CN106238004B - A kind of preparation of cyanurotriamide modified magnetic fiber crops adsorbent - Google Patents

A kind of preparation of cyanurotriamide modified magnetic fiber crops adsorbent Download PDF

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CN106238004B
CN106238004B CN201610807195.XA CN201610807195A CN106238004B CN 106238004 B CN106238004 B CN 106238004B CN 201610807195 A CN201610807195 A CN 201610807195A CN 106238004 B CN106238004 B CN 106238004B
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fiber crops
adsorbent
magnetic fiber
cyanurotriamide modified
modified magnetic
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CN106238004A (en
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李慧芝
杨秋苹
许崇娟
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University of Jinan
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    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/24Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/06Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28002Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
    • B01J20/28009Magnetic properties
    • GPHYSICS
    • G21NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21FPROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
    • G21F9/00Treating radioactively contaminated material; Decontamination arrangements therefor
    • G21F9/04Treating liquids
    • G21F9/06Processing
    • G21F9/12Processing by absorption; by adsorption; by ion-exchange
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00Aspects relating to sorbent materials
    • B01J2220/40Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/46Materials comprising a mixture of inorganic and organic materials
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00Aspects relating to sorbent materials
    • B01J2220/40Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48Sorbents characterised by the starting material used for their preparation
    • B01J2220/4806Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00Aspects relating to sorbent materials
    • B01J2220/40Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48Sorbents characterised by the starting material used for their preparation
    • B01J2220/4812Sorbents characterised by the starting material used for their preparation the starting material being of organic character
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00Aspects relating to sorbent materials
    • B01J2220/40Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48Sorbents characterised by the starting material used for their preparation
    • B01J2220/4812Sorbents characterised by the starting material used for their preparation the starting material being of organic character
    • B01J2220/4825Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton

Abstract

The invention discloses a kind of preparation method of cyanurotriamide modified magnetic fiber crops adsorbent, it is characterised in that first, raw ramie is pre-processed;Second step, the fiber crops of pretreatment are subjected to oxidation processes;3rd step modifies magnetic particle on oxidation fiber crops, fiber crops is had magnetic;Finally, in the reactor, added by following composition mass percentage concentration, deionized water:72 ~ 80%, melamine:6 ~ 12%, dissolve by heating, magnetic fiber crops:12 ~ 20%, each component sum is dried absolutely, in 70 ± 2 DEG C of constant temperature, stirring, 4 ~ 6h of back flow reaction, after cooling, to be washed respectively with water, ethanol, separation of solid and liquid, obtains cyanurotriamide modified magnetic fiber crops adsorbent.The adsorbent has very high adsorption capacity to uranium, and not only cost was low but also green, high mechanical strength, can Reusability more than 10 times, adsorbent can be easily separated.

Description

A kind of preparation of cyanurotriamide modified magnetic fiber crops adsorbent
Technical field
The present invention relates to a kind of preparation method of biomagnetism adsorbent, more particularly to a kind of cyanurotriamide modified magnetic fiber crops The preparation method of adsorbent and to uranium(Ⅵ)The application technology of absorption, belong to regenerated resources utilization and environment and led with chemical technology Domain.
Background technology
Nuclear energy is the important channel that the world today solves energy shortage, caused however as the fast development of nuclear industry Uranium-bearing radioactive wastewater is more and more.In addition, during the exploitation, smelting and purification of uranium ore, it is usually associated with and largely contains The generation of uranium waste water, the uranium element in these waste water has chemical toxicity and radioactivity simultaneously, if untreated be discharged into week Ecological environment and health will be caused to seriously endanger in surrounding environment, therefore the processing to uranium-containing waste water enjoys pass always Note.
The method of traditional processing uranium-containing waste water mainly has evaporation concentration method, ion-exchange, coagulant sedimentation, oxidation also Former method etc., but the shortcomings of tediously long complicated and cost of technological process is higher be present in these conventional methods.And use biological adsorption material The biosorption process of radioactive wastewater is handled, because it has material source extensive, adsorption rate is fast, selectivity good, pH values and temperature It is wide to spend scope, and does not have the advantages that secondary pollution, is increasingly subject in the radioactive wastewater field containing uranium element is handled at present, Have some researchs both at home and abroad and show that bacterium, fungi, algae and inorganic adsorbing material etc. have certain enrichment to uranium, but Adsorption treatment effect is less desirable.Also there is a few studies person that agriculture and forestry organic waste material is used for the result of the adsorption treatment of uranium to show, Processing cost is low, secondary pollution is few, easy regeneration, reclaim uranium possibility it is big.
