CN110280220A - The preparation method of the carboxyl acid modified magnetic certain herbaceous plants with big flowers stem marrow adsorbent of 5- amino -1H- imidazoles -4- - Google Patents
The preparation method of the carboxyl acid modified magnetic certain herbaceous plants with big flowers stem marrow adsorbent of 5- amino -1H- imidazoles -4- Download PDFInfo
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- CN110280220A CN110280220A CN201910567260.XA CN201910567260A CN110280220A CN 110280220 A CN110280220 A CN 110280220A CN 201910567260 A CN201910567260 A CN 201910567260A CN 110280220 A CN110280220 A CN 110280220A
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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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Abstract
The invention discloses a kind of preparation methods of the carboxyl acid modified magnetic certain herbaceous plants with big flowers stem marrow adsorbent of 5- amino -1H- imidazoles -4-, it is characterized in that, in the reactor, it is added by following composition mass percentage concentration, deionized water: 78 ~ 82%, 5- amino -1H- imidazoles -4- carboxylic acid: 6 ~ 10%, stirring and dissolving, add surface modification magnetism certain herbaceous plants with big flowers stem marrow particle: 10 ~ 14%, the sum of each component is absolutely, in 45 ± 2 DEG C of constant temperature, it is stirred to react 3h, it is cooled to room temperature, it is washed with deionized to neutrality, it is separated by solid-liquid separation, it is dry, obtain the carboxyl acid modified magnetic certain herbaceous plants with big flowers stem marrow adsorbent of 5- amino -1H- imidazoles -4-.The adsorbent has very high adsorption capacity to perfluorochemical, and selectivity is high, not only at low cost but also environmentally protective, light specific gravity, high mechanical strength, can Reusability, adsorbent can be easily separated.
Description
Technical field
The present invention relates to a kind of preparation method of biological adsorption agent, in particular to a kind of 5- amino -1H- imidazoles -4- carboxylic acid
The preparation method of modified magnetic certain herbaceous plants with big flowers stem marrow adsorbent and the application adsorbed to perfluorochemical, belong to regenerated resources utilization and ring
Border and technical field of chemistry.
Background technique
Studies have shown that perfluorinated compound has persistence and bioaccumulation, depot levels in vivo are higher than
The hundreds times to thousands of times of the persistence organic pollutants such as known organo-chlorine pesticide and dioxin.Perfluorinated compound also has
A variety of toxicity such as genotoxicity, mutagenesis toxicity, development toxicity, neurotoxicity, immunotoxicity are a kind of with organs poison
The environmental contaminants of property.Observable toxicity specifically includes in toxicologic study: inhibiting immune system, influences mitochondria generation
It thanks, leads to hepatocellular injury, reproduction cell is impaired, reduces breeding and fecundity, influences the advanced stage development of fetus, gene expression
Change, interfere enzymatic activity, destroy membrane structure, change thyroid function, etc..One of perfluorochemical is organic
Acid is white crystals under room temperature, is mainly used as surfactant, emulsifier.Perfluoro caprylic acid (PFOA) is difficult to degrade from environment,
Enter human body possibly through food, air and water.It may cause fertility-rate decline and other disease of immune system.1947
Year, Minnesota ,USA mining industry Manufacturing Co., Ltd (abbreviation 3M company) successfully develops perfluorochemical, since it is with excellent
Good thermal stability, chemical stability, high surface, hydrophobic and oleophobic performance, start to be widely used in lubricant, go out
The production fields such as fiery agent, surfactant, cleaning agent, cosmetics, textile, indoor decoration, leather and fur products.Wherein perfluoro caprylic acid
It is two kinds of typical perfluorochemicals of greatest concern at present with perfluorooctane sulfonate.Adsorbing separation removes present in ambient water
Organic and inorganic pollutant is had been considered as a kind of largely effective and common processing method, is removed in water using adsorption separation method
PFOA become those skilled in the art's concerned issue.PFOA report is removed seldom using adsorbing separation, is especially had to PFOA
Selective adsorbing separation is less.Therefore it can study and prepare the feasible method gesture that the waste water containing perfluorochemical is effectively treated must
Row.
