CN107262070A - A kind of preparation method of magnetic cellulose/polyglutamic acid coupling material - Google Patents

A kind of preparation method of magnetic cellulose/polyglutamic acid coupling material Download PDF

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Publication number
CN107262070A
CN107262070A CN201710699412.2A CN201710699412A CN107262070A CN 107262070 A CN107262070 A CN 107262070A CN 201710699412 A CN201710699412 A CN 201710699412A CN 107262070 A CN107262070 A CN 107262070A
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cellulose
polyglutamic acid
magnetic
coupling
ultra
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CN201710699412.2A
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Chinese (zh)
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王慧
王玉富
郭媛
邱财生
龙松华
郝冬梅
钟国乾
许雯雯
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中国农业科学院麻类研究所
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Priority to CN201710699412.2A priority Critical patent/CN107262070A/en
Publication of CN107262070A publication Critical patent/CN107262070A/en

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    • 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
    • B01J20/0203Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/0225Compounds of Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt
    • B01J20/0229Compounds of Fe
    • 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
    • B01J20/0203Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/0274Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04 characterised by the type of anion
    • B01J20/0281Sulfates of compounds other than those provided for in B01J20/045
    • 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
    • B01J20/0203Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/0274Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04 characterised by the type of anion
    • B01J20/0288Halides of compounds other than those provided for in B01J20/046
    • 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
    • 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
    • B01J20/22Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/26Synthetic macromolecular compounds
    • 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

Abstract

The present invention relates to a kind of preparation method of magnetic cellulose/polyglutamic acid coupling material charcoal is prepared first with the bluish dogbane stem removed the peel, polyglutamic acid is recycled to prepare cellulose modified material, magnetic particle is loaded into cellulose modified material surface again and prepares magnetic cellulose coupling material, the magnetic cellulose coupling material of preparation possesses more preferable physicochemical property and is easy to separation of solid and liquid and recycling.Magnetic cellulose coupling material prepared by the present invention has huge specific surface area and abundant active group is contained on surface, can be applied in various fields, and more extensive approach is provided for the recycling of bluish dogbane.

Description

A kind of preparation method of magnetic cellulose/polyglutamic acid coupling material

Technical field

The invention belongs to field of functional materials, and in particular to a kind of preparation method of cellulose composite material.

Background technology

Cellulose is natural organic renewable resource the abundantest on the earth, is mainly derived from cotton, wood, numb and various rice The strings such as bar, often and hemicellulose, lignin, pectic substance etc. mix the main body of composition string.Cellulose For high molecular polymer, using glucose as unit, pass through, the interconnection of glycosidic bond, the long chain of line style being polymerized divides greatly Son, its chemical constitution is as shown in the figure.It can be seen that cellulose is because intramolecular is containing the big parent of many porous, specific surface areas The light base group of water and with certain affine adsorptivity, can directly using natural cellulosic material as adsorbent removal metal from Son..

Native cellulose heavy metal ion has certain adsorption capacity, but simultaneously not bery strong, and adsorption capacity is small, choosing Selecting property is low, but has more preferable adsorption capacity by modified cellulose, therefore, and cellulose modified thing turns into a kind of performance Fabulous sorptive material.Polyglutamic acid be it is a kind of can not only have in the amino acid polymer structure of Microbe synthesis it is big The energy of adsorption of heavy metal cation after amount-COOH reaction active groups, also substantial amounts of-NH- active groups, modified cellulose Power is greatly enhanced, and current relevant report both domestic and external is less.Polyglutamic acid is grafted onto to the table of cellulose by certain method Face, prepares a kind of new cellulose modified material, assigns magnetic to it again in addition, assigns the preferably materialization of bastose element Matter, more extensive approach is provided for the application in various fields of bastose element.

The content of the invention

The technical problems to be solved by the invention are:The technical problem existed for prior art, develops a kind of technique letter Preparation method that is single and preparing the plain coupling material of quick bastose.

