CN109912755A - A kind of fulvic acid type three-dimensional network composite material and preparation method and application - Google Patents
A kind of fulvic acid type three-dimensional network composite material and preparation method and application Download PDFInfo
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Abstract
The invention discloses a kind of fulvic acid type three-dimensional network composite material and preparation method and applications, belong to material preparation and technical field of environmental management.Using fulvic acid, natural macromolecular, crosslinking agent and initiator are added after dissolution, polyethylene glycol is added dropwise in a heated condition, by stirring, drying, fulvic acid type three-dimensional network composite material is made.Since fulvic acid is the polymeric organic acid being made of aromatic series and its a variety of functional groups, natural degradable has the function of good physiological activity and absorption absorption, complexing, exchange etc..The porous structure of formation can enhance the absorption or complexing to heavy metal ion particulate matter.When the composite material is used for pollution control, restoration of the ecosystem, it can be alternatively arranged as soil and fertilizer after the completion of adsorbing with the heavy metal in adsorbed water body and soil, improve soil texture, restore the ecological balance, reduce chemical contamination.
Description
Technical field
The invention belongs to material preparation and technical field of environmental management, and in particular to a kind of fulvic acid type three-dimensional network is compound
Material and its preparation method and application.
Background technique
In recent years, the improvement of water body and soil pollution was the serious problem of facing mankind, since pollutant kind is more multiple
Miscellaneous, the content difference in water body or soil is larger, this just adsorption efficiency to the adsorbent during pollution control, adsorption bar
More stringent requirements are proposed for the performances such as part, absorption range.At present using wide chitosan class macromolecule resin adsorbent by
In having a single function, specific surface area is limited, effectively remove water body or the efficiency of soil heavy metal ion and organic pollutant is more low
Problem limits large-scale industrialization application.Therefore a kind of green porosity water-absorbing-retaining multi-functional cure of high activity is prepared
Agent is current problem urgently to be resolved to handle the polluter in water body or soil.
Summary of the invention
To solve the above-mentioned problems, the purpose of the present invention is to provide a kind of fulvic acid type three-dimensional network composite material and its
Preparation method and application, the preparation method simple process, raw material are easy to get, at low cost, it can be achieved that large-scale production；Through our legal system
The fulvic acid type three-dimensional network composite material obtained has good adsorptivity and water-absorbing-retaining performance.By the fulvic acid type three dimensional network
When network composite material is used for pollution control, restoration of the ecosystem, soil texture can be improved, administer water source, restore the ecological balance, reduced
Chemical contamination.
The present invention is to be achieved through the following technical solutions:
The invention discloses a kind of methods of fulvic acid type three-dimensional network composite material, are divided into following steps:
1)/measurement mass parts ratio is referred to as (1.0~6.0): (0.3~1.0): the fulvic acid of (2.0~12.0), natural big
Molecule and acrylic acid；
2) a certain amount of crosslinking agent and initiator is completely soluble in water, obtained solution A；
3) respectively that fulvic acid, natural macromolecular difference is completely soluble in water, obtain fulvic acid solution and natural macromolecular
Dispersion liquid is stirred and from room temperature after mixing fulvic acid solution, natural macromolecular dispersion liquid with the liter of 2~4 DEG C/min
Warm speed is warming up to 55~65 DEG C；
4) acrylic acid and solution A are added dropwise into the reaction system of step 3), continues to heat, with the heating speed of 2~4 DEG C/min
Degree is warming up to 75~80 DEG C, and stirring to system becomes gel and stops reaction, takes out product and is dried, obtains fulvic acid type three
Tie up net composites.
Preferably, initiator is potassium peroxydisulfate or ammonium persulfate, and dosage is the 0.5%~4.5% of fulvic acid dosage.
Preferably, crosslinking agent N, N- methylene-bisacrylamide or N methyldiethanol amine, dosage are fulvic acid dosage
0.5%~1.0%.
Preferably, in step 4), the time for adding of acrylic acid is 30~40min.
Preferably, in step 4), the time that solution A is added dropwise is 35~45min.