Therefore the two big main problems that shortage of resources and environmental pollution have become the world today utilize natural reproducible
Resource, the inexorable trend of sustainable development will be become by developing environmentally friendly product and technology.Sunflower stem pith, Chinese medicine name.For
Medulla in the stem of compositae plant sunflower.There are cultivation in China various regions.Sunflower stem pith has spongiform porous structure, specific gravity
Gently, it also has dentate abundant, be easy to carry out chemical modification, be highly suitable as " skeleton " of adsorbent, sunflower stem
The modified application as adsorbent " skeleton " in adsorption of metal ions of marrow has not been reported.Sunflower stem pith is used as adsorbent
Have many advantages, such as renewable, degradable, environmentally friendly friendly, cheap, is important living resources, sunflower stem pith will be greatly improved
Utilization efficiency.
The application is by after the certain herbaceous plants with big flowers stem marrow premagnetization of natural polymer, using the carboxyl acid modified magnetism of 5- amino -1H- imidazoles -4-
For sunflower stem pith as adsorbent adsorbing separation perfluorochemical, making it i.e. has the characteristic of magnetic adsorbent, and has natural
Polymer characteristics, while also with the selectivity of sp act group.On the one hand the sharp again of agriculture and forestry organic waste material can be achieved in the application
With, turn waste into wealth, on the other hand, the biological adsorption agent of synthesis handles waste water containing perfluorochemical, and have raw material sources extensive, at
This cheap, simple operation and other advantages, and after the perfluorochemical in waste water is adsorbed, by desorbing, being enriched with, realize removal
The sustainable development of perfluorochemical, comprehensive utilization and environment to resource has double meaning.
Summary of the invention
An object of the present invention is to provide the carboxyl acid modified magnetic certain herbaceous plants with big flowers stem marrow adsorbent of two 5- amino -1H- imidazoles -4- of one kind
Preparation method, a kind of carboxyl acid modified magnetic certain herbaceous plants with big flowers stem marrow adsorbent of 5- amino -1H- imidazoles -4- of acquisition is to perfluorinated in water body
Close the carry out adsorbing separation of object.
The purpose of the present invention is achieved through the following technical solutions.
The preparation method of the carboxyl acid modified magnetic certain herbaceous plants with big flowers stem marrow adsorbent of a kind of 5- amino -1H- imidazoles -4-, which is characterized in that should
Method has following processing step:
(1) certain herbaceous plants with big flowers stem marrow powder pre-processes: in a kettle, being added by following composition mass percentage concentration, the NaOH of 1.0mol/L is molten
Liquid: 83 ~ 87%, sodium metasilicate: 2 ~ 4%, stirring and dissolving adds certain herbaceous plants with big flowers stem marrow powder: 10 ~ 14%, the sum of each component be absolutely, it is close
Capping is washed with deionized to neutrality after cooling, is separated by solid-liquid separation in 110 ± 2 DEG C of isothermal reaction 8h, dry, obtains pre- place
Manage certain herbaceous plants with big flowers stem marrow powder；
(2) it magnetic certain herbaceous plants with big flowers stem marrow particle preparation: in the reactor, is added by following composition mass percentage concentration, deionized water: 30 ~
34%, AEO-9:1 ~ 2%, xanthan gum: 4 ~ 6%, it dissolves by heating, nano-magnetic powder: 18 ~ 22%, pretreatment certain herbaceous plants with big flowers stem marrow powder: 38 ~ 42%, respectively
The sum of component is that absolutely, strong stirring, extrusion forming is granulated, and partial size obtains magnetic certain herbaceous plants with big flowers in 0.4 ~ 1.0mm, freeze-drying
Stem marrow particle；
(3) it magnetic certain herbaceous plants with big flowers stem marrow particle surface modification: in the reactor, is added by following composition mass percentage concentration, dehydrated alcohol:
58 ~ 62%, N- aminoethyl -3- aminopropyltriethoxy dimethoxysilane: 24 ~ 28%, magnetic certain herbaceous plants with big flowers stem marrow particle: 12 ~ 16%, each component
The sum of for absolutely, in 45 ± 2 DEG C of constant temperature, stirring, 5 h of back flow reaction, be washed with water after completion of the reaction, until filtrate is in neutrality
Until, it is separated by solid-liquid separation, it is dry, obtain surface modification magnetism certain herbaceous plants with big flowers stem marrow particle；
(4) preparation of the carboxyl acid modified magnetic certain herbaceous plants with big flowers stem marrow adsorbent of 5- amino -1H- imidazoles -4-: in the reactor, by following composition
Mass percentage concentration is added, deionized water: 78 ~ 82%, 5- amino -1H- imidazoles -4- carboxylic acid: 6 ~ 10%, stirring and dissolving adds
Surface modification magnetism certain herbaceous plants with big flowers stem marrow particle: 10 ~ 14%, the sum of each component is absolutely, in 45 ± 2 DEG C of constant temperature, to be stirred to react 3h,
It is cooled to room temperature, is washed with deionized to neutrality, is separated by solid-liquid separation, it is dry, obtain the carboxyl acid modified magnetic of 5- amino -1H- imidazoles -4-
Property certain herbaceous plants with big flowers stem marrow adsorbent.
