of 1 g: (20-40) ml of the reaction product is dissolved in water, polyethyleneimine and formaldehyde are sequentially added, the pH of the solution is adjusted to 10.0-11.0, the solution is uniformly stirred and then subjected to Mannich reaction, the reaction product is cooled and washed by water to be neutral, and the reaction product is dried to be constant in weight to obtain polyethyleneimine grafted alkali lignin;
step 2, preparing the alkali lignin modified by the nano lanthanum oxide:
dispersing the alkali lignin grafted by the polyethyleneimine prepared in the step (1) into an ethanol water solution, adding lanthanum oxide or a hydrate thereof, adjusting the pH of the solution to 10.0-11.0, carrying out hydrothermal reaction, cooling a reaction product, fully washing with water, and drying in vacuum to prepare nano lanthanum oxide modified alkali lignin;
and (3) adding the alkali lignin modified by the nano lanthanum oxide prepared in the step (2) into a water body to be treated, and adsorbing to remove orthophosphate.
In the method for removing phosphorus in a water body by adsorbing alkali lignin modified by nano lanthanum oxide, in the Mannich reaction in the step 1, the mass ratio of the alkali lignin to polyethyleneimine to formaldehyde is 1 (0.5-1): (0.5 to 1).
In the method for removing phosphorus in the water body by adsorbing the alkali lignin modified by the nano lanthanum oxide, the temperature of the Mannich reaction in the step 1 is 40-60 ℃, and the reaction time is 20-24 hours.
In the method for removing phosphorus in the water body by adsorbing the alkali lignin modified by the nano lanthanum oxide, the ethanol aqueous solution in the step 2 is prepared by mixing absolute ethanol and deionized water in a ratio of 1: 3-1: 5 (v/v).
In the method for removing phosphorus in a water body by adsorbing alkali lignin modified by nano lanthanum oxide, in the hydrothermal reaction in the step 2, the mass ratio of the alkali lignin grafted by polyethyleneimine to the lanthanum chloride is 1 (1-1.5), preferably, the alkali lignin is reacted for 3-5 h at the reaction temperature of 40-60 ℃, and then the reaction is continued for 20-24 h at room temperature.
In the method for removing phosphorus in the water body by adsorbing the alkali lignin modified by the nano lanthanum oxide, the pH of the adjusting solution is preferably adjusted by using 20 wt.% sodium hydroxide solution.
In the method for removing phosphorus in the water body by adsorbing the alkali lignin modified by the nano lanthanum oxide, the concentration of orthophosphate contained in the water body to be treated in the step 3 is 30-120 Pmg/L.
In the method for removing phosphorus in the water body by adsorbing the alkali lignin modified by the nano lanthanum oxide, the mass ratio of the alkali lignin modified by the adsorbent nano lanthanum oxide to the phosphate-containing water body in the step 3 is 1: 800-2000.
In the method for removing phosphorus in the water body by adsorbing the alkali lignin modified by the nano lanthanum oxide, the adsorption time in the step 3 is 5-10 hours, and the adsorption temperature is 25-45 ℃.
3. Advantageous effects
Compared with the prior art, the invention has the advantages that:
1. the surface of the lanthanum oxide modified alkali lignin prepared by a hydrothermal method has highly dispersed active lanthanum adsorption sites; adsorption experiments show that the alkali lignin adsorbent modified by lanthanum oxide has a remarkable adsorption effect on phosphorus, and the effect is remarkably increased compared with that before modification. Compared with the adsorbent in the prior art, the adsorption effect is obviously improved, and the phosphorus adsorption amount is 85.47mg P/g (namely 162.2mg P g) under the same condition-1(La)) was significantly better than lanthanum hydroxide (72.80mg P g)-1(La)), zeolite supported lanthanum (24)6mg P/g) and bentonite-supported lanthanum (14.0mg P/g).
2. In the prior art, the lanthanum-loaded adsorbing material has the defects of less lanthanum at active adsorption sites and low utilization rate; according to the invention, polyethyleneimine is grafted to the surface of alkali lignin by adopting a Mannich reaction, and lanthanum oxide is anchored on abundant amino groups on the surface of the material by a hydrothermal method, so that the prepared active lanthanum exists in a nano La-OH or La-O form and can be uniformly distributed on the surface of the material, more adsorption sites are exposed, the mass transfer process is promoted, and the adsorption effect is greatly improved.
3. Research shows that the alkali lignin modified by the nano lanthanum oxide can quickly adsorb phosphorus in a water body, and the removal efficiency of the phosphorus can be effectively improved by raising the temperature; the extent to which the adsorbent material is affected by the ionic strength of the aqueous solution is negligible.
4. The base material alkali lignin in the adsorbent adopted by the invention is a biomass material which is renewable, has wide source, is waste residue of papermaking pulping process and has low price; the treatment effect on phosphorus is obvious after the lanthanum oxide is modified.