In water treatment procedure, adsorbent passes through the various active groups in surface in addition using its abundant structure, specific surface area Group and the interaction of adsorbate, extract pollutant, so as to have the function that purification of water quality from liquid phase.Wherein, absorption method Compared with other techniques advantage be to handle the reluctant metal ion of bioanalysis, hardly degraded organic substance and some it is cloudy from Sub- pollutant.But at the same time, for absorption method there is also many weak points, it is always to hinder that wherein the separation of solid and liquid of adsorbent is difficult Hinder a big problem of adsorption technology progress, thus many scholars are directed to studying magnetic adsorbent and applied in water body in recent years The removal of polluter.Research understands that with the help of externally-applied magnetic field, magnetic adsorbent can quickly realize separation of solid and liquid, and Possess the mass transfer rate of high speed and good contacting efficiency simultaneously, thus can largely solve traditional absorption method institute Problems faced.
Flax is the natural plant fibre that the mankind use earliest, away from modern existing more than 10,000 years history.Flax is pure natural Fiber, because flax fiber is soft, tough, glossy, wear-resisting, water imbibition is small, aproll is fast, expansion rate is big after fiber moisture absorption, energy Make textile tissue tight, be not easy permeable, be excellent textile raw material.It has absorbing sweat, good air permeability and harmless Etc. distinguishing feature, increasingly paid attention to by the mankind.Using this natural reproducible resource of flax, development environment friendly product and Technology, environmental pollution is advantageously reduced, by as the inexorable trend of sustainable development.Flax is annual herbaceous plant, is One of most valuable ecological resources, it is a kind of renewable resource.The cultivated area of current national flax is long fine up to more than 300 ten thousand mu The yield of dimension typically has a series of premium properties in 60kg/ mus or so, flax as textile fabric, is very precious weaving Fibrous raw material.But the chopped fiber for having 2% or so in fabrication processes is discarded object, these discarded objects can not be sufficiently using being sub- The serious waste of numb resource, also it is contaminated the environment in enterprise location.These chopped fibers have been made full use of both to reduce Environmental pollution can also create considerable economic benefit, and the suction of dyes is used for using these chopped fiber synthesizing new adsorbents It is attached, make this adsorbent that there is the characteristics of natural, green, biodegradable.
External modified to flax chemical and absorption property also has research, M. Cox etc. to have studied with flax modification preparation activity For charcoal to precious metal adsorption, its adsorption capacity is 1.708 mg/g(M. Cox, Sorption of precious metals onto chemically prepared carbon from flax shive. Hydrometallurgy,78(2005),137- 144).Li Xiaomin, HNO3Research of the linen waste adsorbent of modification to zinc ion adsorptivity.Yili Teacher College's journal(From Right science version), 2011(1), its adsorption capacity of 45-48. is 0.324mmol/g.The water body obtained is modified using flax chemical The adsorbance of the adsorbent of metal ion is smaller in system, and is influenceed bigger, Application No. by the pH of absorption system: 201110276212.9 patent in disclose a kind of preparation method and application of sulfydryl flax, sulfydryl flax is to Cd2+Absorption Capacity may be up to 282mg/g, and highest adsorption rate is up to 99.6%, to Pb2+Maximal absorptive capacity be 519mg/g, to Cu2+Most Big adsorbance is 160mg/g, the absorption prepared is modified using flax uranium absorption report is had no.
The application is adsorbed after the flaxen fiber magnetization of natural polymer using cyanurotriamide modified magnetic fiber crops as adsorbent SEPARATION OF URANIUM, make it that there is the characteristic of magnetic adsorbent, there is natural polymer sub-feature again, while also there is sp act group Selectivity.
The content of the invention
An object of the present invention is to provide a kind of preparation method of cyanurotriamide modified magnetic fiber crops adsorbent, and the one of acquisition Carry out adsorbing separation of the cyanurotriamide modified magnetic fiber crops adsorbent of kind to uranium in aqueous systems.
The purpose of the present invention is achieved through the following technical solutions.
