CN108356276A - A kind of the hypergravity preparation method and device of cellulose modified nano zero valence iron - Google Patents
A kind of the hypergravity preparation method and device of cellulose modified nano zero valence iron Download PDFInfo
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Abstract
The invention discloses a kind of hypergravity preparation method of cellulose modified nano zero valence iron and device, metal nanometer material technical fields.It is designed to provide a kind of method continuously preparing cellulose modified nano zero valence iron, cellulose is sent into supergravity reactor by this method simultaneously with the mixed solution of molysite and reducing agent to react, Magneto separate reaction product after reaction, deionized water is cleaned repeatedly to neutrality, and vacuum drying obtains cellulose modified nano zero-valence iron particle.One step of this method prepares cellulose modified zeroth order iron nano-particle; it is simple for process, the reaction time is short, it is at low cost, be produced on a large scale; the cellulose modified nano zero valence iron grain size of preparation is small simultaneously, favorable dispersibility, has good stability, reactivity height, has industrial applications foreground.
Description
Technical field
The present invention relates to a kind of hypergravity preparation method of cellulose modified nano zero valence iron and devices, belong to nano material
Preparing technical field.
Background technology
Nano zero valence iron（Nano Zerovalent iron, NZVI）Due to the ratio table than common Zero-valent Iron bigger
The advantages that area, stronger reactivity, can be widely used in magneto-rheological fluid preparation, magnetic resonance imaging, magnetic recording material are opened
The various fields such as hair, catalyst environment remediation.Currently, there are many methods of physics, chemistry to be used for zeroth order iron nano-particle
It prepares.Wherein, liquid phase reduction prepares the most common method of nano zero valence iron as laboratory, is to utilize alkali gold in aqueous solution
Belong to borohydride reduction Fe (II) and Fe (III) prepares nano zero valence iron, biggest advantage is easy to operate, experiment condition
Mildly.But nano zero valence iron prepared by this method is easy oxidation and reunites, this makes nano zero valence iron be restricted in the application.
Therefore it is modified reduction to nano zero valence iron to reunite, enhancing inoxidizability is the hot spot studied in recent years.
Nano zero-valence iron surface cladding is modified to its surface, is on the one hand acted on by electrostatic interaction and steric hindrance
It reduces nano grain surface energy state and reduces and reunite, on the other hand by increasing the specific surface area of particle, enhance the reaction of its surface and live
Property.In the covering material reported, water-soluble natural macromolecule amylose due to its it is cheap, environmental-friendly and by as one kind
Outstanding stable dispersant.Cellulose is most abundant on the earth and reproducible natural polymer, is that a kind of threadiness, crinosity are thin
The high molecular polymer of the stereospecificity of pipe has porous and its large specific surface area characteristic, and basic structural unit is D-
For glucopyranosyl by β-Isosorbide-5-Nitrae glucosides key connection, there are three active hydroxyls for each glucose unit in strand, easily send out
The reactions such as raw oxidation, esterification, etherificate, graft copolymerization.Therefore, it using cellulose as stabilizer, can not only be closed in nano zero valence iron
The grain size of nano-particle is efficiently controlled during, moreover it is possible to improve the reunion of nano zero valence iron in the liquid phase, to improve
The stability and reactivity of nano zero valence iron.
Usual cellulose modified nano zero valence iron can obtain by the following method：(1) two-step method：Use liquid phase also first
Former method prepares out nano zero valence iron, and then cellulose matter rationality is adsorbed onto on the nano zero valence iron prepared, prepared by the method
Process is complicated, is unfavorable for large-scale industrial production；(2) one-step method：Under the conditions of existing for cellulose, using liquid-phase reduction
Method synthesizes nano zero valence iron, Simultaneous Stabilization nano zero valence iron.Different coating modification methods is steady to the nano zero valence iron of preparation
Qualitative to have an impact, general one-step method is chemical precipitation process, and nano zero valence iron is synthesized in the presence of cellulose stabilizers,
Cellulose is set to be precipitated out from solvent in nano zero valence iron forming process.Although the method preparation process is simple, its
Reaction unit is usually stirring reactor, is to make reaction mass Strong dispersion hybrid reaction using the shearing force of agitating paddle, is belonged to
In intermittently operated, the microcosmic uniformly mixed time is about 0.01 ~ 0.2 s.Since borohydride reduction iron ion generates zeroth order
Iron simple substance is a quickly reaction precipitation process, and the characteristic time of nucleation is about 1ms（Millisecond）, therefore stirred in traditional
Mix transmission in formula reactor on molecular scale and mixing rate be much smaller than the nucleation rate of liquid-phase reduction precipitation, so as to cause at
Core and growth course are in the uneven environment on molecular scale, and the cellulose thus prepared using traditional stirring reactor is changed
Property nano zero valence iron is uneven there are particle diameter distribution and the industrialness problems such as batch production poor reproducibility, Product management model effect is big.