The certain herbaceous plants with big flowers stem marrow powder is the flesh in the certain herbaceous plants with big flowers stem of mature native through crushing in step (1), with the sieve mistake of 800 mesh
The powder of sieve.
It is a further object of the present invention to provide a kind of carboxyl acid modified magnetic certain herbaceous plants with big flowers stem marrow adsorbents pair of 5- amino -1H- imidazoles -4-
To the absorption of perfluorochemical, feature in water body are as follows: by a kind of carboxyl acid modified magnetic certain herbaceous plants with big flowers stem marrow absorption of 5- amino -1H- imidazoles -4-
Agent impregnates 1 ~ 2h with deionized water, adsorbs by static method.
A kind of carboxyl acid modified magnetic certain herbaceous plants with big flowers stem marrow adsorbent deionized water of 5- amino -1H- imidazoles -4- is impregnated into 1 ~ 2h, is pressed
Dynamic method absorption.
Compared with the prior art, the present invention has the following advantages and beneficial effects:
(1) a kind of carboxyl acid modified magnetic certain herbaceous plants with big flowers stem marrow adsorbent of 5- amino -1H- imidazoles -4- that the present invention obtains has good object
Physicochemical stability and excellent mechanical strength, adsorption capacity is big, is 218.32 mg/g to perfluoro caprylic acid maximum adsorption capacity,
It is wear-resisting can Reusability number up to 10 times or more, the speed of absorption is fast, and absorption chooses, and desorption performance is good, selects different
Eluent can elute the heavy metal of absorption respectively, achieve the purpose that separation, can use within the scope of wider soda acid.
(2) a kind of carboxyl acid modified magnetic certain herbaceous plants with big flowers stem marrow adsorbent of 5- amino -1H- imidazoles -4- that the present invention obtains both has solid
The advantages of phase carrier material, also solves the losing issue that active group is applied in water environment, externally-applied magnetic field can will adsorb
The advantages that adsorbent after the completion is separated from the water, and is easy to separate and recover, and density is small.
(3) stability is good, is natural green product, regrown material, it can be achieved that agriculture and forestry organic waste material recycling, change give up into
Treasured, it is biodegradable, it is from a wealth of sources, it is cheap, there is realistic meaning to the pollution amelioration etc. of ambient water, mitigates environmental protection
Pressure.
(4) condition for crossing range request of synthesis is easy to control, and low energy consumption, easy to operate, is belonged to process for cleanly preparing, is easy to
Industrialized production.
Specific embodiment
Embodiment 1
(1) certain herbaceous plants with big flowers stem marrow powder pre-processes: it in a kettle, is separately added into, the NaOH solution of 1.0mol/L: 85 mL, and sodium metasilicate: 3g,
Stirring and dissolving adds certain herbaceous plants with big flowers stem marrow powder: 12g, seals lid, in 110 ± 2 DEG C of isothermal reaction 8h, is washed with deionized water after cooling
It washs to neutrality, is separated by solid-liquid separation, it is dry, obtain pretreatment certain herbaceous plants with big flowers stem marrow powder；
(2) it magnetic certain herbaceous plants with big flowers stem marrow particle preparation: in the reactor, is separately added into, deionized water: 32 mL, AEO-9:1g, xanthan gum:
5g is dissolved by heating, nano-magnetic powder, and: 20g pre-processes certain herbaceous plants with big flowers stem marrow powder: 42g, strong stirring, and extrusion forming is granulated, partial size 0.4 ~
1.0mm, freeze-drying, obtains magnetic certain herbaceous plants with big flowers stem marrow particle；
(3) it magnetic certain herbaceous plants with big flowers stem marrow particle surface modification: in the reactor, is separately added into, dehydrated alcohol: 76 mL, N- aminoethyl -3-
Aminopropyltriethoxy dimethoxysilane: 26g, magnetic certain herbaceous plants with big flowers stem marrow particle: 14g, in 45 ± 2 DEG C of constant temperature, stirring, 5 h of back flow reaction,
It is washed with water, until filtrate is in neutrality, is separated by solid-liquid separation after completion of the reaction, it is dry, obtain surface modification magnetism certain herbaceous plants with big flowers stem marrow particle；
(4) it the preparation of the carboxyl acid modified magnetic certain herbaceous plants with big flowers stem marrow adsorbent of 5- amino -1H- imidazoles -4-: in the reactor, is separately added into, goes
Ionized water: 80 mL, 5- amino -1H- imidazoles -4- carboxylic acid: 8g, stirring and dissolving add surface modification magnetism certain herbaceous plants with big flowers stem marrow particle:
12g in 45 ± 2 DEG C of constant temperature, is stirred to react 3h, is cooled to room temperature, and is washed with deionized to neutrality, is separated by solid-liquid separation, dry, obtains
To the carboxyl acid modified magnetic certain herbaceous plants with big flowers stem marrow adsorbent of 5- amino -1H- imidazoles -4-.