A kind of preparation method of cyanurotriamide modified magnetic fiber crops adsorbent, it is characterised in that this method has following technique Step:
(1)Fiber crops pretreatment:Raw ramie is immersed in 1.5mol/L sodium hydroxide solution by solid-to-liquid ratio for 1g: 20 ~ 25mL, The h of soaking at room temperature 8 ~ 10, then 10min is boiled, it is washed with deionized after cooling to neutrality, separation of solid and liquid, dries, obtain pre- place Reason fiber crops;
(2)It is prepared by oxidation fiber crops:In the reactor, added by following composition mass percentage concentration, the concentrated sulfuric acid:25 ~ 30%, go Ionized water:50 ~ 60%, stir, be cooled to room temperature, potassium peroxydisulfate:3 ~ 7%, mix, add pretreatment fiber crops:10 ~ 18%, each group / and be the absolutely h of soaking at room temperature 4, then 10min is boiled, it is washed with deionized after cooling to neutrality, separation of solid and liquid, Dry, obtain oxidation fiber crops;
(3)It is prepared by magnetic fiber crops:In the reactor, added by following composition mass percentage concentration, ethanol:52 ~ 60%, nanometer Fe3O4Magnetic particle:4 ~ 8%, sodium tripolyphosphate:1.0 ~ 4.0%, γ-glycidyl ether oxygen propyl trimethoxy silicane:20 ~ 26%, Ultrasonic disperse adds oxidation fiber crops into suspension:8 ~ 15%, each component sum is absolutely, temperature rises to 60 ± 2 DEG C of constant temperature, stirred Mix, 3 ~ 5h of back flow reaction, after reaction terminates, be cooled to room temperature, separation of solid and liquid, wash, dry, obtain magnetic fiber crops;
(4)The preparation of cyanurotriamide modified magnetic fiber crops adsorbent:In the reactor, add by following composition mass percentage concentration Enter, deionized water:72 ~ 80%, melamine:6 ~ 12%, dissolve by heating, magnetic fiber crops:12 ~ 20%, each component sum is percent Hundred, in 70 ± 2 DEG C of constant temperature, stirring, 4 ~ 6h of back flow reaction, after cooling, washed respectively with water, ethanol, separation of solid and liquid, dry, obtain To cyanurotriamide modified magnetic fiber crops adsorbent.
In step(1)Described raw ramie is that flax is chopped fiber flax or the waste and old rope made of hemp or gunnysack that textile mills discard, It is eluted with water, dry, pulverize, sieves, particle diameter is between 120 ~ 140 mesh.
In step(3)Described nanometer Fe3O4The particle diameter of magnetic particle is less than 120nm.
It is special it is a further object of the present invention to provide cyanurotriamide modified magnetic fiber crops adsorbent to the absorption in aqueous systems to uranium Put and be:The cyanurotriamide modified magnetic fiber crops adsorbent deionized water prepared is soaked into 1 ~ 2h, adsorbed by static method.
The cyanurotriamide modified magnetic fiber crops adsorbent deionized water prepared is soaked into 1 ~ 2h, adsorbed by dynamic method.
The present invention compared with the prior art, has the following advantages that and beneficial effect:
(1)The cyanurotriamide modified magnetic fiber crops adsorbent that the present invention obtains has good physical and chemical stability and excellent Mechanical strength, adsorption capacity is big, to uranium maximum adsorption capacity up to 68.15 mg/g, it is wear-resisting can Reusability number up to 8 times More than, the speed of absorption is fast, and absorption chooses, and desorption performance is good, can be used in the range of wider soda acid.
(2)The cyanurotriamide modified magnetic fiber crops adsorbent that the present invention obtains both has the advantages of solid support material, also solves Active group of having determined is applied to the losing issue in water environment, and externally-applied magnetic field can divide the adsorbent after the completion of absorption from water From can be easily separated recovery, the advantages that density is small.
(3)Stability is good, is natural green product, and regrown material, discarded object is biodegradable, its wide material sources, price It is cheap, there is realistic meaning to pollution amelioration of ambient water etc., mitigate environmental protection pressure.
(4)The condition for crossing range request of synthesis is easily controlled, and energy consumption is low, simple to operate, belongs to process for cleanly preparing, is easy to Industrialized production.
