CN104744731A - Preparation method of cellulose-based magnetic super-hydrophobic material - Google Patents
Preparation method of cellulose-based magnetic super-hydrophobic material Download PDFInfo
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Abstract
The invention discloses a preparation method of a cellulose-based magnetic super-hydrophobic material. The method comprises the following steps: dissolving bamboo pulp or wood pulp or cotton pulp by using a homogeneous dissolving reagent to obtain cellulose particles; freezing and drying the cellulose particles and magnetically modifying the cellulose particles to obtain magnetic cellulose particles; and carrying out alkylated modification on the magnetic cellulose particles, washing, freezing and drying the magnetic cellulose particles to obtain the cellulose-based magnetic super-hydrophobic material. By taking cellulose as a matrix, magnetic ferroferric oxide is loaded, so that the material is magnetic. Moreover, surface alkylated modification is carried out on the material, so that the material is endowed with a super-hydrophobic performance. The material can be used in the fields of buildings, bioengineering, chemistry and chemical engineering, environmental monitoring and the like.
Description
Technical field
The present invention relates to a kind of for superhydrophobic surface material field, specifically, relate to a kind of magnetic superhydrophobic fibers cellulosic material and preparation method thereof.
Background technology
When drop directly contacts with solid, the wettability of liquid can produce contact angle and hysteresis phenomenon at solid surface.When drop moves at solid surface, the power of this delayed generation one opposing liquid movement, causes drop to stick on material surface, and causes the problems such as serious surface contamination and corrosion thus.Therefore develop a kind of super-hydrophobic particulate material, be used for constructing super hydrophobic surface, have important practical significance.
Mierocrystalline cellulose is the natural polymer that occurring in nature enriches the most, and wide material sources are cheap, good biocompatibility and to have good mechanical property good.Suitable chemistry can be passed through or physical method is combined with inorganic magnetic material, form the magnetic functional material of special construction, particle can be manipulated under field drives, make it assemble and displacement to target site.After its modification is prepared into super-hydrophobic magnetic particle, this material not only has that production cost is low, less energy consumption, the advantage such as pollution-free, and has ultra-hydrophobicity (lotus leaf effect).
For this reason, the present invention discloses a kind of super-hydrophobic magnetic fibre cellulosic material, has magnetic and ultra-hydrophobicity concurrently, can be applied to the numerous areas such as building, biotechnology, chemical, environmental monitoring.
Summary of the invention
The object of the present invention is to provide a kind of novel magnetic superhydrophobic fibers cellulosic material and preparation method thereof.
For realizing object of the present invention, the technical scheme adopted is: described one
the preparation method of cellulose base magnetic super hydrophobic material, comprise the steps:
(1) cellulosic material is smashed, dissolved with homogeneous phase solubilising reagent, after high speed centrifugation, obtain upper strata clear viscous liquids; Water is added dropwise to upper strata clear viscous liquids, or upper strata clear viscous liquids is instilled in the mixed solution of this class 80/ whiteruss, produce cellulose particulates;
(2) the cellulose particulates powder that step (1) is obtained is placed in the mixing solutions of iron protochloride/iron(ic) chloride, adds ammoniacal liquor, obtain the cellulose particulates being loaded with magnetic ferroferric oxide;
(3) be dispersed in inert solvent at a year magnetic cellulose particulates, with alkylating reagent by its modification, through cleaning, after lyophilize, obtain super-hydrophobic magnetic cellulose particle.
Homogeneous phase solubilising reagent described in above-mentioned steps (1) be selected from the mixing solutions of sodium hydroxide/urea, the mixing solutions of lithium chloride/N,N-DIMETHYLACETAMIDE, 4-methylmorpholine-
n-oxide compound or ionic liquid, the cellulosic mass percent in cellulose particulates obtained in described step (1) is 0.1-8.0wt.%.
FeCl described in above-mentioned steps (2)
2/ FeCl
3feCl in mixing solutions
2concentration be 0.3-2.5wt.%, FeCl
3concentration be 0.8-6.4wt.%; FeCl in described mixing solutions
2with FeCl
3solid masses than for 1.0:2.0-3.2; FeCl in described mixing solutions
2and FeCl
3total solids quality and step (1) in the mass ratio of obtained cellulose particulates be 1.0-9.0:1.0.