Embodiment 2
(1) certain herbaceous plants with big flowers stem marrow powder pre-processes: it in a kettle, is separately added into, the NaOH solution of 1.0mol/L: 166 mL, and sodium metasilicate:
8g, stirring and dissolving add certain herbaceous plants with big flowers stem marrow powder: 26g, seal lid, in 110 ± 2 DEG C of isothermal reaction 8h, use deionized water after cooling
Washing is separated by solid-liquid separation, drying to neutrality, obtains pretreatment certain herbaceous plants with big flowers stem marrow powder；
(2) it magnetic certain herbaceous plants with big flowers stem marrow particle preparation: in the reactor, is separately added into, deionized water: 60 mL, AEO-9:4g, xanthan gum:
12g is dissolved by heating, nano-magnetic powder, and: 44g pre-processes certain herbaceous plants with big flowers stem marrow powder: 80g, strong stirring, and extrusion forming is granulated, partial size 0.4 ~
1.0mm, freeze-drying, obtains magnetic certain herbaceous plants with big flowers stem marrow particle；
(3) it magnetic certain herbaceous plants with big flowers stem marrow particle surface modification: in the reactor, is separately added into, dehydrated alcohol: 146mL, N- aminoethyl -3-
Aminopropyltriethoxy dimethoxysilane: 54g, magnetic certain herbaceous plants with big flowers stem marrow particle: 30g, in 45 ± 2 DEG C of constant temperature, stirring, 5 h of back flow reaction,
It is washed with water, until filtrate is in neutrality, is separated by solid-liquid separation after completion of the reaction, it is dry, obtain surface modification magnetism certain herbaceous plants with big flowers stem marrow particle；
(4) it the preparation of the carboxyl acid modified magnetic certain herbaceous plants with big flowers stem marrow adsorbent of 5- amino -1H- imidazoles -4-: in the reactor, is separately added into, goes
Ionized water: 158 mL, 5- amino -1H- imidazoles -4- carboxylic acid: 14g, stirring and dissolving add surface modification magnetism certain herbaceous plants with big flowers stem marrow
Grain: 28g in 45 ± 2 DEG C of constant temperature, is stirred to react 3h, is cooled to room temperature, and is washed with deionized to neutrality, is separated by solid-liquid separation, does
It is dry, obtain the carboxyl acid modified magnetic certain herbaceous plants with big flowers stem marrow adsorbent of 5- amino -1H- imidazoles -4-.