In order to solve the above technical problems, technical scheme is as follows:

A kind of preparation method of cellulose composite material, comprises the following steps:

Step 1: preparing or purchase cellulose, the cellulose of alkalization is prepared;

Step 2: preparing cellulose/polyglutamic acid composite using the cellulose of polyglutamic acid and alkalization;

Coupled Step 3: magnetic particle is loaded into cellulose modified material surface and prepares magnetic cellulose/polyglutamic acid Material.

2. the preparation method of cellulose composite material as claimed in claim 1, it is characterised in that in the step one, The method for preparing alkalinized celluloses is as follows:

A. the stem after bluish dogbane is removed the peel, 1-4h is dried at 70-90 DEG C, is ground to 100-150 μm, then clear with ultra-pure water Wash, 50-75 DEG C of drying 1-3h obtains powdered product

B. powdered product is taken to be distributed in n-hexane, the solid-to-liquid ratio of powdered product and n-hexane is 5-10:40-800g/ Ml30-60 DEG C of heating 1-4h, removes vegetable wax;

C. by the bastose of dewaxing be added to molar concentration be 1-5mol/L sodium hydroxide solution in, powdered product with The solid-to-liquid ratio of sodium hydroxide solution is 5-10:Filtration product is filtered to obtain after 400-600g/ml, 20-30 DEG C of vibration 10-48h, respectively Filtration product is cleaned with ultra-pure water, ethanol and methanol successively, 1-4h is dried at 50-70 DEG C, room temperature is cooled to and obtains at alkalization The bastose element of reason;

Further to improve, in the step 2, the preparation method of cellulose/polyglutamic acid composite is as follows:

D. the bastose element and polyglutamic acid, the bastose of basification and the matter of polyglutamic acid of basification are weighed Amount is than being 1-3:2-6;10-40min is ground under infrared lamp after mixing, uniform fine-powder is obtained;

E. the use of dimethyl sulfoxide is cosolvent, ultrasonic agitation 20-40min makes it be dispersed in dimethylsulfoxide solvent body In system, oil bath heating is recycled to be warming up to 110-125 DEG C, stirring, enriching sulfuric acid is reacted as catalyst, reaction 4-8h Thing, wherein, the volume ratio of the concentrated sulfuric acid and dimethylsulfoxide solvent is 1-10:20;By the filtering of obtained reactant, filter residue is utilized successively Ethanol, deionized water are cleaned to neutrality;

F. washed, then dried at 70-85 DEG C with ethanol and acetone successively, modified cellulose/polyglutamic acid is made The solid-to-liquid ratio of composite, fine-powder and dimethyl sulfoxide is:3-9:20g/ml.

It is further to improve, in the step 3, the following institute of preparation method of magnetic cellulose/polyglutamic acid coupling material Show:

G. FeCl is taken3·6H2O and/or FeSO4·4H2Being dissolved at ambient temperature in ultra-pure water for O obtains mixing molten Liquid;2-10g celluloses/polyglutamic acid composite is added in mixed solution, controls temperature to be stirred for 75-90 DEG C in water-bath Mix 1-4 minutes, then add ammoniacal liquor and adjust pH to 9.8-10.2, continue to stir 35-50 minutes, obtained mixed liquor is cooled down, point From sediment and wash, obtain magnetic cellulose/polyglutamic acid coupling material, wherein, cellulose/polyglutamic acid composite with The solid-to-liquid ratio of ultra-pure water is 2-10:50-200g/ml;FeCl3·6H2O and FeSO4·4H2O mol ratio is 0-0.02:0- 0.01;FeCl3·6H2O and FeSO4·4H2O total amount and the molal volume ratio of ultra-pure water are:0.001-0.03:50- 200mol/ml。

Specific material amounts scope and step are as follows in experiment:

The preparation method of the plain coupling material of bastose is provided, cellulose is prepared first with the bluish dogbane stem removed the peel, then Cellulose modified material is prepared using polyglutamic acid, then magnetic particle is loaded into cellulose modified material surface and prepares magnetic fibre The plain coupling material of dimension, the magnetic cellulose coupling material of preparation possesses more preferable physicochemical property and is easy to separation of solid and liquid and profit again With comprising the following steps that:

(1) stem after bluish dogbane is removed the peel, dries 1-4h at 70-90 DEG C, is ground to 100-150 μm, then is cleaned with ultra-pure water, 50-75 DEG C of drying 1-3h, takes 5-10g to be distributed in 40-800ml n-hexanes obtained powdered product, 30-60 DEG C of heating 1- 4h, removes vegetable wax, then the bastose of dewaxing is added into the sodium hydroxide that 400-600ml molar concentrations are 1-5mol/L In, filtered after 20-30 DEG C of vibration 10-48h, cleaned with substantial amounts of ultra-pure water, ethanol and methanol, 1-4h is dried at 50-70 DEG C, It is cooled to the bastose element that room temperature obtains basification.

(2) (monomer mole ratio is about with 2.0-6.0g polyglutamic acids by the bastose element 1.0-3.0g for weighing obtained by step (1) 1:10-40min is fully ground under infrared lamp after 2.5-3) mixing, uniform fine-powder is obtained, is with 20ml dimethyl sulfoxides Cosolvent, ultrasonic agitation 20-40min is made it be dispersed in dimethylsulfoxide solvent system, is warming up to using oil bath heating 110-125 DEG C, stirring adds the 1-10ml concentrated sulfuric acids as catalyst, reacts 4-8h, obtained reactant is filtered, filter residue profit Cleaned with ethanol, deionized water to neutrality, finally with ethanol and acetone once washing, then the drying at 70-85 DEG C, it is made and is modified Cellulose afterwards/polyglutamic acid composite.

(3) 0.005-0.02mol FeCl36H2O and 0.001-0.01mol FeSO44H2O is taken in room temperature condition Under be dissolved in 50-200ml ultra-pure waters, obtained mixed solution is added to the 1.0-4.0g celluloses of step (2) preparation/poly- In glutamic acid composite, control temperature to be stirred 1-4 minutes rapidly for 75-90 DEG C in water-bath, be then rapidly added ammoniacal liquor PH to 9.8-10.2 or so is adjusted, continues to stir 35-50 minutes, obtained mixed liquor is cooled down, sediment separate out is simultaneously washed, obtained Magnetic cellulose/polyglutamic acid coupling material.Compared with prior art, the advantage of the invention is that:

1. the raw material sources used in the cellulose coupling material preparation process of the present invention are extensively, and cheap, mainly Raw material is conventional chemical products.

2. product prepared by the method for the present invention is nontoxic, environmentally friendly.

3. the preparation technology of the cellulose coupling material of the present invention is simple and convenient to operate, it is easy to accomplish industrialized production.

4. the cellulose coupling material of the present invention has huge specific surface area, and surface active groups are abundant, and molten Separation of solid and liquid can be quickly realized in liquid, new approach is provided for bluish dogbane recycling.

Brief description of the drawings

Fig. 1 be the embodiment of the present invention 2 cellulose composite material under the conditions of different adsorption times to waste water sexavalence The absorption change curve of chromium.(Fig. 1 abscissa is PH, but according to narration, it should it is the time)

Embodiment

The present invention is described in further details below with reference to Figure of description and specific embodiment.

Embodiment 1:

In the Reaction conditions range of description, choose a certain value and be illustrated, wherein in specification scope Interior condition can prepare magnetic cellulose/polyglutamic acid coupling material of the present invention, and instantiation is as follows:This kind of hair The preparation method of bright described cellulose composite material:

Stem after bluish dogbane peeling, 80 DEG C of dry 2h, pulverizer is ground again after crushing, and crosses 100 mesh sieves, 65 DEG C of dry 2h.Take The above-mentioned powder of 10g is distributed to 60 milliliters of n-hexanes, and 50 DEG C, 3h removes vegetable wax, then the ramee of dewaxing is added into 500ml Molar concentration in 4mol/L NaOH, 25 DEG C of vibration 24h then are filtered, cleaned with substantial amounts of ultra-pure water, ethanol, methanol, 65 DEG C of drying 2h, are cooled to the bastose element that room temperature obtains basification again;