Above-mentioned steps (2) described ammonia concn is 20 ~ 25wt.%, described ammoniacal liquor and described FeCl
2/ FeCl
3the volume ratio of mixing solutions is 1:12-24.
Inert solvent described in above-mentioned steps (3) is selected from any one in toluene, benzene, dimethylbenzene, pentane, hexane, hexanaphthene, chloroform; Inert solvent toluene be loaded with magnetic Fe
3o
4cellulose particulates in cellulosic mass ratio be 20-200:1.0.
The mass ratio of cellulose particulates obtained in the alkylating reagent described in above-mentioned steps (3) and step (1) is 0.05-5.0:1.0, described alkylating reagent is selected from octadecyl trimethoxysilane, hexadecyl trimethoxy silane, dodecyltrimethoxysilane, 1H, 1H, 2H, 2H-perfluoro capryl trimethyl silane, 1H, 1H, 2H, 2H-perfluoro decyl Trimethoxy silane, 1H, 1H, 2H, 2H-perfluorododecyl Trimethoxy silane, octadecyltriethoxy silane, hexadecyl, dodecyl triethoxysilane, 1H, 1H, 2H, 2H-perfluoro capryl triethoxyl silane, 1H, 1H, 2H, 2H-perfluoro decyl triethoxyl silane, 1H, 1H, 2H, 2H-perfluorododecyl triethoxyl silane, octadecyl trichlorosilane alkane, hexadecyl trichlorosilane, dodecyltrichlorosilane, 1H, 1H, 2H, 2H-perfluoro capryl trichlorosilane, 1H, 1H, 2H, 2H-perfluoro decyl trichlorosilane, 1H, 1H, 2H, any one of 2H-perfluorododecyl trichlorosilane.
Described cellulosic material has at least one to be selected from bamboo pulp, wood pulp, cotton pulp, jute pulp, bagasse pulp, straw pulp, mulberry root bark pulp or reed pulp, wherein content of cellulose >=85 wt.%, the cellulosic polymerization degree >=200.
Cellulosic mass percent in cellulose particulates obtained in described step (1) is preferably 1.0-6.0wt.%, FeCl in described mixing solutions
2with FeCl
3solid masses than be preferably 1.0:2.6; FeCl in described mixing solutions
2and FeCl
3total solids quality and step (1) in the mass ratio of obtained cellulose particulates be preferably 4.5:1.0; Described ammoniacal liquor and described FeCl
2/ FeCl
3the volume ratio of mixing solutions is preferably 1:18; Described inert solvent toluene be loaded with magnetic Fe
3o
4cellulose particulates in cellulosic mass ratio be preferably 50-100:1.0; The mass ratio of cellulose particulates obtained in the alkylating reagent described in step (3) and step (1) is preferably 0.5:1.0.
The carried magnetic Fe that above-mentioned preparation method obtains
3o
4cellulose base super hydrophobic material, for Powdered.
Specifically, a kind of magnetic superhydrophobic fibers cellulosic material material of the present invention and preparation method thereof, comprises the steps:
(1) adopt bamboo (wood or cotton) pulp, smash, be placed in NaOH/ urea soln or LiCl/DMAc solution or NMMO solution or ionic liquid, Mierocrystalline cellulose is dissolved completely.After high speed centrifugation, instilled by water in solution, washing and filtering, gained solid carries out lyophilize, obtains cellulose particulates; The mass percent concentration of described cellulose solution is 0.1-8.0wt.%, is preferably 1.0-4.0wt.%.
(2) or by the cellulosic pulp after centrifugal to (1) whiteruss and Si Ban 80(Span80 is instilled) in, solidification, obtains cellulose microsphere particle; The concentration of volume percent of described Span80 in whiteruss is 0.5-10.0%, is preferably 2.0-8.0%.