Preferably, in step 4), acrylic acid before dropwise addition under the conditions of 0 DEG C of ice-water bath in aqueous slkali and, degree of neutralization is
20%~80%.
Preferably, when temperature≤65 DEG C of reaction system, mixing speed is 120~160r/min；When reaction system
At 65 DEG C of temperature >, mixing speed is 100~120r/min.
Preferably, water is deionized water or distilled water.
The invention also discloses the fulvic acid type three-dimensional network composite materials using above method preparation.
The invention also discloses obtained fulvic acid type three-dimensional network composite materials in terms of pollution control, restoration of the ecosystem
Application.
Compared with prior art, the invention has the following beneficial technical effects:
The preparation method of fulvic acid type three-dimensional network composite material of the invention uses fulvic acid, natural macromolecular, dissolution
Crosslinking agent and initiator are added afterwards, polyethylene glycol is added dropwise in a heated condition, by stirring, drying, it is three-dimensional that fulvic acid type is made
Net composites.Fulvic acid is widely present in soil, lake, river, ocean and peat (also known as turf), lignite, weathering
In coal.This method is easy to operate, raw material is easy to get, low for equipment requirements, at low cost.Fulvic acid is to pollutant and dyestuff and heavy metal
The suction-operated of ion etc., but adsorption efficiency is limited, and adsorption site is indefinite.It is modified through natural macromolecular, there is ammonia
The chief actives unit structure such as base, hydroxyl, can remove includes the pollutants such as heavy metal, dyestuff, anion, and the porous knot formed
Structure can enhance the absorption or complexing to heavy metal ion particulate matter.The preparation method simple process, raw material are easy to get, cost
It is low, it can be achieved that large-scale production.
Further, the time for adding for controlling acrylic acid is 30~40min, prevents propylene hyper acid and it is anti-to generate autohemagglutination
It answers.
Further, the time that control solution A is added dropwise is 35~45min, and preventing a large amount of initiator moments from causing causes certainly
Implode reaction is excessively generated by base.
Further, when temperature≤65 DEG C of reaction system, mixing speed is 120~160r/min；Work as reaction system
65 DEG C of temperature > when, mixing speed is 100~120r/min, and when temperature≤65 DEG C of reaction system, quickly stirring makes to react
Object is sufficiently mixed, and at 65 DEG C of the temperature > of reaction system, reducing mixing speed prevents auto-acceleration effect.
Using fulvic acid type three-dimensional network composite material made from this method, since fulvic acid is by aromatic series and its a variety of
The polymeric organic acid that functional group is constituted, natural degradable have good physiological activity and absorption absorption, complexing, exchange etc.
Function.The porous structure of formation can enhance the absorption or complexing to heavy metal ion particulate matter.
It, can be with adsorbed water body and soil when the fulvic acid type three-dimensional network composite material is used for pollution control, restoration of the ecosystem
Heavy metal in ground is alternatively arranged as soil and fertilizer after the completion of absorption, improve soil texture, restores the ecological balance, and it is dirty to reduce chemistry
Dye.
Specific embodiment
Below with reference to specific embodiment, the present invention is described in further detail, it is described be explanation of the invention and
It is not to limit.
Fulvic acid used is mainly extracted from weathered coal or lignite in embodiment, and natural products macromolecular can be poly- using shell
Sugar or cellulose.Chitosan (CTS) is polysaccharide natural macromolecular made of being coupled as very more cycloaliphatic ring and ehter bond.Ammonia
Base, hydroxyl also can remove multiple pollutant, including heavy metal, dyestuff, anion etc. as chief active unit structure, and
No matter all very considerable to the physical absorption of pollutant or chemisorption effect this adsorbent is, also certain desorption ability,
It can be used as the modifying agent of fulvic acid adsorbent.The reaction mechanism is as follows:
Embodiment 1:
Weigh 1 part of fulvic acid, 0.3 part of chitosan is added in three-necked flask, and 60 parts of distilled water are added, open agitating device with
The rate of 120r/min is stirred, while being warming up to 55 DEG C from room temperature with the heating rate of 2 DEG C/min；It instills in advance 0
It is neutralized under the conditions of DEG C ice-water bath with KOH, degree of neutralization is 5.5 parts of acrylic acid of 20%, and control time for adding is 30min；Then again
It is added dropwise by 0.005 part of potassium peroxydisulfate and 0.005 part of N, N- methylene-bisacrylamide is dissolved in 15 parts of distilled water and solution is made, control
Time for adding is 35min；Then proceed to be warming up to 80 DEG C with the heating rate of 2 DEG C/min, then with the rate of 100r/min into
Row stirring stops reaction when reaction is sticky difficult in gel stirring to system, product is taken out and is dried at 80 DEG C,
Obtain fulvic acid type three-dimensional network composite material.