Therefore, it is that nano zero valence iron is modified institute that exploitation can prepare the new process of nano zero-valence iron composite material and new method with continuous batch
The critical problem to be solved.
Invention content
The present invention is intended to provide the hypergravity preparation method and device of a kind of cellulose modified nano zero valence iron, prepared by a step
Cellulose modified nano zero valence iron, this method have the characteristics that simple for process, the reaction time is short, it is at low cost, be produced on a large scale,
Simultaneously prepare cellulose modified nano zero valence iron good dispersion, stability is good, reactivity is high, grain size is small, have industrialization
Application prospect.
The characteristics of high-gravity technology strengthens microcosmic mixing and mass transport process because of it, can make reaction system moment reach higher
And the degree of supersaturation that is evenly distributed and the Determining Micromixing Characteristic Time less than nucleation induction time, it is therefore widely used in a nanometer material
In the preparation of material.High-gravity technology preparation nano material is short with the reaction time, formation nano particle diameter is small, particle diameter distribution
Uniformly, manufacturing cost is low, is easy to industrial amplification production（4-20 times can be improved compared with conventional method）The advantages that.Currently, super
Gravity techniques have been successfully applied to Fe3O4、TiO2、ZnO、BaSO4、CaCO3、BaTiO3、SiO2, ceria, LiMn2O4Deng more
Among the industrialized production of kind nano-powder.Therefore, it is combined with reaction precipitation method using high-gravity technology, one-step synthesis dispersibility
Good, stability is good, reactivity is high, the uniform cellulose modified nano zero valence iron of particle diameter distribution, and nano zero valence iron may be implemented
The continuous preparation of based composites provides new approaches for efficient utilize of nano zero valence iron.
The present invention provides a kind of hypergravity preparation method of cellulose modified nano zero valence iron, by cellulose and molysite
Mixed solution and reducing agent are sent into supergravity reactor simultaneously to react, after reaction Magneto separate reaction product, deionized water
It is cleaned repeatedly to neutrality, vacuum drying obtains cellulose modified nano zero-valence iron particle, is as follows：
(1) cellulose and molysite mixed solution are prepared：By cellulose derivative be dissolved in water be configured to cellulose concentration be 0.1% ~
Then molysite is configured to iron ion or ferrous ion concentration is 0.05 ~ 1.0 mol/L cellulose and molysite is added in 1% solution
Mixed solution；The molysite is trivalent iron salt or ferrous salt；
(2) reducing agent solution is prepared：Use sodium borohydride or potassium borohydride for reducing agent, by BH4 -With the molar ratio of iron ion
It is 2:1~4:1 prepares the aqueous solution that reductant concentration is 0.1 ~ 4.0 mol/L；
(3) synthetic cellulose modified Nano Zero-valent Iron：The mixed solution of cellulose and molysite, reducing agent aqueous solution are set respectively
In reservoir, two strands of isometric reaction masses, which are delivered to by liquid distribution trough in supergravity reactor, to be reacted,
Any one moment cellulose and molysite mixed solution are all anti-after being mixed according to set proportion with reducing agent aqueous solution
Cellulose modified nano zero-valence iron particle should be generated, the volume flow of two strands of material liquids of control is 20 ~ 100 L/h, and hypergravity is anti-
Answer the rotating speed of device in 100 ~ 2500 rpm；
(4) after reaction, reaction product is collected using magnetic separation technique, is cleaned repeatedly with deionized water to neutrality, vacuum
It is dried to obtain cellulose modified nano zero-valence iron particle.
In the above method, the trivalent iron salt, ferrous salt are ferric sulfate, ferric nitrate, iron chloride, ferrous sulfate, nitric acid Asia
One kind in iron, frerrous chloride.
In the above method, the cellulose is cellulose derivative, including carboxymethyl cellulose, hydroxyethyl cellulose, hydroxyl
One kind in propyl methocel.