Embodiment 3
(1) certain herbaceous plants with big flowers stem marrow powder pre-processes: it in a kettle, is separately added into, the NaOH solution of 1.0mol/L: 87 mL, and sodium metasilicate: 2g,
Stirring and dissolving adds certain herbaceous plants with big flowers stem marrow powder: 11g, seals lid, in 110 ± 2 DEG C of isothermal reaction 8h, is washed with deionized water after cooling
It washs to neutrality, is separated by solid-liquid separation, it is dry, obtain pretreatment certain herbaceous plants with big flowers stem marrow powder；
(2) it magnetic certain herbaceous plants with big flowers stem marrow particle preparation: in the reactor, is separately added into, deionized water: 34mL, AEO-9:1g, xanthan gum:
4g is dissolved by heating, nano-magnetic powder, and: 22g pre-processes certain herbaceous plants with big flowers stem marrow powder: 39g, strong stirring, and extrusion forming is granulated, partial size 0.4 ~
1.0mm, freeze-drying, obtains magnetic certain herbaceous plants with big flowers stem marrow particle；
(3) it magnetic certain herbaceous plants with big flowers stem marrow particle surface modification: in the reactor, is separately added into, dehydrated alcohol: 78 mL, N- aminoethyl -3-
Aminopropyltriethoxy dimethoxysilane: 25g, magnetic certain herbaceous plants with big flowers stem marrow particle: 13g, in 45 ± 2 DEG C of constant temperature, stirring, 5 h of back flow reaction,
It is washed with water, until filtrate is in neutrality, is separated by solid-liquid separation after completion of the reaction, it is dry, obtain surface modification magnetism certain herbaceous plants with big flowers stem marrow particle；
(4) it the preparation of the carboxyl acid modified magnetic certain herbaceous plants with big flowers stem marrow adsorbent of 5- amino -1H- imidazoles -4-: in the reactor, is separately added into, goes
Ionized water: 78 mL, 5- amino -1H- imidazoles -4- carboxylic acid: 10g, stirring and dissolving add surface modification magnetism certain herbaceous plants with big flowers stem marrow particle:
12g in 45 ± 2 DEG C of constant temperature, is stirred to react 3h, is cooled to room temperature, and is washed with deionized to neutrality, is separated by solid-liquid separation, dry, obtains
To the carboxyl acid modified magnetic certain herbaceous plants with big flowers stem marrow adsorbent of 5- amino -1H- imidazoles -4-.
Embodiment 4
(1) certain herbaceous plants with big flowers stem marrow powder pre-processes: it in a kettle, is separately added into, the NaOH solution of 1.0mol/L: 86 mL, and sodium metasilicate: 4g,
Stirring and dissolving adds certain herbaceous plants with big flowers stem marrow powder: 10g, seals lid, in 110 ± 2 DEG C of isothermal reaction 8h, is washed with deionized water after cooling
It washs to neutrality, is separated by solid-liquid separation, it is dry, obtain pretreatment certain herbaceous plants with big flowers stem marrow powder；
(2) it magnetic certain herbaceous plants with big flowers stem marrow particle preparation: in the reactor, is separately added into, deionized water: 33 mL, AEO-9:2g, xanthan gum:
6g is dissolved by heating, nano-magnetic powder, and: 18g pre-processes certain herbaceous plants with big flowers stem marrow powder: 41g, strong stirring, and extrusion forming is granulated, partial size 0.4 ~
1.0mm, freeze-drying, obtains magnetic certain herbaceous plants with big flowers stem marrow particle；
(3) it magnetic certain herbaceous plants with big flowers stem marrow particle surface modification: in the reactor, is separately added into, dehydrated alcohol: 76 mL, N- aminoethyl -3-
Aminopropyltriethoxy dimethoxysilane: 24g, magnetic certain herbaceous plants with big flowers stem marrow particle: 16g, in 45 ± 2 DEG C of constant temperature, stirring, 5 h of back flow reaction,
It is washed with water, until filtrate is in neutrality, is separated by solid-liquid separation after completion of the reaction, it is dry, obtain surface modification magnetism certain herbaceous plants with big flowers stem marrow particle；
(4) it the preparation of the carboxyl acid modified magnetic certain herbaceous plants with big flowers stem marrow adsorbent of 5- amino -1H- imidazoles -4-: in the reactor, is separately added into, goes
Ionized water: 82mL, 5- amino -1H- imidazoles -4- carboxylic acid: 6g, stirring and dissolving add surface modification magnetism certain herbaceous plants with big flowers stem marrow particle:
11g in 45 ± 2 DEG C of constant temperature, is stirred to react 3h, is cooled to room temperature, and is washed with deionized to neutrality, is separated by solid-liquid separation, dry, obtains
To the carboxyl acid modified magnetic certain herbaceous plants with big flowers stem marrow adsorbent of 5- amino -1H- imidazoles -4-.