Embodiment 2:
Weigh 2 parts of fulvic acids, 0.5 part of cellulose is added in three-necked flask, and 70 parts of distilled water are added, open agitating device with
The rate of 160r/min is stirred, while being warming up to 65 DEG C from room temperature with the heating rate of 4 DEG C/min；It instills in advance 0
It is neutralized under the conditions of DEG C ice-water bath with NaOH, degree of neutralization is 7.5 parts of acrylic acid of 80%, and control time for adding is 40min；Then again
Dropwise addition is dissolved in 15 parts of distilled water by 0.09 part of ammonium persulfate and 0.02 part of N methyldiethanol amine and solution is made, and controls time for adding
For 45min；It then proceedes to be warming up to 75 DEG C with the heating rate of 4 DEG C/min, be then stirred with the rate of 120r/min, when
Reaction stops reaction when sticky difficult in gel stirring to system, and product is taken out and is dried at 80 DEG C, yellow corruption is obtained
Acid type three-dimensional network composite material.
Embodiment 3:
Weigh 3 parts of fulvic acids, 0.5 part of cellulose is added in three-necked flask, and 80 parts of distilled water are added, open agitating device with
The rate of 140r/min is stirred, while being warming up to 60 DEG C from room temperature with the heating rate of 3 DEG C/min；It instills in advance 0
It is neutralized under the conditions of DEG C ice-water bath with KOH, the acrylic acid 75g that degree of neutralization is 60%, control time for adding is 40min；Then it drips again
Add and 15 parts of distilled water are dissolved in by 0.09 part of potassium peroxydisulfate and 0.03 part of N methyldiethanol amine are made solution, control time for adding is
40min；It then proceedes to be warming up to 80 DEG C with the heating rate of 3 DEG C/min, be then stirred with the rate of 110r/min, when anti-
Stop reaction when should be sticky difficult in gel stirring to system, product is taken out and is dried at 80 DEG C, fulvic acid is obtained
Type three-dimensional network composite material.
Embodiment 4:
Weigh 4 parts of fulvic acids, 0.5 part of cellulose is added in three-necked flask, and 90 parts of distilled water are added, open agitating device with
The rate of 140r/min is stirred, while being warming up to 60 DEG C from room temperature with the heating rate of 3 DEG C/min；It instills in advance 0
It is neutralized under the conditions of DEG C ice-water bath with KOH, degree of neutralization is 8 parts of acrylic acid of 50%, and control time for adding is 40min；Then it drips again
Add by 0.12 part of potassium peroxydisulfate and 0.04 part of N, N- methylene-bisacrylamide is dissolved in 15 parts of distilled water and solution is made, and control is added dropwise
Time is 40min；It then proceedes to be warming up to 80 DEG C with the heating rate of 3 DEG C/min, then be stirred with the rate of 110r/min
It mixes, stops reaction when reaction is sticky difficult in gel stirring to system, product is taken out and is dried at 80 DEG C, is obtained
Fulvic acid type three-dimensional network composite material.
Embodiment 5:
Weigh 5 parts of fulvic acids, 0.5 part of cellulose is added in three-necked flask, and 100 parts of distilled water are added, open agitating device
It is stirred with the rate of 140r/min, while being warming up to 60 DEG C from room temperature with the heating rate of 3 DEG C/min；Instillation exists in advance
It is neutralized under the conditions of 0 DEG C of ice-water bath with KOH, degree of neutralization is 8 parts of acrylic acid of 50%, and control time for adding is 40min；Then it drips again
Add by 0.15 part of potassium peroxydisulfate and 0.05 part of N, N- methylene-bisacrylamide is dissolved in 15 parts of distilled water and solution is made, and control is added dropwise
Time is 40min；It then proceedes to be warming up to 80 DEG C with the heating rate of 3 DEG C/min, then be stirred with the rate of 110r/min
It mixes, stops reaction when reaction is sticky difficult in gel stirring to system, product is taken out and is dried at 80 DEG C, is obtained
Fulvic acid type three-dimensional network composite material.