5. In addition, the method has mild adsorption treatment conditions and short time consumption, and can greatly improve the water treatment efficiency. Therefore, the alkali lignin modified by the nano lanthanum oxide is applied to adsorption removal of phosphorus in water, and has good economic and environmental benefits.
Drawings
Fig. 1 is a fourier infrared spectrum of alkali lignin before and after lanthanum oxide modification.
As shown in the figure, the lignin content at 1656cm after grafting of Polyethyleneimine (PEI) compared to the Alkali Lignin (AL) before modification-1And 1599cm-1Obvious vibration peak of amide group and 1125cm appear-1The C-N stretching vibration peak appears, and the result shows that PEI has been successfully grafted to AL; for alkali lignin (AL-PEI-La) modified by lanthanum oxide, 3609cm-1And 647cm-1The obvious hydroxyl characteristic peak of lanthanum hydroxide appears, and meanwhile, the pure La (OH)3The same characteristic peak was observed at the same position, and the result showed that La (OH)3Have been successfully sequestered on the surface of materials.
Detailed Description
The present invention will be described in detail with reference to specific embodiments. In the specific embodiment, alkali lignin modified by lanthanum oxide is used as an adsorbent to adsorb and remove phosphorus in a water body, and a static batch treatment process is adopted for adsorption. However, the present invention is not limited to the specific embodiments described in the examples, and any person skilled in the art can modify or change the technical content disclosed within the scope of the present invention, so as to obtain the embodiments or methods with substantially the same effect. However, any modification, equivalent or equivalent changes and modifications of the embodiments described above are within the scope of the technical solution of the present invention without departing from the spirit of the technical solution of the present invention. It is intended that the scope of the invention be limited not by this detailed description, but rather by the claims appended hereto.
Example 1
The method for removing phosphorus in the water body by adsorbing the alkali lignin modified by the nano lanthanum oxide comprises the following steps:
step 1, dissolving 5.0g of alkali lignin in 100mL of aqueous solution, adding 4.0g of polyethyleneimine (PEI, 99 wt.%) and 4.0g of formaldehyde (37 wt.%), adjusting the pH of 20 wt.% of sodium hydroxide solution to 10.0-11.0, uniformly stirring, heating to 50 ℃, reacting for 24 hours, carrying out suction filtration, washing for multiple times until the solution is neutral, and carrying out vacuum drying at 60 ℃ until the solution is constant in weight to obtain alkali lignin grafted polyethyleneimine, which is marked as AL-PEI.
Step 2, adding 2.0g of AL-PEI into 100mL of a mixed solution of absolute ethyl alcohol and distilled water (v/v is 1:4), adding 3.71g of lanthanum chloride heptahydrate, adjusting the pH value of a 20 wt.% sodium hydroxide solution to 10.0-11.0, reacting at 60 ℃ for 3h, continuing to react at room temperature for 24h, cooling the reaction product, fully washing with water, and drying in vacuum to obtain nano lanthanum oxide modified alkali lignin, which is marked as AL-PEI-La.
And 3, adsorbing and treating the phosphorus-containing water body by using the nano lanthanum oxide modified alkali lignin AL-PEI-La synthesized in the step 2 as an adsorbent. The specific adsorption treatment process is as follows: performing static adsorption in a 40mL EPA bottle with a polytetrafluoroethylene gasket, wherein the mass ratio of the adsorbent to the phosphate-containing water body is 1:2000, the pH value is 6.0, the initial concentration of phosphorus is 39.27mg P/L, NaCl is not contained in the water body, the adsorption temperature is 25 ℃, and the adsorption time is 10 h. After the adsorption equilibrium, the filtrate was filtered through a 45. mu.L aqueous filter, and the concentration of phosphorus in the filtrate was measured at 700nm by molybdenum blue colorimetry. The adsorbed amount (in terms of phosphorus) was found to be 31.54mg P/g.
Comparative example 2
And (3) adsorbing and treating the phosphorus-containing water body by using the alkali lignin grafted polyethyleneimine AL-PEI synthesized in the example 1 as an adsorbent. The adsorption conditions were the same as in example 1, and the phosphorus adsorption amount was found to be 12.73mg P/g.
Comparative example 3
And (3) adsorbing and treating the phosphorus-containing water body by using the alkali lignin in the example 1 as an adsorbent. The adsorption conditions were the same as in example 1, and the amount of phosphorus adsorbed was 0.17mg of P/g.
Therefore, the lanthanum oxide loaded with the active component can effectively improve the removal effect of phosphorus in the water body.