The present invention provides the above-mentioned hypergravity preparation facilities for preparing cellulose modified nano zero valence iron, including hypergravity are anti-
Device, molysite storage tank, reducing agent storage tank, molysite storage tank and reducing agent storage tank is answered to be separately connected supergravity reactor, divide in connecting tube
Not She You valve and spinner flowmeter, distributor is equipped in supergravity reactor, supergravity reactor bottom is equipped with product storage tank.
The supergravity reactor be Impinging Stream-Rotating Packed Bed, it is rotary packed bed, in rotating bed with helix channel one
Kind.
In above-mentioned preparation facilities, the supergravity reactor is Impinging Stream-Rotating Packed Bed, starts centrifugal pump by raw material
Liquid is conveyed into through spinner flowmeter in Impinging Stream-Rotating Packed Bed, and two strands of isometric reaction masses pass through liquid distribution trough
Nozzle constant speed hit after be ejected on rotary packed bed inner edge, under the influence of centrifugal force along the outside edge stream of filler hole
It is dynamic, and reaction is mutually mixed in packing layer；Finally, reaction product is thrown to shell from the outer rim of filler under the influence of centrifugal force
On, it is pooled to exit under gravity, is discharged through outlet.
In above-mentioned preparation facilities, the supergravity reactor is rotary packed bed, starts centrifugal pump and passes through raw material liq
Spinner flowmeter is conveyed into rotary packed bed, and two strands of isometric reaction masses are sprayed by the nozzle of trepanning on liquid distribution trough
Onto filler, liquid is flowed along filler hole from rotor inner edge to rotor periphery under the influence of centrifugal force, and multiple by filler
Cutting, coalescence and dispersion, are mutually mixed reaction in packing layer；Finally, reaction product is under the influence of centrifugal force outside filler
It is thrown on shell at edge, is pooled to outlet discharge under the effect of gravity.
In above-mentioned preparation facilities, the supergravity reactor is rotating bed with helix channel, starts centrifugal pump by raw material
Liquid is conveyed into through spinner flowmeter in rotating bed with helix channel, and two strands of isometric reaction masses are entered by liquid distribution trough
In helical duct, liquid acts on from inside to outside centrifugal force along the rotor stream with spiral of Archimedes shape channel
Go out；And it is mutually mixed, reacts in helical duct；Finally, reaction product is thrown to from rotor periphery outer under the influence of centrifugal force
On shell, it is pooled to outlet discharge under gravity.
The present invention utilizes high-speed rotating filler pair by the cellulose modified nano zero valence iron of supergravity reactor one-step synthesis
Fluid process is acutely sheared and is crushed, and generates huge and quick newer boundary so that microcosmic mix obtains with mass transport process
Great reinforcing, the microcosmic uniformly mixed characteristic time is 10-100 μ s in supergravity reactor, heavy much smaller than Traditional liquid phase
It forms sediment the induction Nucleation characteristics time reacted.That is, by hypergravity reaction technology, zeroth order Fe nanometer particles are in crystallization nucleation
Before, uniform degree of supersaturation is had reached in reactor, therefore the nucleation of prepared Zero-valent Iron and growth are uniform at one
It is carried out under conditions of degree of supersaturation, meets desired homogeneous into nuclear environment, control nucleation process, particle is made to show relatively narrow distribution
Therefore the grain size of prepared nano material is smaller, particle diameter distribution is uniform；In addition, by high-gravity technology, cellulose modified nanometer
Zero-valent iron particle may be implemented continuously to prepare, and production efficiency can reach 0.056 ~ 5.60 Kg/h, this is common stirred tank
What method was difficult to realize, industrial applications foreground outclass traditional reaction kettle paddling process.Hypergravity reaction of the present invention is altogether
The precipitation method are to control the forming process of nano material by controlling the nanoparticle nucleated crystallization time of Zero-valent Iron.
Beneficial effects of the present invention：
The present invention reacts the supergravity reactor with powerful microcosmic composite character applied to quick chemical precipitation, while profit
Use the cellulose of biomass as the dispersant and surface modifier of zeroth order iron nano-particle, the nano zero valence iron of preparation, which has, to be divided
Dissipate property is good, stability is good, reactivity is high, preparation method is simple, manufacturing cost is low, can continuous batch prepare, therefore with prominent
The industrial applications foreground gone out.It is expected to be widely used in the necks such as environment remediation, magnetic catalysis, magnetic recording, magnetorheological, magnetic resonance imaging
Domain.