Embodiment
Embodiment 1
(1)Fiber crops pretreatment:100g raw ramies are immersed in 2200mL 1.5mol/L sodium hydroxide solution, soaking at room temperature 9 h, then 10min is boiled, it is washed with deionized to neutrality, separation of solid and liquid, dries after cooling, obtains pretreatment fiber crops;
(2)It is prepared by oxidation fiber crops:In the reactor, it is separately added into, the concentrated sulfuric acid:75mL, deionized water:270mL, stirring are equal It is even, it is cooled to room temperature, potassium peroxydisulfate:25g, mix, add pretreatment fiber crops:60g, the h of soaking at room temperature 4, then 10min is boiled, cool down After be washed with deionized to neutrality, separation of solid and liquid, dry, obtain oxidation fiber crops;
(3)It is prepared by magnetic fiber crops:In the reactor, it is separately added into, ethanol:270mL, nanometer Fe3O4Magnetic particle:24g, three Polyphosphate sodium:8g, γ-glycidyl ether oxygen propyl trimethoxy silicane:85mL, ultrasonic disperse add oxidation fiber crops into suspension: 56g, temperature rises to 60 ± 2 DEG C of constant temperature, stirring, back flow reaction 4h, after reaction terminates, is cooled to room temperature, separation of solid and liquid, washs, do It is dry, obtain magnetic fiber crops;
(4)The preparation of cyanurotriamide modified magnetic fiber crops adsorbent:In the reactor, it is separately added into, deionized water:150mL, Melamine:16g, dissolve by heating, magnetic fiber crops:34g, in 70 ± 2 DEG C of constant temperature, stirring, back flow reaction 5h, after cooling, use respectively Water, ethanol washing, separation of solid and liquid, dry, obtain cyanurotriamide modified magnetic fiber crops adsorbent.
Embodiment 2
(1)Fiber crops pretreatment:100g raw ramies are immersed in 2000mL 1.5mol/L sodium hydroxide solution, soaking at room temperature 8 h, then 10min is boiled, it is washed with deionized to neutrality, separation of solid and liquid, dries after cooling, obtains pretreatment fiber crops;
(2)It is prepared by oxidation fiber crops:In the reactor, it is separately added into, the concentrated sulfuric acid:82mL, deionized water:250mL, stirring are equal It is even, it is cooled to room temperature, potassium peroxydisulfate:15g, mix, add pretreatment fiber crops:85g, the h of soaking at room temperature 4, then 10min is boiled, cool down After be washed with deionized to neutrality, separation of solid and liquid, dry, obtain oxidation fiber crops;
(3)It is prepared by magnetic fiber crops:In the reactor, it is separately added into, ethanol:330mL, nanometer Fe3O4Magnetic particle:40g, three Polyphosphate sodium:5g, γ-glycidyl ether oxygen propyl trimethoxy silicane:110mL, ultrasonic disperse add oxidation into suspension Fiber crops:75g, temperature rises to 60 ± 2 DEG C of constant temperature, stirring, back flow reaction 3h, after reaction terminates, is cooled to room temperature, separation of solid and liquid, washs, Dry, obtain magnetic fiber crops;
(4)The preparation of cyanurotriamide modified magnetic fiber crops adsorbent:In the reactor, it is separately added into, deionized water:142mL, Melamine:20g, dissolve by heating, magnetic fiber crops:36g, in 70 ± 2 DEG C of constant temperature, stirring, back flow reaction 4h, after cooling, use respectively Water, ethanol washing, separation of solid and liquid, dry, obtain cyanurotriamide modified magnetic fiber crops adsorbent.
Embodiment 3
(1)Fiber crops pretreatment:100g raw ramies are immersed in 2500mL 1.5mol/L sodium hydroxide solution, soaking at room temperature 10 h, then 10min is boiled, it is washed with deionized to neutrality, separation of solid and liquid, dries after cooling, obtains pretreatment fiber crops;
(2)It is prepared by oxidation fiber crops:In the reactor, it is separately added into, the concentrated sulfuric acid:68mL, deionized water:300mL, stirring are equal It is even, it is cooled to room temperature, potassium peroxydisulfate:20g, mix, add pretreatment fiber crops:55g, the h of soaking at room temperature 4, then 10min is boiled, cool down After be washed with deionized to neutrality, separation of solid and liquid, dry, obtain oxidation fiber crops;
(3)It is prepared by magnetic fiber crops:In the reactor, it is separately added into, ethanol:360mL, nanometer Fe3O4Magnetic particle:20g, three Polyphosphate sodium:20g, γ-glycidyl ether oxygen propyl trimethoxy silicane:120mL, ultrasonic disperse add oxidation into suspension Fiber crops:40g, temperature rises to 60 ± 2 DEG C of constant temperature, stirring, back flow reaction 5h, after reaction terminates, is cooled to room temperature, separation of solid and liquid, washs, Dry, obtain magnetic fiber crops;
(4)The preparation of cyanurotriamide modified magnetic fiber crops adsorbent:In the reactor, it is separately added into, deionized water:160mL, Melamine:12g, dissolve by heating, magnetic fiber crops:28g, in 70 ± 2 DEG C of constant temperature, stirring, back flow reaction 6h, after cooling, use respectively Water, ethanol washing, separation of solid and liquid, dry, obtain cyanurotriamide modified magnetic fiber crops adsorbent.