(3) cellulose particulates is placed in FeCl
2/ FeCl
3in mixing solutions, described FeCl
2/ FeCl
3feCl in mixing solutions
2and FeCl
3total mass and the mass ratio of cellulose particulates be 1.0-9.0:1.0, be preferably 4.5:1.0.
(4) in step (2), gained contains FeCl
2/ FeCl
3in/cellulosic liquid, add ammoniacal liquor, obtain Fe after washing after filtration
3o
4/ Mierocrystalline cellulose composite particles; The mass percent concentration of described ammonia soln is 10-30wt.%, described ammoniacal liquor and described FeCl
2/ FeCl
3the volume ratio of/cellulose mixed solution is 1:12-24; Be preferably 1:18.
(5) by gained Fe in step (4)
3o
4/ Mierocrystalline cellulose composite particles is dispersed in toluene or benzene or dimethylbenzene or pentane or hexane or hexanaphthene or chloroform, adds alkylating reagent, stirring reaction.Through cleaning, after lyophilize, obtain magnetic superhydrophobic fibers element particle.Described alkylating reagent is octadecyl trimethoxysilane (C
18h
37si (OCH
3)
3), hexadecyl trimethoxy silane (C
16h
37si (OCH
3)
3), dodecyltrimethoxysilane (C
12h
37si (OCH
3)
3), 1H, 1H, 2H, 2H-perfluoro capryl trimethyl silane (C
6f
13cH
2cH
2si (OCH
3)
3), 1H, 1H, 2H, 2H-perfluoro decyl Trimethoxy silane (C
8f
17cH
2cH
2si (OCH
3)
3), 1H, 1H, 2H, 2H-perfluorododecyl Trimethoxy silane (C
10f
21cH
2cH
2si (OCH
3)
3), octadecyltriethoxy silane (C
18h
37si (OC
2h
5)
3), hexadecyl (C
16h
37si (OC
2h
5)
3), dodecyl triethoxysilane (C
12h
37si (OC
2h
5)
3), 1H, 1H, 2H, 2H-perfluoro capryl triethoxyl silane (C
6f
13cH
2cH
2si (OC
2h
5)
3), 1H, 1H, 2H, 2H-perfluoro decyl triethoxyl silane (C
8f
17cH
2cH
2si (OC
2h
5)
3), 1H, 1H, 2H, 2H-perfluorododecyl triethoxyl silane (C
10f
21cH
2cH
2si (OC
2h
5)
3), octadecyl trichlorosilane alkane (C
18h
37siCl
3), hexadecyl trichlorosilane (C
16h
37siCl
3), dodecyltrichlorosilane (C
12h
37siCl
3), 1H, 1H, 2H, 2H-perfluoro capryl trichlorosilane (C
6f
13cH
2cH
2siCl
3), 1H, 1H, 2H, 2H-perfluoro decyl trichlorosilane (C
8f
17cH
2cH
2siCl
3), 1H, 1H, 2H, 2H-perfluorododecyl trichlorosilane (C
10f
21cH
2cH
2siCl
3) any one.Inert solvent toluene and cellulosic mass ratio are 20-200:1.0, are preferably 50-100:1.0.Alkylating reagent and cellulosic mass ratio are 0.05-5.0:1.0, are preferably 0.5:1.0.
The cellulosic material that the present invention adopts can be selected from bamboo pulp or the raw material such as wood pulps or Cotton Pulp, owing to the object of the invention is to get its Mierocrystalline cellulose, as long as fiber therefore wherein have or the raw material such as commercially available bamboo pulp, wood pulp, cotton pulp, jute pulp, bagasse pulp, straw pulp, mulberry root bark pulp or the reed pulp that can reach more than 85wt.% better, all can be used as preparation of the present invention "
cellulose base magnetic super hydrophobic material" raw material, the preferred bamboo of cellulosic material of the present invention (wood or cotton) pulp, wherein content of cellulose>=85 wt.%, the cellulosic polymerization degree>=200.
One of the present invention
cellulose base magnetic super hydrophobic material, prepared by aforesaid method.