Example 4
The preparation method of the alkali lignin adsorbent modified by the nano lanthanum oxide comprises the following steps:
step 1, dissolving 5.0g of alkali lignin in 100mL of aqueous solution, adding 5.0g of polyethyleneimine (PEI, M.W.10000, 99 wt.%) and 5.0g of formaldehyde (37 wt.%) aqueous solution, adjusting the pH of 20 wt.% of sodium hydroxide solution to 10.0-11.0, uniformly stirring, heating to 50 ℃, reacting for 24 hours, carrying out suction filtration, washing for multiple times to neutrality, and carrying out vacuum drying at 60 ℃ to constant weight to obtain alkali lignin grafted polyethyleneimine, wherein the mark is AL-PEI.
Step 2, adding 2.0g of AL-PEI into 100mL of a mixed solution of absolute ethyl alcohol and distilled water (v/v is 1:4), adding 4.90g of lanthanum chloride heptahydrate, adjusting the pH value of a 20 wt.% sodium hydroxide solution to 10.0-11.0, reacting at 60 ℃ for 3h, continuing to react at room temperature for 24h, cooling the reaction product, fully washing with water, and drying in vacuum to obtain nano lanthanum oxide modified alkali lignin, which is marked as AL-PEI-La.
Example 5
And (3) adsorbing and treating the phosphorus-containing water body by using the nano lanthanum oxide modified alkali lignin AL-PEI-La synthesized in the example 1 as an adsorbent. The initial concentration of phosphorus was 46.72mg P/L, the change of the adsorption amount with the adsorption time was studied under the same other adsorption conditions as in example 1, and the experimental result showed that the time for the adsorption to reach equilibrium was 60min and the equilibrium adsorption amount was 37.28mg P/g.
It can be seen that compared with the time for other adsorbents reported in the literature to reach adsorption equilibrium (ACF-LaFe (120min) (Chemical Engineering Journal,2013,215-216,859-867.), ACF-LaOH (360min) (Chemical Engineering Journal,2012, 185-186, 160-167), MFC @ La (OH) (240min) (Chemical Engineering Journal,2018,335,443-449.), lanthanum-loaded ordered mesoporous hollow silicon spheres (1440min) (Journal of Materials Chemistry A,2014,2, 8839-8848)), the adsorbent can realize rapid and efficient capture of phosphorus in water body, and has remarkably superior performance.
Example 6
The preparation method of the alkali lignin modified by the nano lanthanum oxide is the same as that of the example 1, the adsorption conditions are basically the same as that of the example 1, and the difference is that the adsorption temperature is 35 ℃, and the final adsorption amount of the adsorbent to phosphorus is 32.52mg P/g.
Example 7
The preparation method of the alkali lignin modified by the nano lanthanum oxide is the same as that of the example 1, the adsorption conditions are basically the same as that of the example 1, and the difference is that the adsorption temperature is 45 ℃, and the phosphorus adsorption amount of the final adsorbent is 37.37mg P/g.
Therefore, the adsorption temperature is 25-45 ℃, the removal effect is good, and the adsorption temperature is improved, so that the phosphate can be adsorbed and removed.
Example 8
The preparation method of the nano lanthanum oxide modified alkali lignin is the same as that in example 1, and the adsorption conditions are basically the same as that in example 1, except that the phosphorus-containing water body contains 0.01mol/L NaCl, and the adsorption removal amount of phosphate is 31.60 mgP/g.
Example 9
The preparation method of the nano lanthanum oxide modified alkali lignin is the same as that in example 1, and the adsorption conditions are basically the same as that in example 1, except that the phosphorus-containing water body contains 0.1mol/L NaCl, and the adsorption removal amount of phosphate is 31.75mg P/g.
Therefore, the ionic strength in the water body has little influence on the adsorption and phosphorus removal of the alkali lignin modified by the nano lanthanum oxide.
Example 10
The preparation method of the nano lanthanum oxide modified alkali lignin is the same as that of example 1, and the adsorption conditions are basically the same as that of example 1, except that the initial concentration of phosphorus is 97.35mg P/L, and the adsorption removal amount of phosphate is 68.12mg P/g.
Example 11
In the same way as in example 10, the phosphorus-containing water contained 100mg/L of CO3 2-The amount of adsorbed phosphate removed was 67.34mg P/g.
Example 12
In the same way as in example 10, the phosphorus-containing water contained 200mg/L of CO3 2-The amount of adsorbed phosphate removed was 65.13mg P/g.
Example 13
In the same manner as in example 10, the phosphorus-containing water contained 300mg/L of CO3 2-The amount of adsorbed phosphate removed was 64.05mg of P/g.
It can be seen that the removal amount of phosphorus by adsorption of the adsorbent is dependent on CO3 2-The concentration is increased and slightly decreased, but the effect is not great.