The present invention introduces three kinds of different natural polymer cellulose derivatives, the zeroth order iron nano-particle point of preparation respectively
Scattered property is good, has good stability, reactivity height, it is expected to be widely used in the fields such as environmental protection, biological medicine, chemical industry.
Description of the drawings
Fig. 1 is hypergravity preparation facilities figure of the present invention.
Fig. 2 is that the TEM of 1 obtained Modified by Carboxymethyl Cellulose nano zero valence iron of embodiment schemes.
Fig. 3 is the X-ray diffractogram of 1 obtained Modified by Carboxymethyl Cellulose nano zero valence iron of embodiment.
Fig. 4 is the infrared spectrogram of 1 obtained Modified by Carboxymethyl Cellulose nano zero valence iron of embodiment.
In figure：1- molysite storage tanks;2- centrifugal pumps；3- valves；4- spinner flowmeters；5- supergravity reactors；6- products store up
Slot；7- reducing agent storage tanks.
Specific implementation mode
It is further illustrated the present invention below by embodiment, but is not limited to following embodiment.
The positions Fig. 1 hypergravity preparation facilities provided by the invention for preparing cellulose modified nano zero valence iron, including hypergravity
Reactor 5, molysite storage tank 1, reducing agent storage tank 7, molysite storage tank 1 and reducing agent storage tank 7 are separately connected supergravity reactor 5, even
It takes over road and is respectively equipped with centrifugal pump 2 and spinner flowmeter 4, pass through centrifugal pump control fiber element and molysite mixed solution and reduction
The flow of agent solution is equal；Distributor is equipped in supergravity reactor 5, control fiber element and molysite mixed solution and reducing agent are molten
Liquid is mixed；5 bottom of supergravity reactor is equipped with product storage tank 6.
Specific experiment step is：The mixed solution and reducing agent solution of cellulose and molysite are added separately to molysite storage tank
1 and reducing agent storage tank 7 in, start centrifugal pump material liquid is conveyed into through spinner flowmeter 4 in supergravity reactor 5, constant speed
Two strands of material liquids enter the rotor of rotation by liquid distribution trough, and liquid flows through rotation from inside to outside under the influence of centrifugal force
Rotor, and the hybrid reaction in rotor.Final reaction product is thrown on shell under the influence of centrifugal force, under gravity
It is pooled to outlet discharge.
Embodiment 1：
A kind of hypergravity preparation method of cellulose modified nano zero valence iron, by the mixed solution and reducing agent of cellulose and molysite
It is sent into supergravity reactor and reacts simultaneously, Magneto separate reaction product, deionized water are cleaned to neutrality, very repeatedly after reaction
Sky is dried to obtain cellulose modified nano zero-valence iron particle, is as follows：
Fig. 1 is that Modified by Carboxymethyl Cellulose nano zero-valence is prepared by reactor of Impinging Stream-Rotating Packed Bed shown in the embodiment
The experiment flow figure of iron particle, the specific steps are：The carboxymethyl cellulose for weighing 2 g is dissolved in 1L water and is configured to carboxymethyl cellulose
The aqueous solution of element a concentration of 0.2%, is added the FeCl of 39.76 g thereto2•4H2It is 0.2 mol/ that O, which is configured to ferrous ion concentration,
The iron salt solutions of L；In addition, pressing BH4 -Molar ratio with ferrous ion is 2.5:1, weigh 18.92 g NaBH4It is dissolved in 1L water and matching
NaBH is made4The aqueous solution of a concentration of 0.5 mol/L；By above-mentioned carboxymethyl cellulose and molysite mixed solution and NaBH4Aqueous solution
It is added separately in storage tank, starts centrifugal pump and liquid is conveyed into Impinging Stream-Rotating Packed Bed agent set through spinner flowmeter
Interior, two strands of isometric reaction masses are ejected into rotary packed bed inner edge after being hit by the nozzle constant speed of liquid distribution trough
On, under the influence of centrifugal force along the outside edge flowing of filler hole, and reaction is mutually mixed in packing layer.Finally, reaction production
Object is thrown to from the outer rim of filler on shell under the influence of centrifugal force, is pooled to exit under gravity, is arranged through outlet
Go out.It is 60 L/h to adjust the volume flow of two kinds of material liquids in the process, and the rotating speed for controlling Impinging Stream-Rotating Packed Bed is
1000 rpm；After reaction, it using magnetic separation technique collecting reaction product, is cleaned repeatedly with deionized water to neutrality, vacuum
It is dried to obtain Modified by Carboxymethyl Cellulose nano zero-valence iron particle.
