CN109797579A - A kind of preparation method of dyefunctionalized cotton fiber composite material - Google Patents

A kind of preparation method of dyefunctionalized cotton fiber composite material Download PDF

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CN109797579A
CN109797579A CN201910056167.2A CN201910056167A CN109797579A CN 109797579 A CN109797579 A CN 109797579A CN 201910056167 A CN201910056167 A CN 201910056167A CN 109797579 A CN109797579 A CN 109797579A
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cotton fiber
composite material
solution
dyefunctionalized
preparation
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赖沅祺
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Abstract

The present invention discloses a kind of preparation method of dyefunctionalized cotton fiber composite material: cotton fiber being put into sulfuric acid solution, heats and stirs 1 hour, be washed out and dry;The cotton fiber of acidification is put into ferric chloride solution, is placed into vacuum plant, is kept for 8 hours, is washed after cotton fiber is taken out, is dry;Above-mentioned cotton fiber is put into potassium ferrocyanide solution, is quickly stirred, stands 4 hours;Into above-mentioned solution, ferric chloride solution is added, quickly stirs, stands 4 hours;Cotton fiber is taken out, washs, dry, obtains dyefunctionalized cotton fiber composite material;The preparation method is easy to operate, high-efficient, and prepared dyefunctionalized cotton fiber composite material has excellent performance, has broad prospect of application in fields such as wastewater treatments.