First innovative point of aforesaid method of the present invention is: select nature abundant natural polymer--Mierocrystalline cellulose is that basic raw material is to prepare super hydrophobic material.Mierocrystalline cellulose has the advantage such as cheap and easy to get, environmental friendliness, excellent biodegradability.For the biocompatibility of material and the strategy of sustainable development demand of environment, make full use of and develop Mierocrystalline cellulose and its range of application is extended in the preparation of super hydrophobic material, utilize Mierocrystalline cellulose as the unique advantage of base material, be of great practical significance.
Second innovative point is that load is magnetic particle on cellulose particulates, makes particle have magnetic, can manipulate particle under field drives, make it assemble with displacement to target site.
3rd innovative point is that magnetic cellulose particle has ultra-hydrophobicity (lotus leaf effect).After being built into a hydrophobic surface layer, water droplet naturally tumbles on particle surface layer, and can take away the dust pollutant on surface, makes base material have significant waterproof and self-cleaning effects.
The preparation of current magnetic cellulose based super hydrophobic material not yet has bibliographical information.
Accompanying drawing explanation
Fig. 1 is the Flied emission Electronic Speculum figure of the magnetic superhydrophobic fibers cellulosic material of cellulose base particle prepared by embodiments of the invention 1,2.
Fig. 1-1 is the Flied emission Electronic Speculum figure of the magnetic superhydrophobic fibers cellulosic material of cellulose base particle prepared by embodiments of the invention 3,4.
Fig. 2 is the picture of the super-hydrophobic particle of arbitrary obtained magnetic movement under field drives in embodiment of the present invention 1-4.
Water droplet is dropped in the spring picture on the super hydrophobic surface of arbitrary obtained superhydrophobic fibers cellulosic material structure in embodiment of the present invention 1-4 by Fig. 3.
Embodiment
Below in conjunction with embodiment, the inventive method is described in further detail.It should be noted that, protection scope of the present invention should include but not limited to the technology contents disclosed in the present embodiment.
Embodiment 1
(1) (bamboo pulp is selected from Sichuan nandina bamboo resource development corporation, Ltd. to get the business bamboo pulp that 2g smashes, its content of cellulose >=95wt.%), soak after one day in 1000mL water, the product after filtration joins in 500mL DMAc solution and soaks, filter, three times repeatedly.Being joined 200mL concentration is again (mass ratio of LiCl solid and DMAc liquid is 2:23) in 8 wt.% LiCl/DMAc solution, is heated to 60 ° of C vigorous stirring and makes cellulose dissolution.Be added dropwise to by 750mL ultrapure water in described cellulose solution, washing, lyophilize, obtains cellulose powder particle.
(2) 1g cellulose powder particle being joined 50mL, to contain concentration be 1.3wt.% FeCl
2with 3.2 wt.% FeCl
3in mixing solutions, instillation 2.8mL concentration is that the ammoniacal liquor of 25wt.% reacts 120 min at normal temperatures, and washing, lyophilize, obtains being loaded with Fe
3o
4magnetic cellulose particle.
(3) by step (2) gained containing Fe
3o
4cellulose particulates join in 50mL toluene, add 0.5mL octadecyl trimethoxysilane (C
18h
37si (OCH
3)
3), react three days at normal temperatures, filter, dry, obtain magnetic superhydrophobic fibers element particle.
Embodiment 2
(1) (bamboo pulp is selected from Sichuan nandina bamboo resource development corporation, Ltd. to get the business bamboo pulp that 2g smashes, its content of cellulose >=95wt.%), joining 200mL concentration is in the NMMO solution of 75%, vigorous stirring, and is heated to 110 ° of C and makes cellulose dissolution.Be added dropwise to by 750mL ultrapure water in thick transparent liquid and cellulose solution, washing, lyophilize, obtains cellulose powder particle.
(2) 1g cellulose powder particle being joined 50mL, to contain concentration be 1.3wt.% FeCl
2with 3.2 wt.% FeCl
3in mixing solutions, instillation 2.8mL concentration is that the ammoniacal liquor of 25wt.% reacts 120 min at normal temperatures, and washing, lyophilize, obtains being loaded with Fe
3o
4magnetic cellulose particle.