Embodiment 6:
Weigh 6 parts of fulvic acids, 1 part of cellulose is added in three-necked flask, and 110 parts of distilled water are added, open agitating device with
The rate of 140r/min is stirred, while being warming up to 60 DEG C from room temperature with the heating rate of 3 DEG C/min；It instills in advance 0
It is neutralized under the conditions of DEG C ice-water bath with KOH, degree of neutralization is 12 parts of acrylic acid of 50%, and control time for adding is 40min；Then it drips again
Add by 0.18 part of potassium peroxydisulfate and 0.06 part of N, N- methylene-bisacrylamide is dissolved in 15 parts of distilled water and solution is made, and control is added dropwise
Time is 40min；It then proceedes to be warming up to 80 DEG C with the heating rate of 3 DEG C/min, then be stirred with the rate of 110r/min
It mixes, stops reaction when reaction is sticky difficult in gel stirring to system, product is taken out and is dried at 80 DEG C, is obtained
Fulvic acid type three-dimensional network composite material.
Embodiment 7:
Weigh 4 parts of fulvic acids, 1 part of cellulose is added in three-necked flask, and 140 parts of distilled water are added, open agitating device with
The rate of 140r/min is stirred, while being warming up to 60 DEG C from room temperature with the heating rate of 3 DEG C/min；It instills in advance 0
It is neutralized under the conditions of DEG C ice-water bath with KOH, degree of neutralization is 8 parts of acrylic acid of 60%, and control time for adding is 40min；Then it drips again
Add by 0.12 part of potassium peroxydisulfate and 0.04 part of N, N- methylene-bisacrylamide is dissolved in 15 parts of distilled water and solution is made, and control is added dropwise
Time is 40min；It then proceedes to be warming up to 80 DEG C with the heating rate of 3 DEG C/min, then be stirred with the rate of 110r/min
It mixes, stops reaction when reaction is sticky difficult in gel stirring to system, product is taken out and is dried at 80 DEG C, is obtained
Fulvic acid type three-dimensional network composite material.
Effect in order to further illustrate the present invention, the fulvic acid type three-dimensional network obtained to above-described embodiment 1~7 are compound
Material carries out water-absorbing-retaining and absorption property is further studied.
Water-absorbing-retaining experiment and result
The test of fulvic acid type three-dimensional network composite material water-absorbing-retaining performance: 0.5g above-described embodiment 1~7 is weighed respectively
Fulvic acid type three-dimensional network composite material obtained is put into the beaker of 7 500mL, and the tap water of 300g is added and it is allowed to absorb water
Then saturation is filtered with 200 mesh nylon net cloths, after water has been filtered, hydrogel is put into beaker and is weighed.Water absorbent rate is pressed
Formula: Q=(m2-m1)/m1It calculates, Q is water absorbent rate, m1Weight before absorbing water for product, m2For weight after water suction.Test result is shown in
Table 1.
The test of water retention property: fulvic acid type three-dimensional network composite wood made from 0.5g above-described embodiment 1~7 is weighed respectively
Material is put into the beaker of 7 500mL, and the tap water of 300g is added and its water suction is allowed to be saturated, then with 200 mesh nylon net cloth mistakes
Hydrogel after water suction saturation is put into beaker by filter, dry under natural conditions, daily the weight of measurement of same time hydrogel
It changes with time, water retention presses q=Q/Qmax× 100% calculates, and q is water retention in formula, and Q is to place water-setting after certain number of days
The weight of glue, QmaxFor the weight of hydrogel after water suction saturation.Test result is shown in Table 1.