Embodiment 5
It weighs the carboxyl acid modified magnetic certain herbaceous plants with big flowers stem marrow adsorbent of 0.10g 5- amino -1H- imidazoles -4- and is respectively placed in 250mL tool plug taper
Impregnate 2h in bottle, after filtration washing, then be separately added into 100mL concentration and be in 200mg/L perfluoro caprylic acid standard solution, with diluted acid or
The pH value of alkali regulation system is in 4.0 ~ 10.0 ranges, and 0.5 ~ 2.5h of concussion absorption, takes supernatant, using efficient liquid at room temperature
Phase chromatography measures the concentration of perfluoro caprylic acid, according to the concentration difference of perfluoro caprylic acid in the water of absorption front and back, calculates 5- amino -1H-
The adsorption capacity of the carboxyl acid modified magnetic certain herbaceous plants with big flowers stem marrow adsorbent of imidazoles -4-, 5- amino -1H- imidazoles -4- carboxylic acid obtained by the present invention
Modified magnetic certain herbaceous plants with big flowers stem marrow adsorbent to the absorption pH value of perfluoro caprylic acid in 5.0 ~ 7.5 ranges, suction of the adsorbent to perfluoro caprylic acid
Attached capacity is maximum and stablizes, and concussion absorption 0.6h, adsorption saturation reach perfluoro caprylic acid maximum adsorption capacity at room temperature
218.32 mg/g。
Embodiment 6
It weighs the carboxyl acid modified magnetic certain herbaceous plants with big flowers stem marrow adsorbent of 1.0g 5- amino -1H- imidazoles -4- and is respectively placed in 250mL stuffed conical flask
Middle immersion 2h, after filtration washing, it is to adjust body in 10mg/L perfluoro caprylic acid standard solution with diluted acid or alkali that 100mL concentration, which is added,
The pH value of system is 6.0, and concussion absorption 1.0h, takes supernatant, measure the concentration of perfluoro caprylic acid at room temperature, according to absorption front and back water
The concentration difference of middle perfluoro caprylic acid calculates the carboxyl acid modified magnetic certain herbaceous plants with big flowers stem marrow adsorbent of 5- amino -1H- imidazoles -4- to perfluoro caprylic acid
Removal rate, to the removal rate of perfluoro caprylic acid all 96.81% or more.
Claims (3)
1. a kind of preparation method of the carboxyl acid modified magnetic certain herbaceous plants with big flowers stem marrow adsorbent of 5- amino -1H- imidazoles -4-, which is characterized in that the party
Method has following processing step:
(1) certain herbaceous plants with big flowers stem marrow powder pre-processes: in a kettle, being added by following composition mass percentage concentration, the NaOH of 1.0mol/L is molten
Liquid: 83 ~ 87%, sodium metasilicate: 2 ~ 4%, stirring and dissolving adds certain herbaceous plants with big flowers stem marrow powder: 10 ~ 14%, the sum of each component be absolutely, it is close
Capping is washed with deionized to neutrality after cooling, is separated by solid-liquid separation in 110 ± 2 DEG C of isothermal reaction 8h, dry, obtains pre- place
Manage certain herbaceous plants with big flowers stem marrow powder；
(2) it magnetic certain herbaceous plants with big flowers stem marrow particle preparation: in the reactor, is added by following composition mass percentage concentration, deionized water: 30 ~
34%, AEO-9:1 ~ 2%, xanthan gum: 4 ~ 6%, it dissolves by heating, nano-magnetic powder: 18 ~ 22%, pretreatment certain herbaceous plants with big flowers stem marrow powder: 38 ~ 42%, respectively
The sum of component is that absolutely, strong stirring, extrusion forming is granulated, and partial size obtains magnetic certain herbaceous plants with big flowers in 0.4 ~ 1.0mm, freeze-drying
Stem marrow particle；
(3) it magnetic certain herbaceous plants with big flowers stem marrow particle surface modification: in the reactor, is added by following composition mass percentage concentration, dehydrated alcohol:
58 ~ 62%, N- aminoethyl -3- aminopropyltriethoxy dimethoxysilane: 24 ~ 28%, magnetic certain herbaceous plants with big flowers stem marrow particle: 12 ~ 16%, each component
The sum of for absolutely, in 45 ± 2 DEG C of constant temperature, stirring, 5 h of back flow reaction, be washed with water after completion of the reaction, until filtrate is in neutrality
Until, it is separated by solid-liquid separation, it is dry, obtain surface modification magnetism certain herbaceous plants with big flowers stem marrow particle；
(4) preparation of the carboxyl acid modified magnetic certain herbaceous plants with big flowers stem marrow adsorbent of 5- amino -1H- imidazoles -4-: in the reactor, by following composition
Mass percentage concentration is added, deionized water: 78 ~ 82%, 5- amino -1H- imidazoles -4- carboxylic acid: 6 ~ 10%, stirring and dissolving adds
Surface modification magnetism certain herbaceous plants with big flowers stem marrow particle: 10 ~ 14%, the sum of each component is absolutely, in 45 ± 2 DEG C of constant temperature, to be stirred to react 3h,
It is cooled to room temperature, is washed with deionized to neutrality, is separated by solid-liquid separation, it is dry, obtain the carboxyl acid modified magnetic of 5- amino -1H- imidazoles -4-
Property certain herbaceous plants with big flowers stem marrow adsorbent.