(3) step (2) gained is contained Fe
3o
4magnetic cellulose particle join in 50mL toluene, add 0.5mL 1H, the fluorine-containing octyl trimethyl silane of 1H, 2H, 2H-(C
6f
13cH
2cH
2si (OCH
3)
3), react three days at normal temperatures, filter, dry, obtain magnetic superhydrophobic fibers element particle.
Embodiment 3
(1) following Mierocrystalline cellulose NaOH/ urea system prepares method reference literature (Luo, the X. of magnetic microsphere; Liu, S.; Zhou, J.; Zhang, L. In situ synthesis of Fe
3o
4/ cellulose microspheres with magnetic-induced protein delivery. J. Mater. Chem. 2009,19,3538) described method.(wood pulps is selected from Qingshan Paper limited-liability company of Fujian Province to get the business wood pulps that 11g smashes, its content of cellulose >=93wt.%), joining 200mL is chilled in the NaOH/ urea soln (the NaOH solid wherein contained and the mass ratio of urea are 7:12) of-13 ° of C in advance, vigorous stirring makes cellulose dissolution, obtains the thick transparent liquid in upper strata after 8000r/min is centrifugal.By in the cellulose solution of thick transparent liquid instillation 400mL Span80/ whiteruss mixing solutions (volume ratio of Span80/ whiteruss is 1:20), stir 8 hours, washing, lyophilize, obtains cellulose microsphere particle.
(2) 1g cellulose powder particle being joined 50mL, to contain concentration be 1.3wt.% FeCl
2with 3.2 wt.% FeCl
3in mixing solutions, instillation 2.8mL concentration is that the ammoniacal liquor of 25wt.% reacts 120 min at normal temperatures, and washing, lyophilize, obtains being loaded with Fe
3o
4magnetic cellulose particle.
(3) step (2) gained is contained Fe
3o
4magnetic cellulose particle join in 50mL toluene, add 0.5mL octadecyltriethoxy silane (C
18h
37si (OC
2h
5)
3), react three days at normal temperatures, filter, dry, obtain magnetic superhydrophobic fibers element particle.
Embodiment 4
(1) following Mierocrystalline cellulose NaOH/ urea system prepares method reference literature (Luo, the X. of magnetic microsphere; Liu, S.; Zhou, J.; Zhang, L. In situ synthesis of Fe
3o
4/ cellulose microspheres with magnetic-induced protein delivery. J. Mater. Chem. 2009,19,3538) described method.(Cotton Pulp is selected from Hu'nan Tuopu Bamboo & Ramie Industrial Development Co., Ltd. to get the business Cotton Pulp that 11g smashes, its content of cellulose >=97wt.%), joining 200mL is chilled in the NaOH/ urea soln (wherein the mass ratio of NaOH solid and urea is 7:12) of-13 ° of C in advance, vigorous stirring makes cellulose dissolution, obtains the thick transparent liquid in upper strata after 8000r/min is centrifugal.By in the cellulose solution of thick transparent liquid instillation 400mL Span80/ whiteruss mixing solutions (wherein the volume ratio of Span80/ whiteruss is 1:20), stir 8 hours, washing, lyophilize, obtains cellulose microsphere particle.
(2) powder of 1g cellulose microsphere particle being joined 50mL, to contain concentration be 1.3wt.% FeCl
2with 3.2 wt.% FeCl
3in mixing solutions, instillation 2.8mL concentration is that the ammoniacal liquor of 25wt.% reacts 120 min at normal temperatures, and washing, lyophilize, obtains being loaded with Fe
3o
4magnetic cellulose particle.
(3) step (2) gained is contained Fe
3o
4magnetic cellulose particle join in 50mL toluene, add 0.5mL 1H, the fluorine-containing octyl group triethyl silicane of 1H, 2H, 2H-, (C
6f
13cH
2cH
2si (OC
2h
5)
3), react three days at normal temperatures, filter, dry, obtain magnetic superhydrophobic fibers element particle.