Fig. 2 shows the TEM figures of the Modified by Carboxymethyl Cellulose nano zero-valence iron particle of embodiment synthesis, can from figure
To find out that the grain size of Modified by Carboxymethyl Cellulose nano zero-valence iron particle is about 11 nm, particle size is uniform, favorable dispersibility.
Fig. 3 is the X-ray diffractogram for the Modified by Carboxymethyl Cellulose nano zero-valence iron particle that the embodiment 1 obtains.It can from figure
Go out, Modified by Carboxymethyl Cellulose nano zero-valence iron particle α-Fe occurs 2 θ=44.85 °, 65.15 °0Characteristic diffraction peak, and not
It is the oxidation peak of iron that the XRD diagram of modified nano zero valence iron has an apparent peak, the peak at 2 θ=35.56 °, and corresponding
Place, Modified by Carboxymethyl Cellulose nano zero valence iron do not occur oxidation peak, illustrate that unmodified nano zero valence iron easily aoxidizes,
The introducing for also demonstrating carboxymethyl cellulose simultaneously is effectively protected nano zero valence iron and Zero-valent Iron is inhibited to be aoxidized.Fig. 4
Show the infrared spectrum of the Modified by Carboxymethyl Cellulose nano zero-valence iron particle prepared by the embodiment, as can be seen from the figure
The infrared spectrum of Modified by Carboxymethyl Cellulose nano zero valence iron is in 1284 and 1048 cm-1Corresponding to the C-H of carboxymethyl cellulose
Flexural vibrations peak, in 2846 and 2929 cm-1Corresponding to the symmetrical and asymmetric stretching vibration peak of methylene, in 582 cm-1It is right
It should be in the stretching vibration peak of Fe-O.Illustrate that carboxymethyl cellulose is successfully modified in Zero-valent Iron nano grain surface.
Embodiment 2：
A kind of hypergravity preparation method of cellulose modified nano zero valence iron, it includes the following steps：
The hydroxyethyl cellulose for weighing 1 g is dissolved in the aqueous solution that hydroxyethyl cellulose a concentration of 0.1% is configured in 1L water, Xiang Qi
13.52 g FeCl of middle addition3•6H2O is configured to the iron salt solutions that iron concentration is 0.05 mol/L；In addition, pressing BH4 -And iron
The molar ratio of ion is 4:1, weigh 10.79 g KBH4It is dissolved in 1L water and is configured to KBH4The aqueous solution of a concentration of 0.2 mol/L；
By above-mentioned hydroxyethyl cellulose and molysite mixed solution and KBH4Aqueous solution is added separately in storage tank, starts centrifugal pump by two kinds
Material liquid has liquid distribution trough to be delivered to rotary packed bed middle hybrid reaction respectively, adjusts the body of two kinds of material liquids in the process
Product flow is 20 L/h, and the rotating speed of adults power reactor is 100 rpm；After reaction, it is received using magnetic separation technique
Collect reaction product, is cleaned repeatedly with deionized water to neutrality, vacuum drying obtains hydroxyethyl cellulose modified nano zero valence iron
Particle.
Embodiment 3：
A kind of hypergravity preparation method of cellulose modified nano zero valence iron, it includes the following steps：
It weighs 10 g hypromellose and is dissolved in the aqueous solution for being configured to hypromellose a concentration of 1% in 1L water, to
278.03 g FeSO are wherein added4•7H2O is configured to the iron salt solutions that ferrous ion concentration is 1.0 mol/L；In addition, pressing BH4 -
Molar ratio with iron ion is 2:1, weigh 75.66 g NaBH4It is dissolved in 1 L water and is configured to NaBH4A concentration of 2.0 mol/L's
Aqueous solution；By above-mentioned hypromellose and molysite mixed solution and NaBH4Aqueous solution is added separately in storage tank 1 and 4, is opened
Liquid is conveyed into through spinner 3 in Impinging Stream-Rotating Packed Bed agent set 5 by dynamic centrifugal pump, isometric two bursts reactions
Material is ejected into after being hit by the nozzle constant speed of liquid distribution trough on rotary packed bed inner edge, under the influence of centrifugal force edge
The outside edge flowing of filler hole, and reaction is mutually mixed in packing layer.Finally, reaction product is under the influence of centrifugal force from filling out
The outer rim of material is thrown on shell, is pooled to exit under gravity, is discharged through outlet.Two kinds of originals are adjusted in the process
The volume flow of feed liquid is 100 L/h, and the rotating speed for controlling Impinging Stream-Rotating Packed Bed is 2500 rpm；After reaction, it adopts
With magnetic separation technique collecting reaction product, cleaned repeatedly with deionized water to neutrality, vacuum drying obtains hypromellose
Modified Nano zero-valent iron particle.