Table 1
Fulvic acid type three-dimensional network composite material made from embodiment 7 has maximum water suction and guarantor as can be seen from Table 1
Aqueous energy, it is 291g/g that maximum, which inhales tap water multiplying power, and the water retention after 5 days under field conditions (factors) is 41.8%, with preferable
Water-absorbing-retaining effect.
The test of fulvic acid type three-dimensional network composite material absorption property: in the port grinding bottle of 7 same sizes, respectively plus
Enter fulvic acid type three-dimensional network composite material made from 50mg above-described embodiment 1~7 and the initial pH of 100mL is 4.0, but is initial dense
Identical methylene blue dye solution is spent, is put into constant temperature oscillation case and vibrates 4h, completely arrives at dye solution and composite material
Adsorption equilibrium.It takes supernatant to stand 15min after the completion of to be adsorbed, surveys it at 665nm with UV-752 type ultraviolet specrophotometer
Absorbance calculates the equilibrium concentration of the methylene blue dye of absorption front and back.In the port grinding bottle of 7 same sizes, it is separately added into
Fulvic acid type three-dimensional network composite material made from 50mg above-described embodiment 1~7 and the initial pH of 100mL are 4.0, initial concentration phase
Same methyl orange dye solution, is put into constant temperature oscillation case and vibrates 4h, so that dye solution and composite material is completely arrived at absorption flat
Weighing apparatus.It takes supernatant to stand 15min after the completion of to be adsorbed, surveys its absorbance at 507nm with UV-752 type ultraviolet specrophotometer,
The equilibrium concentration of the methylene blue dye of absorption front and back is calculated, test result is shown in Table 2.
Table 2
As can be seen from Table 2, fulvic acid type three-dimensional network composite material made from embodiment 3~7 is to methylene blue processing
Rate is 85% or more, and fulvic acid type three-dimensional network composite material made from embodiment 1 is 75% to methylene blue handling rate, is implemented
Fulvic acid type three-dimensional network composite material made from example 2 is 82% to methylene blue handling rate.
Fulvic acid type three-dimensional network composite material made from embodiment 3~7 is 80% or more to methyl orange handling rate, is implemented
Fulvic acid type three-dimensional network composite material made from example 4,7 is 85% or more to methyl orange handling rate, and Huang made from embodiment 1 is rotten
Acid type three-dimensional network composite material is 68% to methyl orange handling rate, fulvic acid type three-dimensional network composite wood made from embodiment 2
Material is 78% to methyl orange handling rate.
Two groups will be divided into the port grinding bottle of 14 same sizes, every group is respectively 7 port grinding bottles, is separately added into above-mentioned implementation
Fulvic acid type three-dimensional network composite material made from example 1~7 and the initial pH of 50mL are 0.9, the identical lead solution of initial concentration and
Chromium solution is put into constant temperature oscillation case and vibrates 120min, and lead solution and chromium solution and composite material is made to completely arrive at adsorption equilibrium.
Supernatant is taken to stand 15min, the equilibrium concentration of the lead after being adsorbed with complexometric titration and the balance of chromium after the completion of to be adsorbed
Solution.Test result is shown in Table 3.
Table 3
Fulvic acid type three-dimensional network composite material made from embodiment 3~7 is 50% or more to lead ion handling rate, is implemented
Fulvic acid type three-dimensional network composite material made from example 4,7 is 65% or more to lead ion handling rate, and Huang made from embodiment 1 is rotten
Acid type three-dimensional network composite material is 41% to lead ion handling rate, fulvic acid type three-dimensional network composite wood made from embodiment 2
Material is 47% to lead ion handling rate.
Fulvic acid type three-dimensional network composite material made from embodiment 2~7 is 50% or more to chromium ion handling rate, is implemented
Fulvic acid type three-dimensional network composite material made from example 4,7 is 65% or more to chromium ion handling rate, and Huang made from embodiment 1 is rotten
Acid type three-dimensional network composite material is 48% to chromium ion handling rate.And the fulvic acid type three-dimensional network composite material can drop
It solves, is pollution-free, being alternatively arranged as soil and fertilizer after the completion of absorption, soil texture can be improved, restoring the ecological balance, reducing chemical dirty
Dye.