Salient features is tested
Magnetic superhydrophobic fibers cellulosic material prepared by the present invention, its important feature is that material has magnetic and super-hydrophobic dual property, therefore measures the microscopic pattern of this material, magnetic and ultra-hydrophobicity.
Super hydrophobic material (powdered sample) form (Fig. 1): it is the powdered material that embodiment 1 and 2 is produced, and is erose nanoparticle, through laser particle analyzer test, its particle diameter is at about 10 μm.The powdered material that embodiment 3 and 4 is produced is microspheroidal, and its particle diameter is at about 30 μm, and its form is shown in Fig. 1-1.
As shown in Figure 2, magnetic cellulose basal granule obtained for either method in embodiment of the present invention 1-4 can the schematic diagram of qualitative movement under magnetic field.Apply a magnetic field in one end of particle, particle moves with stirring magneton under the driving in magnetic field.
Cellulose base particle in all embodiments has ultra-hydrophobicity.
Embodiment 5
Obtained particle double faced adhesive tape arbitrary in embodiment of the present invention 1-4 is bonded at any solid (glass, plank, stone etc.) on the surface, makes solid have water resistance.As shown in Figure 3, be coated in the one side of double faced adhesive tape by super-hydrophobic uniform particle, now on double faced adhesive tape, the super-hydrophobic particle of cellulose base is built into the super-hydrophobic layer of thin layer.Again the magnetic particle being loaded with double faced adhesive tape is bonded on glass, is built into a super hydrophobic surface.When water droplet is dropped on particle, water droplet bounces in cellulose base particle super-hydrophobic layer, can not adhere on a solid surface, has significant lotus leaf effect.
In addition, when upper layer is by Substances Pollution such as dust, when water droplet is dropped on the surface, can rolls and take away dust pollution thing.Thus make hydrophobic particles layer have cleaning effect.
Claims (9)
1. a preparation method for cellulose base magnetic super hydrophobic material, comprises the steps:
(1) cellulosic material is smashed, dissolved with homogeneous phase solubilising reagent, after high speed centrifugation, obtain upper strata clear viscous liquids; Water is added dropwise to upper strata clear viscous liquids, or upper strata clear viscous liquids is instilled in the mixed solution of this class 80/ whiteruss, produce cellulose particulates;
(2) the cellulose particulates powder that step (1) is obtained is placed in the mixing solutions of iron protochloride/iron(ic) chloride, adds ammoniacal liquor, obtain the cellulose particulates being loaded with magnetic ferroferric oxide;
(3) be dispersed in inert solvent at a year magnetic cellulose particulates, with alkylating reagent by its modification, through cleaning, after lyophilize, obtain super-hydrophobic magnetic cellulose particle.
2. preparation method according to claim 1, is characterized in that: the homogeneous phase solubilising reagent described in step (1) be selected from the mixing solutions of sodium hydroxide/urea, the mixing solutions of lithium chloride/N,N-DIMETHYLACETAMIDE, 4-methylmorpholine-
n-oxide compound or ionic liquid, the cellulosic mass percent in cellulose particulates obtained in described step (1) is 0.1-8.0wt.%.
3. preparation method according to claim 1, is characterized in that: the FeCl described in step (2)
2/ FeCl
3feCl in mixing solutions
2concentration be 0.3-2.5wt.%, FeCl
3concentration be 0.8-6.4wt.%; FeCl in described mixing solutions
2with FeCl
3solid masses than for 1.0:2.0-3.2; FeCl in described mixing solutions
2and FeCl
3total solids quality and step (1) in the mass ratio of obtained cellulose particulates be 1.0-9.0:1.0.
4. preparation method according to claim 1, is characterized in that: step (2) described ammonia concn is 20 ~ 25wt.%, described ammoniacal liquor and described FeCl
2/ FeCl
3the volume ratio of mixing solutions is 1:12-24.
5. preparation method according to claim 1, is characterized in that: the inert solvent described in step (3) is selected from any one in toluene, benzene, dimethylbenzene, pentane, hexane, hexanaphthene, chloroform; Inert solvent toluene be loaded with magnetic Fe
3o
4cellulose particulates in cellulosic mass ratio be 20-200:1.0.