2. a kind of system of the carboxyl acid modified magnetic certain herbaceous plants with big flowers stem marrow adsorbent of 5- amino -1H- imidazoles -4- according to claim 1
Preparation Method, which is characterized in that certain herbaceous plants with big flowers stem marrow powder as described in step (1) is the flesh in the certain herbaceous plants with big flowers stem of mature native through crushing, with 800 mesh
Sieve powder.
3. a kind of system of the carboxyl acid modified magnetic certain herbaceous plants with big flowers stem marrow adsorbent of 5- amino -1H- imidazoles -4- according to claim 1
The carboxyl acid modified magnetic certain herbaceous plants with big flowers stem marrow adsorbent of 5- amino -1H- imidazoles -4- prepared by Preparation Method.
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| CN201910567260.XA CN110280220A (en) | 2019-06-27 | 2019-06-27 | The preparation method of the carboxyl acid modified magnetic certain herbaceous plants with big flowers stem marrow adsorbent of 5- amino -1H- imidazoles -4- |
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Citations (7)
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| CN102500330A (en) * | 2011-10-13 | 2012-06-20 | 西南科技大学 | Preparation and use methods of helianthus stem and leaf adsorbing material for heavy metals |
| CN102500338A (en) * | 2011-11-23 | 2012-06-20 | 清华大学 | PFOA (perfluorooctanoic acid) adsorbent and preparation method thereof |
| CN104759260A (en) * | 2015-04-14 | 2015-07-08 | 河海大学 | Amino-functionalization magnetic silicon dioxide-ferroferric oxide composite nanomaterial and preparation method thereof |
| CN106215881A (en) * | 2016-09-07 | 2016-12-14 | 济南大学 | A kind of preparation method of cyanurotriamide modified porous magnetic dextran microspheres |
| CN106268675A (en) * | 2016-09-07 | 2017-01-04 | 济南大学 | A kind of preparation of triethylene tetramine modified magnetic palm bark adsorbent |
| CN106345432A (en) * | 2016-09-07 | 2017-01-25 | 济南大学 | Preparation method of polyacrylamide modified magnetic loofah sponge adsorbent |
| CN108543524A (en) * | 2018-05-14 | 2018-09-18 | 济南大学 | A kind of diethylenetriamines is modified the preparation method of banana fiber adsorbent |
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Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102500330A (en) * | 2011-10-13 | 2012-06-20 | 西南科技大学 | Preparation and use methods of helianthus stem and leaf adsorbing material for heavy metals |
| CN102500338A (en) * | 2011-11-23 | 2012-06-20 | 清华大学 | PFOA (perfluorooctanoic acid) adsorbent and preparation method thereof |
| CN104759260A (en) * | 2015-04-14 | 2015-07-08 | 河海大学 | Amino-functionalization magnetic silicon dioxide-ferroferric oxide composite nanomaterial and preparation method thereof |
| CN106215881A (en) * | 2016-09-07 | 2016-12-14 | 济南大学 | A kind of preparation method of cyanurotriamide modified porous magnetic dextran microspheres |
| CN106268675A (en) * | 2016-09-07 | 2017-01-04 | 济南大学 | A kind of preparation of triethylene tetramine modified magnetic palm bark adsorbent |
| CN106345432A (en) * | 2016-09-07 | 2017-01-25 | 济南大学 | Preparation method of polyacrylamide modified magnetic loofah sponge adsorbent |
| CN108543524A (en) * | 2018-05-14 | 2018-09-18 | 济南大学 | A kind of diethylenetriamines is modified the preparation method of banana fiber adsorbent |
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Application publication date: 20190927 |