Example 14
The preparation method of the alkali lignin modified by the nano lanthanum oxide is the same as the example 4, the adsorption condition is the same as the example 10, wherein the phosphorus-containing water body contains 100mg/L of HCO3 -The amount of adsorbed phosphate removed was 67.42mg P/g.
Example 15
In the same manner as in example 14, the phosphorus-containing water body contains 200mg/L of HCO3 -The amount of adsorbed phosphate removed was 65.72mg P/g.
Example 16
In the same manner as in example 14, the phosphorus-containing water contained 300mg/L of HCO3 -The amount of adsorbed phosphate removed was 63.50mg P/g.
It can be seen that the removal amount of phosphorus by adsorption of the adsorbent depends on HCO3 -The concentration is increased and slightly decreased, but the effect is not great.
Example 17
In the same manner as in example 10, the phosphorus-containing water contained 100mg/L SO4 2-The amount of adsorbed phosphate removed was 67.67mg of P/g.
Example 18
In the same manner as in example 10, the phosphorus-containing water contained 200mg/L SO4 2-The amount of adsorbed phosphate removed was 66.85mg P/g.
Example 19
In the same manner as in example 10, the phosphorus-containing water contained 300mg/L SO4 2-The amount of adsorbed phosphate removed was 64.43mg P/g.
It can be seen that the removal amount of the phosphorus by the adsorbent depends on the SO4 2-The concentration is increased and slightly decreased, but the effect is not great.
Claims (7)
1. A method for removing phosphorus in a water body by adsorbing alkali lignin modified by nano lanthanum oxide comprises the following steps:
step 1, grafting alkali lignin on polyethyleneimine:
alkali lignin is added into the mixture according to the mass volume ratio of 1 g: (20-40) ml of the reaction product is dissolved in water, polyethyleneimine and formaldehyde are sequentially added, the pH of the solution is adjusted to 10.0-11.0, the solution is uniformly stirred and then subjected to Mannich reaction, the reaction product is cooled and washed by water to be neutral, and the reaction product is dried to be constant in weight to obtain polyethyleneimine grafted alkali lignin;
step 2, preparing the alkali lignin modified by the nano lanthanum oxide:
dispersing the alkali lignin grafted by the polyethyleneimine prepared in the step (1) into an ethanol water solution, adding lanthanum oxide or a hydrate thereof, adjusting the pH of the solution to 10.0-11.0, carrying out hydrothermal reaction, cooling a reaction product, fully washing with water, and drying in vacuum to prepare nano lanthanum oxide modified alkali lignin;
step 3, adsorbing and removing phosphorus:
and (3) adding the alkali lignin modified by the nano lanthanum oxide prepared in the step (2) into a water body to be treated, and adsorbing to remove orthophosphate.
2. The method for removing phosphorus in water through adsorption of alkali lignin modified by nano lanthanum oxide according to claim 1, wherein the Mannich reaction temperature in step 1 is 40-60 ℃ and the reaction time is 20-24 h.
3. The method for removing phosphorus in a water body through adsorption of alkali lignin modified by nano lanthanum oxide according to claim 1, wherein the ethanol aqueous solution in the step 2 is prepared from absolute ethanol and deionized water in a ratio of 1: 3-1: 5 v/v.
4. The method for removing phosphorus in a water body through adsorption of nano lanthanum oxide modified alkali lignin according to claim 1, wherein in the hydrothermal reaction in the step 2, the mass ratio of the alkali lignin grafted with polyethyleneimine to the lanthanum chloride is 1 (1-1.5), the alkali lignin is reacted at the reaction temperature of 40-60 ℃ for 3-5 hours, and then the reaction is continued at room temperature for 20-24 hours.
5. The method for removing phosphorus in water through adsorption of alkali lignin modified by nano lanthanum oxide according to claim 1, wherein the concentration of orthophosphate contained in the water to be treated in the step 3 is 30-120 Pmg/L.
6. The method for removing phosphorus in water through adsorption of nano lanthanum oxide modified alkali lignin according to claim 1, wherein the mass ratio of the adsorbent nano lanthanum oxide modified alkali lignin to the phosphate-containing water in the step 3 is 1: 800-2000.
7. The method for removing phosphorus in water through adsorption of alkali lignin modified by nano lanthanum oxide according to claim 1, wherein the adsorption time in step 3 is 5-10 hours, and the adsorption temperature is 25-45 ℃.
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| CN104437396B (en) * | 2014-11-04 | 2017-03-22 | 广西大学 | Preparation method of lignin-amine microsphere |
| CN104984744B (en) * | 2015-06-02 | 2017-05-17 | 中山大学 | Plant fiber based solid amine adsorption material, preparation method and application thereof |
| CN105214629A (en) * | 2015-10-30 | 2016-01-06 | 南京信息工程大学 | A kind of biomass-based nano lanthanum oxide dephosphorization compound adsorbent and preparation method thereof |
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2018
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