Weigh 2.0g celluloses and 4.0g polyglutamic acids (monomer mole ratio about 1:After 2.5-3) mixing under infrared lamp fully Grinding 30min obtains uniform fine-powder, is cosolvent with 20ml dimethyl sulfoxides (DMSO), and ultrasonic agitation 30min makes its uniform In scattered DMSO dicyandiamide solutions;Oil bath, is warming up to 120 DEG C, heating stirring adds the 1ml concentrated sulfuric acids as catalyst, reacts 6h;Will Obtain reactant filtering, filter residue is cleaned using ethanol, deionized water, then washed with saturated sodium bicarbonate solution, then spend from Sub- water washing is finally washed, 80 DEG C of drying successively to neutrality with ethanol and acetone, and modified polyglutamic acid/cellulose is made Coupling material;

Take 0.01mol FeCl3·6H2O and 0.005mol FeSO4·4H2O is dissolved in 100ml and surpassed at ambient temperature In pure water, in 2g celluloses/polyglutamic acid composite that obtained mixed solution is added to previous step preparation, in water-bath It is middle to control temperature to be stirred 2 minutes rapidly for 85 DEG C, then it is rapidly added ammoniacal liquor and adjusts pH to 10 or so, continues to stir 45 minutes, by Obtained mixed liquor cooling, sediment separate out is simultaneously washed, and obtains magnetic cellulose/polyglutamic acid coupling material.

Cellulose composite material outward appearance obtained above is in black, and possesses magnetic, can quickly realize separation of solid and liquid, It can apply in various fields.

Embodiment 2:

The magnetic cellulose coupling material of the present invention goes heavy metal ion in water removal, including following step for water treatment field Suddenly:

It is 50mL to take ten volumes, and initial concentration is 100mg/L pending hexavalent chromium wastewater sample, with nitric acid or hydrogen-oxygen Change sodium and adjust pH value to 3, fibrin magnetic composite made from embodiment 1 is added in wastewater sample, in every liter of waste water Addition 2g is calculated as with cellulose composite material weight, by reactor be placed in rotating speed be 150rpm water bath with thermostatic control vibrate case In, keeping temperature is 30 DEG C, is combined cellulose after vibration 5min, 10min, 30min, 1h, 3h, 6h, 9h, 12h, 18h, 24h Material is separated with solution, completes the processing to hexavalent chromium wastewater.The concentration of remaining Cr VI uses ultraviolet spectrometry light in solution Degree meter is measured, and the adsorbance result of calculating is shown in Fig. 1.

As shown in Figure 1, magnetic cellulose coupling material is increased over time and increased to the removal amount of hexavalent chromium And tend to balance.

It the above is only the preferred embodiment of the present invention, protection scope of the present invention is not limited merely to above-described embodiment, With various process programs of the present inventive concept without substantial differences in protection scope of the present invention.

Claims (4)