Embodiment 4
(1)Fiber crops pretreatment:50g raw ramies are immersed in 1000mL 1.5mol/L sodium hydroxide solution, soaking at room temperature 9 H, then 10min is boiled, it is washed with deionized to neutrality, separation of solid and liquid, dries after cooling, obtains pretreatment fiber crops;
(2)It is prepared by oxidation fiber crops:In the reactor, it is separately added into, the concentrated sulfuric acid:30mL, deionized water:110mL, stirring are equal It is even, it is cooled to room temperature, potassium peroxydisulfate:14g, mix, add pretreatment fiber crops:28g, soaking at room temperature 4h, then 10min is boiled, cool down After be washed with deionized to neutrality, separation of solid and liquid, dry, obtain oxidation fiber crops;
(3)It is prepared by magnetic fiber crops:In the reactor, it is separately added into, ethanol:75mL, nanometer Fe3O4Magnetic particle:4g, trimerization Sodium phosphate:4g, γ-glycidyl ether oxygen propyl trimethoxy silicane:26mL, ultrasonic disperse add oxidation fiber crops into suspension: 15g, temperature rises to 60 ± 2 DEG C of constant temperature, stirring, back flow reaction 4.5h, after reaction terminates, is cooled to room temperature, separation of solid and liquid, washs, Dry, obtain magnetic fiber crops;
(4)The preparation of cyanurotriamide modified magnetic fiber crops adsorbent:In the reactor, it is separately added into, deionized water:76mL, Melamine:12g, dissolve by heating, magnetic fiber crops:12g, in 70 ± 2 DEG C of constant temperature, stirring, back flow reaction 5h, after cooling, use respectively Water, ethanol washing, separation of solid and liquid, dry, obtain cyanurotriamide modified magnetic fiber crops adsorbent.
Embodiment 5
Weigh the cyanurotriamide modified magnetic fiber crops adsorbents of 0.10g and be placed in 1 ~ 2h of immersion in 250mL conical flask with cover, cross diafiltration After washing, it is 400mg/L uranium to add 100mL concentration(Ⅵ)In standard liquid, using the pH value of diluted acid or alkali regulation system as 2.0 ~ In the range of 11.0,2 ~ 4h of concussion absorption, takes supernatant at room temperature, with the concentration of Spectrophotometric Determination of Uranium, before absorption Afterwards in water uranium concentration difference, calculate the adsorption capacity of cyanurotriamide modified magnetic fiber crops adsorbent, the trimerization obtained by the present invention Absorption pH value of the cyanamide modified magnetic fiber crops adsorbent to uranium adsorbent in the range of 4.0 ~ 8.0 it is maximum to the adsorption capacity of uranium and Stable, concussion absorption 2h, uranium adsorb completely substantially at room temperature, and the adsorption capacity of uranium is up to 68.15 mg/g.
Embodiment 6
Weigh the cyanurotriamide modified magnetic fiber crops adsorbents of 1.0g and be placed in 1 ~ 2h of immersion in 250mL conical flask with cover, cross diafiltration After washing, it is in 200mg/L uranium standard liquids, using the pH value of diluted acid or alkali regulation system as 7.0, in room temperature to add 100mL concentration Lower concussion absorption 4h, takes supernatant, with the concentration of Spectrophotometric Determination of Uranium, according to the concentration difference of uranium in water before and after absorption, counts Clearance of the cyanurotriamide modified magnetic fiber crops adsorbent to uranium is calculated, the cyanurotriamide modified magnetic fiber crops absorption obtained by the present invention Agent all more than 94.12%, reaches as high as 98% to the clearance of uranium.