6. preparation method according to claim 1, is characterized in that: the mass ratio of cellulose particulates obtained in the alkylating reagent described in step (3) and step (1) is 0.05-5.0:1.0, described alkylating reagent is selected from octadecyl trimethoxysilane, hexadecyl trimethoxy silane, dodecyltrimethoxysilane, 1H, 1H, 2H, 2H-perfluoro capryl trimethyl silane, 1H, 1H, 2H, 2H-perfluoro decyl Trimethoxy silane, 1H, 1H, 2H, 2H-perfluorododecyl Trimethoxy silane, octadecyltriethoxy silane, hexadecyl, dodecyl triethoxysilane, 1H, 1H, 2H, 2H-perfluoro capryl triethoxyl silane, 1H, 1H, 2H, 2H-perfluoro decyl triethoxyl silane, 1H, 1H, 2H, 2H-perfluorododecyl triethoxyl silane, octadecyl trichlorosilane alkane, hexadecyl trichlorosilane, dodecyltrichlorosilane, 1H, 1H, 2H, 2H-perfluoro capryl trichlorosilane, 1H, 1H, 2H, 2H-perfluoro decyl trichlorosilane, 1H, 1H, 2H, any one of 2H-perfluorododecyl trichlorosilane.
7. the preparation method according to claim 1 or 2 or 3 or 4 or 5 or 6, it is characterized in that: described cellulosic material has at least one to be selected from bamboo pulp, wood pulp, cotton pulp, jute pulp, bagasse pulp, straw pulp, mulberry root bark pulp or reed pulp, wherein content of cellulose >=85 wt.%, the cellulosic polymerization degree >=200.
8. the preparation method according to claim 1 or 2 or 3 or 4 or 5 or 6, is characterized in that: the cellulosic mass percent in cellulose particulates obtained in described step (1) is 1.0-6.0wt.%, FeCl in described mixing solutions
2with FeCl
3solid masses than for 1.0:2.6; FeCl in described mixing solutions
2and FeCl
3total solids quality and step (1) in the mass ratio of obtained cellulose particulates be 4.5:1.0; Described ammoniacal liquor and described FeCl
2/ FeCl
3the volume ratio of mixing solutions is 1:18; Described inert solvent toluene be loaded with magnetic Fe
3o
4cellulose particulates in cellulosic mass ratio be 50-100:1.0; The mass ratio of cellulose particulates obtained in the alkylating reagent described in step (3) and step (1) is 0.5:1.0.
9. the carried magnetic Fe that obtains of the arbitrary described preparation method of a claim 1-8
3o
4cellulose base super hydrophobic material, for Powdered.
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| CN106475067A (en) * | 2016-11-08 | 2017-03-08 | 华南理工大学 | A kind of silicon dioxide/fibrin magnetic foam and preparation method thereof |
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| CN108560246A (en) * | 2018-05-05 | 2018-09-21 | 汕头市雪果制衣实业有限公司 | A kind of preparation method of the water-fastness bamboo fibre fabric of the pro-skin of children |
| CN109054101A (en) * | 2018-07-06 | 2018-12-21 | 福建农林大学 | A kind of super-hydrophobic magnetic Nano cellulose and preparation method thereof |
| CN109054101B (en) * | 2018-07-06 | 2021-04-09 | 福建农林大学 | Super-hydrophobic magnetic nanocellulose and preparation method thereof |
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| CN111116762A (en) * | 2020-01-10 | 2020-05-08 | 天津科技大学 | Preparation method of hydrophobic cellulose nanocrystals |
| CN111116762B (en) * | 2020-01-10 | 2022-02-18 | 天津科技大学 | Preparation method of hydrophobic cellulose nanocrystals |
| CN111471521A (en) * | 2020-03-16 | 2020-07-31 | 浙江工业大学 | Refining method for extracting safflower camellia seed oil by aqueous enzymatic method |
| CN112791703A (en) * | 2020-12-25 | 2021-05-14 | 广东工业大学 | Kapok fiber-based magnetic composite material and preparation method and application thereof |
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