1. the preparation method of a kind of magnetic cellulose/polyglutamic acid coupling material, it is characterised in that comprise the following steps:
Step 1: preparing or purchase cellulose, the cellulose of alkalization is prepared;
Step 2: preparing cellulose/polyglutamic acid composite using the cellulose of polyglutamic acid and alkalization;
Step 3: magnetic particle is loaded into cellulose modified material surface prepares magnetic cellulose/polyglutamic acid coupling material.
2. the preparation method of magnetic cellulose as claimed in claim 1/polyglutamic acid coupling material, it is characterised in that described In step one, the method for preparing alkalinized celluloses is as follows:
A. the stem after bluish dogbane is removed the peel, 1-4h is dried at 70-90 DEG C, is ground to 100-150 μm, then cleaned with ultra-pure water, 50- 75 DEG C of drying 1-3h, obtain powdered product;
B. powdered product is taken to be distributed in n-hexane, the solid-to-liquid ratio of powdered product and n-hexane is 5-10:40-800g/ml30-60 DEG C heating 1-4h, remove vegetable wax;
C. the bastose of dewaxing is added in the sodium hydroxide solution that molar concentration is 1-5mol/L, powdered product and hydrogen-oxygen The solid-to-liquid ratio for changing sodium solution is 5-10:Filtration product is filtered to obtain after 400-600g/ml, 20-30 DEG C of vibration 10-48h, respectively successively Filtration product is cleaned with ultra-pure water, ethanol and methanol, 1-4h is dried at 50-70 DEG C, room temperature is cooled to and obtains basification Bastose element.
3. the preparation method of magnetic cellulose as claimed in claim 2/polyglutamic acid coupling material, it is characterised in that described In step 2, the preparation method of cellulose/polyglutamic acid composite is as follows:
D. the bastose element and polyglutamic acid, the bastose of basification and the mass ratio of polyglutamic acid of basification are weighed For 1-3:2-6;10-40min is ground under infrared lamp after mixing, uniform fine-powder is obtained;
E. the use of dimethyl sulfoxide is cosolvent, ultrasonic agitation 20-40min makes it be dispersed in dimethylsulfoxide solvent system, Oil bath heating is recycled to be warming up to 110-125 DEG C, stirring adds the concentrated sulfuric acid as catalyst, reaction 4-8h obtains reactant, its In, the volume ratio of the concentrated sulfuric acid and dimethylsulfoxide solvent is 1-10:20;By obtained reactant filtering, filter residue successively using ethanol, Deionized water is cleaned to neutrality;
F. washed, then dried at 70-85 DEG C with ethanol and acetone successively, the cellulose/polyglutamic acid for being made modified is combined The solid-to-liquid ratio of material, fine-powder and dimethyl sulfoxide is:3-9:20g/ml.
4. the preparation method of magnetic cellulose as claimed in claim 1/polyglutamic acid coupling material, it is characterised in that described In step 3, the preparation method of magnetic cellulose/polyglutamic acid coupling material is as follows:
G. FeCl is taken3·6H2O and/or FeSO4·4H2Being dissolved at ambient temperature in ultra-pure water for O obtains mixed solution; 2-10g celluloses/polyglutamic acid composite is added in mixed solution, it is 75-90 DEG C of stirring 1-4 that temperature is controlled in water-bath Minute, then add ammoniacal liquor and adjust pH to 9.8-10.2, continue to stir 35-50 minutes, obtained mixed liquor is cooled down, precipitation and separation Thing is simultaneously washed, and obtains magnetic cellulose/polyglutamic acid coupling material, wherein, cellulose/polyglutamic acid composite and ultra-pure water Solid-to-liquid ratio be 2-10:50-200g/ml;FeCl3·6H2O and FeSO4·4H2O mol ratio is 0-0.02:0-0.01; FeCl3·6H2O and FeSO4·4H2O total amount and the molal volume ratio of ultra-pure water are:0.001-0.03:50-200mol/ml.
CN201710699412.2A 2017-08-16 2017-08-16 A kind of preparation method of magnetic cellulose/polyglutamic acid coupling material CN107262070A (en)

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Publication number Priority date Publication date Assignee Title
CN102476043A (en) * 2010-11-26 2012-05-30 中国科学院理化技术研究所 Cellulose base/Fe3O4 composite adsorption material used for removing arsenic in water and preparation method thereof
CN103663661A (en) * 2013-09-13 2014-03-26 西南石油大学 Treatment method of hexavalent chromium ion containing industrial wastewater
CN105551704A (en) * 2015-12-09 2016-05-04 江苏大学 Preparation and application of dopamine functional magnetic nano-carrier
CN106944007A (en) * 2017-03-31 2017-07-14 启东祥瑞建设有限公司 A kind of metatitanic acid modified cellulose and preparation method thereof

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