Claims (4)

1. a kind of preparation method of cyanurotriamide modified magnetic fiber crops adsorbent, it is characterised in that there is this method following technique to walk Suddenly:
(1) fiber crops pretreatment:Raw ramie is immersed in 1.5mol/L sodium hydroxide solution by solid-to-liquid ratio for 1g: 20~25mL, room Temperature 8~10h of immersion, then 10min is boiled, it is washed with deionized after cooling to neutrality, separation of solid and liquid, dries, pre-processed Fiber crops;
(2) prepared by oxidation fiber crops:In the reactor, added by following composition mass percent, the concentrated sulfuric acid:25~30%, deionization Water:50~60%, stir, be cooled to room temperature, potassium peroxydisulfate:3~7%, mix, add pretreatment fiber crops:10~18%, respectively Constituent mass percentage sum is absolutely soaking at room temperature 4h, then boils 10min, is washed with deionized after cooling into Property, separation of solid and liquid is dried, obtains aoxidizing fiber crops;
(3) prepared by magnetic fiber crops:In the reactor, added by following composition mass percent, ethanol:52~60%, nanometer Fe3O4 Magnetic particle:4~8%, sodium tripolyphosphate:1.0~4.0%, γ-glycidyl ether oxygen propyl trimethoxy silicane:20~ 26%, ultrasonic disperse adds oxidation fiber crops into suspension:8~15%, each component mass percent sum is absolutely temperature 60 ± 2 DEG C of constant temperature, stirring, 3~5h of back flow reaction are risen to, after reaction terminates, is cooled to room temperature, separation of solid and liquid, washs, dry, obtain To magnetic fiber crops;
(4) preparation of cyanurotriamide modified magnetic fiber crops adsorbent:In the reactor, add, go by following composition mass percent Ionized water:72~80%, melamine:6~12%, dissolve by heating, magnetic fiber crops:12~20%, each component mass percent it With for absolutely, in 70 ± 2 DEG C of constant temperature, stirring, 4~6h of back flow reaction, after cooling, washed respectively with water, ethanol, solid-liquid divides From, it is dry, obtain cyanurotriamide modified magnetic fiber crops adsorbent.
2. according to a kind of preparation method of cyanurotriamide modified magnetic fiber crops adsorbent described in claim 1, it is characterised in that Raw ramie described in step (1) is flax, is eluted with water, dry, pulverize, and sieving, particle diameter is between 120~140 mesh.
3. according to a kind of preparation method of cyanurotriamide modified magnetic fiber crops adsorbent described in claim 1, it is characterised in that Nanometer Fe described in step (3)3O4The particle diameter of magnetic particle is less than 120nm.
4. according to the trimerization prepared by a kind of preparation method of cyanurotriamide modified magnetic fiber crops adsorbent described in claim 1 Cyanamide modified magnetic fiber crops adsorbent.
CN201610807195.XA 2016-09-07 2016-09-07 A kind of preparation of cyanurotriamide modified magnetic fiber crops adsorbent Expired - Fee Related CN106238004B (en)

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Publication number Priority date Publication date Assignee Title
US20040124151A1 (en) * 2000-12-12 2004-07-01 Maxim, Llc, A Limited Liability Corporation Fibrous protein adsorption of heavy metals
CN101357325B (en) * 2008-09-18 2012-05-23 福州大学 Globular cellulose chelate sorbent containing amidoxime group and carboxy and preparation method thereof
CN101440526B (en) * 2008-12-29 2011-04-13 王宗乾 Preparation of kendir spinnable fiber
CN103993364B (en) * 2014-05-20 2016-10-12 东华大学 A kind of method aoxidizing degumming raising ramee performance
CN104258817B (en) * 2014-07-30 2016-08-24 青岛科技大学 The chitosan magnetic of melamine modification, preparation method and applications
CN104226271A (en) * 2014-09-28 2014-12-24 陕西华陆化工环保有限公司 Preparation method of adsorbent for heavy metal ions in water
CN104772123A (en) * 2015-04-01 2015-07-15 南华大学 Method for preparing amino modified sawdust adsorbent and application of method
CN105386132A (en) * 2015-10-15 2016-03-09 东华大学 Method for improving performance of ramine fibers in oxidation degumming mode through slow-release type weak base source

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