Embodiment 4：
A kind of hypergravity preparation method of cellulose modified nano zero valence iron, it includes the following steps：
It weighs 5 g carboxymethyl celluloses and is dissolved in the aqueous solution for being configured to carboxymethyl cellulose a concentration of 0.5% in 1L water, thereto
97.48 g Fe are added2(SO4)3•H2O is configured to the iron salt solutions that iron concentration is 0.5 mol/L；In addition, pressing BH4 -And iron
The molar ratio of ion is 3:1, weigh 80.91 g KBH4It is dissolved in 1L water and is configured to KBH4The aqueous solution of a concentration of 1.5 mol/L；
By above-mentioned carboxymethyl cellulose and molysite mixed solution and KBH4Aqueous solution is respectively placed in storage tank, by pumping respectively by two kinds of originals
Feed liquid is entered by liquid distribution trough in rotating bed with helix channel simultaneously, is reacted in super gravity field, is adjusted in the process
The volume flow of two kinds of material liquids of section is 40 L/h, and the rotating speed of adults power reactor is 600 rpm；After reaction,
Using magnetic separation technique collecting reaction product, cleaned repeatedly with deionized water to neutrality, vacuum drying obtains carboxymethyl cellulose
Modified Nano zero-valent iron particle.
Embodiment 5：
A kind of hypergravity preparation method of cellulose modified nano zero valence iron, it includes the following steps：
It weighs 7.5 g hydroxyethyl celluloses and is dissolved in the aqueous solution for being configured to ethoxy a concentration of 0.75% in 1L water, be added thereto
303 g Fe(NO3)3•9H2O is configured to the iron salt solutions that iron concentration is 0.75 mol/L；In addition, pressing BH4 -With iron ion
Molar ratio is 3.5:1, weigh 99.30 g NaBH4It is dissolved in 1 L water and is configured to NaBH4A concentration of 2.625 mol/L aqueous solutions；
By above-mentioned hydroxyethyl cellulose and molysite mixed solution and NaBH4Aqueous solution is added separately in storage tank, starts centrifugal pump by two
Kind of material liquid has liquid distribution trough to be delivered to rotary packed bed middle hybrid reaction respectively, adjusts two kinds of material liquids in the process
Volume flow is 80 L/h, and the rotating speed of adults power reactor is 1500 rpm；After reaction, using magnetic separation technique
Collecting reaction product is cleaned with deionized water repeatedly to neutrality, and vacuum drying obtains hydroxyethyl cellulose modified nano zero-valence
Iron particle.
Claims (9)
1. a kind of hypergravity preparation method of cellulose modified nano zero valence iron, it is characterised in that：By the mixed of cellulose and molysite
It closes solution and reducing agent is sent into supergravity reactor reacts simultaneously, Magneto separate reaction product, deionized water are anti-after reaction
Multiple cleaning to neutrality, vacuum drying obtains cellulose modified nano zero-valence iron particle.