In conclusion including that raw material is yellow rotten in the preparation method of fulvic acid type three-dimensional network composite material disclosed by the invention
Acid and natural macromolecular raw material, fulvic acid are that solubility is best in humic acid, activity is highest, and component is by aromatic series and its more
The polymeric organic acid that kind functional group is constituted, natural degradable have good physiological activity and absorption absorption, complexing, exchange
Etc. functions.It is widely present in soil, lake, river, ocean and peat (also known as turf), lignite, in weathered coal.Fulvic acid
Three-dimensional net structure is formed with natural macromolecular and then enhances the absorption or complexing to heavy metal ion particulate matter.This method
It is easy to operate, it is low for equipment requirements, it is environmentally protective, it is suitble to industrial amplification production.
Claims (10)
1. a kind of preparation method of fulvic acid type three-dimensional network composite material, which is characterized in that be divided into following steps:
1)/measurement mass parts ratio is referred to as (1.0~6.0): (0.3~1.0): fulvic acid, the natural macromolecular of (2.0~12.0)
And acrylic acid；
2) crosslinking agent and initiator is completely soluble in water, obtained solution A；
3) respectively that fulvic acid, natural macromolecular difference is completely soluble in water, obtain fulvic acid solution and natural macromolecular dispersion
Liquid is stirred and from room temperature with the heating speed of 2~4 DEG C/min after mixing fulvic acid solution, natural macromolecular dispersion liquid
Degree is warming up to 55~65 DEG C；
4) acrylic acid and solution A are added dropwise into the reaction system of step 3), continues to heat, with the heating rate liter of 2~4 DEG C/min
To 75~80 DEG C, stirring to system becomes gel and stops reaction temperature, takes out product and is dried, obtains fulvic acid type three dimensional network
Network composite material.
2. the preparation method of fulvic acid type three-dimensional network composite material according to claim 1, which is characterized in that initiator
For potassium peroxydisulfate or ammonium persulfate, dosage is the 0.5%~4.5% of fulvic acid dosage.
3. the preparation method of fulvic acid type three-dimensional network composite material according to claim 1, which is characterized in that crosslinking agent
For N, N- methylene-bisacrylamide or N methyldiethanol amine, quality are the 0.5%~1.0% of fulvic acid.
4. the preparation method of fulvic acid type three-dimensional network composite material according to claim 1, which is characterized in that step 4)
In, the time for adding of acrylic acid is 30~40min.
5. the preparation method of fulvic acid type three-dimensional network composite material according to claim 1, which is characterized in that step 4)
In, the time that solution A is added dropwise is 35~45min.
6. the preparation method of fulvic acid type three-dimensional network composite material according to claim 1, which is characterized in that step 4)
In, acrylic acid before dropwise addition under the conditions of 0 DEG C of ice-water bath in aqueous slkali and, degree of neutralization be 20%~80%.
7. the preparation method of fulvic acid type three-dimensional network composite material according to claim 1, which is characterized in that work as reaction
When temperature≤65 DEG C of system, mixing speed is 120~160r/min；When 65 DEG C of temperature > of reaction system, mixing speed
For 100~120r/min.
8. the preparation method of fulvic acid type three-dimensional network composite material according to claim 1, which is characterized in that water is to go
Ionized water or distilled water.
9. fulvic acid made from the preparation method of any one fulvic acid type three-dimensional network composite material according to claim 1~8
Type three-dimensional network composite material.
10. fulvic acid type three-dimensional network composite material as claimed in claim 9 as agricultural water-retaining agent, water pollution adsorbent,
The application of haze improvement agent.
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| CN111250060A (en) * | 2020-01-20 | 2020-06-09 | 陕西科技大学 | Cross network, natural recyclable humic acid type adsorption material, and preparation method and application thereof |
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| CN112755978A (en) * | 2021-01-12 | 2021-05-07 | 陕西科技大学 | Graphene oxide type adsorption material and preparation method and application thereof |
| CN113667071A (en) * | 2021-08-26 | 2021-11-19 | 东北石油大学 | Acrylic acid water-absorbing resin with potassium fulvate as base slow-release base material |
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