2. the hypergravity preparation method of cellulose modified nano zero valence iron according to claim 1, it is characterised in that：Including
Following steps：
(1) cellulose and molysite mixed solution are prepared：It is 0.1% ~ 1% that cellulose derivative, which is dissolved in water to be configured to cellulose concentration,
Solution, molysite is then added and is configured to cellulose that iron ion or ferrous ion concentration are 0.05 ~ 1.0 mol/L and molysite
Mixed solution；The molysite is trivalent iron salt or ferrous salt；
(2) reducing agent solution is prepared：Use sodium borohydride or potassium borohydride for reducing agent, by BH4 -Molar ratio with iron ion is
2:1~4:1 prepares the aqueous solution that reductant concentration is 0.1 ~ 4.0 mol/L；
(3) synthetic cellulose modified Nano Zero-valent Iron：The mixed solution of cellulose and molysite, reducing agent aqueous solution are placed in respectively
In reservoir, two strands of isometric reaction masses, which are delivered to by liquid distribution trough in supergravity reactor, to be reacted, in office
Anticipate moment cellulose and molysite mixed solution with reducing agent aqueous solution is all to react generation after being mixed according to set proportion
The volume flow of cellulose modified nano zero-valence iron particle, two strands of material liquids of control is 20 ~ 100L/h, and supergravity reactor turns
Speed is in 100 ~ 2500 rpm；
(4) after reaction, reaction product is collected using magnetic separation technique, is cleaned repeatedly with deionized water to neutrality, vacuum
It is dried to obtain cellulose modified nano zero-valence iron particle.
3. the hypergravity preparation method of cellulose modified nano zero valence iron according to claim 2, it is characterised in that：It is described
Trivalent iron salt, ferrous salt are one kind in ferric sulfate, ferric nitrate, iron chloride, ferrous sulfate, ferrous nitrate, frerrous chloride.
4. the hypergravity preparation method of cellulose modified nano zero valence iron according to claim 2, it is characterised in that：It is described
Cellulose is a kind of in cellulose derivative, including carboxymethyl cellulose, hydroxyethyl cellulose, hydroxypropyl methyl cellulose.
5. a kind of hypergravity preparing cellulose modified nano zero valence iron using claim 1 ~ 4 any one of them preparation method
Preparation facilities, it is characterised in that：Including supergravity reactor, molysite storage tank, reducing agent storage tank, molysite storage tank and reducing agent storage tank
It is separately connected supergravity reactor, valve and spinner flowmeter are respectively equipped in connecting tube, distribution is equipped in supergravity reactor
Device, supergravity reactor bottom are equipped with product storage tank.
6. the hypergravity preparation facilities of cellulose modified nano zero valence iron according to claim 5, it is characterised in that：It is described
Supergravity reactor is any one of Impinging Stream-Rotating Packed Bed, rotary packed bed or rotating bed with helix channel.
7. the hypergravity preparation facilities of cellulose modified nano zero valence iron according to claim 5, it is characterised in that：It is described
Supergravity reactor is Impinging Stream-Rotating Packed Bed, starts centrifugal pump and raw material liq is conveyed into percussion flow-through spinner flowmeter
In rotary packed bed, two strands of isometric reaction masses are ejected into rotation filler after being hit by the nozzle constant speed of liquid distribution trough
On the inner edge of bed, under the influence of centrifugal force along the outside edge flowing of filler hole, and reaction is mutually mixed in packing layer；Most
Eventually, reaction product is thrown to from the outer rim of filler on shell under the influence of centrifugal force, is pooled to exit under gravity,
It is discharged through outlet.
8. the hypergravity preparation facilities of cellulose modified nano zero valence iron according to claim 5, it is characterised in that：It is used
Supergravity reactor is rotary packed bed, starts centrifugal pump and is conveyed into raw material liq in rotary packed bed through spinner flowmeter,
Two strands of isometric reaction masses are sprayed onto by the nozzle of trepanning on liquid distribution trough on filler, and liquid is under the influence of centrifugal force
It is flowed, and repeatedly cut by filler, coalescence and dispersion from rotor inner edge to rotor periphery along filler hole, it is mutual in packing layer
Hybrid reaction；Finally, reaction product is thrown to from filler outer rim on shell under the influence of centrifugal force, is collected under the effect of gravity
It is discharged to outlet.
9. the hypergravity preparation facilities of cellulose modified nano zero valence iron according to claim 5, it is characterised in that：It is used
Supergravity reactor is rotating bed with helix channel, starts centrifugal pump and raw material liq is conveyed into helical duct through spinner flowmeter
In type revolving bed, two strands of isometric reaction masses are entered by liquid distribution trough in helical duct, effect of the liquid in centrifugal force
It is flowed out from inside to outside along the rotor with spiral of Archimedes shape channel；And it is mutually mixed, reacts in helical duct；
Finally, reaction product is thrown to from rotor periphery on shell under the influence of centrifugal force, is pooled to outlet row under gravity
Go out.
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