Description

A kind of preparation method of dyefunctionalized cotton fiber composite material
Technical field
The present invention relates to functional composite material field, especially a kind of preparation side of dyefunctionalized cotton fiber composite material Method.
Background technique
With the fast development and extensive use of the nuclear technology such as nuclear power, radioactive isotope, nuclear medicine, environment is radiated The threat of property nucleic.2011, during Fukushima, Japan nuclear power plant accident, a large amount of radioactive wastewaters can not be handled and direct in time It is discharged into ocean, water body and biology are caused and seriously affected.Caesium -137 is the important fission product of nuclear power station, long half time (30 years), the extent of injury are big, are one of the radionuclides paid close attention in Spent Radioactive water treatment procedure.Currently, extraction, Concentration method, membrane separation process, electroosmose process, ion exchange adsorption etc. have been applied to Spent Radioactive water process, wherein absorption method Have many advantages, such as that at low cost, selectivity is high, easily operated and one of as mainstream technology.
Prussian blue also known as Chinese blue is a kind of ancient blue dyes, is widely used in the neck such as printing and dyeing, oil painting, coating Domain.It is Prussian blue that there is special crystal structure, ion exchange can be carried out with many metal ions, shown many excellent Performance has important application prospect in fields such as catalysis, absorption.It is Prussian blue to be used as drug for treating in thallium Poison.It is Prussian blue selective absorption to be carried out to cesium ion, for handling radioactive wastewater.Powder adsorbent material is easy group It is poly-, specific surface area is small, difficult separation, easily cause secondary pollution.How to optimize Prussian blue structure, improve its adsorption efficiency and realizes Quick separating is emphasis concerned by people.It is multiple that Yang etc. is prepared for magnetic ferroferric oxide/graphene oxide/prussian blue nano Object is closed, the caesium in aqueous solution can be effectively removed and realize Magnetic Isolation.Xie Fei etc. is prepared for Prussian blue/active carbon composite wood Material, for recycling the caesium in salt lake bittern.Vincent etc. is prepared for the Prussian blue sponge of chitosan-by freeze-drying, uses In absorption cesium ion.Jia etc., as carrier modification Prussian, is proved using polyacrylonitrile film by filtration experiment The effectively catching to cesium ion can be achieved.Guo Yijiao etc. is prepared for porous light reticulated ceramic matrix first, then on its surface Prussian is grown, stronger ion-exchange capacity is shown.There are still prepared for existing Prussian blue composite material The deficiencies of journey is cumbersome, price is higher limits its large-scale application.Develop Novel Prussian blue nanocomposite and its preparation Method still has very big exploration value and application space.
Currently, the Prussian blue dyefunctionalized cotton using the preparation of two step in-situ synthesis for Spent Radioactive water process is fine Composite material is tieed up, there is not been reported.
Summary of the invention
The present invention is directed to the limitation of existing wastewater processing technology demand and dyefunctionalized composite material and preparation method thereof, mentions For a kind of preparation method of dyefunctionalized cotton fiber composite material, the specific steps of which are as follows:
Cotton fiber is put into sulfuric acid solution, is heated to 60 DEG C, stirs 1 hour, is washed with deionized 3 times, 70 DEG C of vacuum It is dry, the cotton fiber being acidified;The cotton fiber of acidification is put into ferric chloride solution, is placed into vacuum plant, Room temperature keeps 8h, after cotton fiber is taken out, washs 3 times, 70 DEG C of vacuum drying obtain the cotton fiber of load iron chloride;It will be above-mentioned Cotton fiber is put into potassium ferrocyanide solution, is quickly stirred, and stands 4 hours, and solution system becomes blue;Into above-mentioned solution, Ferric chloride solution is added, quickly stirring 20 minutes, stands 4 hours;Cotton fiber is taken out, is washed with deionized to cleaning solution and is Colorless and transparent, 70 DEG C of vacuum drying obtain dyefunctionalized cotton fiber composite material.
Further, a kind of preparation method of dyefunctionalized cotton fiber composite material of the present invention, which is characterized in that institute The concentration for stating sulfuric acid solution is 0.1-1M.
Further, a kind of preparation method of dyefunctionalized cotton fiber composite material of the present invention, which is characterized in that institute The mass ratio for stating iron chloride, acidification cotton fiber and deionized water is 1:0.5-1:50.
Further, a kind of preparation method of dyefunctionalized cotton fiber composite material of the present invention, which is characterized in that institute The mass ratio 1:0.2-0.5:50 for stating potassium ferrocyanide, loading iron chloride cotton fiber and deionized water.
Further, a kind of preparation method of dyefunctionalized cotton fiber composite material of the present invention, which is characterized in that institute The mass ratio for stating second of addition iron chloride and potassium ferrocyanide is 1:0.3-0.6.
Dyefunctionalized cotton fiber composite material is prepared in situ using natural cotton fiber as matrix, using two-step method in the present invention, Method is simple, high-efficient, has the advantage that
(1) with active carbon, graphene etc. for inorganic material compared with, main group of cotton fiber becomes cellulose, containing big The functional group of amount, have with reactive ion compatibility with higher, be conducive to being uniformly distributed for product;
(2) compared with other materials, cotton fiber density is small, burn after residue it is few, be used as adsorbent material, such as convenient for burning Volume reduction treatment.
(3) compared with one-step method, it is using the advantage of two-step method, forms equally distributed dye in fibrous inside first Material, then in fibrous external carried dye, dyestuff is distributed in cotton fiber and load capacity has improvement.
(4) the dyefunctionalized cotton fiber composite material prepared by the present invention has good absorption property, at waste water Reason field has broad prospect of application.
Specific embodiment
Embodiment 1
5g cotton fiber is put into 50mL 0.1M sulfuric acid solution, is heated to 60 DEG C, stirs 1 hour, is washed with deionized 3 It is secondary, 70 DEG C of vacuum drying, the cotton fiber being acidified;The cotton fiber of 1g acidification is put into 50mL2% ferric chloride solution In, it is placed into vacuum plant, room temperature keeps 8h, after cotton fiber is taken out, washs 3 times, 70 DEG C of vacuum drying obtain load chlorine Change the cotton fiber of iron;Above-mentioned cotton fiber is put into 50mL2% potassium ferrocyanide solution, is quickly stirred, stands 4 hours, solution System becomes blue;Into above-mentioned solution, 4% ferric chloride solution of 50mL is added, quickly stirring 20 minutes, stands 4 hours;It will Cotton fiber takes out, and it is colorless and transparent for being washed with deionized to cleaning solution, and 70 DEG C of vacuum drying obtain dyefunctionalized cotton fiber Composite material.It after tested, is 91.6% to the eliminating rate of absorption of cesium ion.
Embodiment 2
5g cotton fiber is put into 50mL 1M sulfuric acid solution, is heated to 60 DEG C, stirs 1 hour, is washed with deionized 3 times, 70 DEG C of vacuum drying, the cotton fiber being acidified;The cotton fiber of 0.5g acidification is put into 2% ferric chloride solution of 50mL In, it is placed into vacuum plant, room temperature keeps 8h, after cotton fiber is taken out, washs 3 times, 70 DEG C of vacuum drying obtain load chlorine Change the cotton fiber of iron;Above-mentioned cotton fiber is put into 2% potassium ferrocyanide solution of 50mL, is quickly stirred, stands 4 hours, solution System becomes blue;Into above-mentioned solution, 4% ferric chloride solution of 50mL is added, quickly stirring 20 minutes, stands 4 hours;It will Cotton fiber takes out, and it is colorless and transparent for being washed with deionized to cleaning solution, and 70 DEG C of vacuum drying obtain dyefunctionalized cotton fiber Composite material.It after tested, is 97.8% to the eliminating rate of absorption of cesium ion.
Embodiment 3
5g cotton fiber is put into 50mL 0.8M sulfuric acid solution, is heated to 60 DEG C, stirs 1 hour, is washed with deionized 3 It is secondary, 70 DEG C of vacuum drying, the cotton fiber being acidified;The cotton fiber of 2g acidification is put into 2% ferric chloride solution of 50mL In, it is placed into vacuum plant, room temperature keeps 8h, after cotton fiber is taken out, washs 3 times, 70 DEG C of vacuum drying obtain load chlorine Change the cotton fiber of iron;Above-mentioned cotton fiber is put into 2% potassium ferrocyanide solution of 50mL, is quickly stirred, stands 4 hours, solution System becomes blue;Into above-mentioned solution, 6% ferric chloride solution of 50mL is added, quickly stirring 20 minutes, stands 4 hours;It will Cotton fiber takes out, and it is colorless and transparent for being washed with deionized to cleaning solution, and 70 DEG C of vacuum drying obtain dyefunctionalized cotton fiber Composite material.It after tested, is 85.7% to the eliminating rate of absorption of cesium ion.
Embodiment 4
5g cotton fiber is put into 50mL 1M sulfuric acid solution, is heated to 60 DEG C, stirs 1 hour, is washed with deionized 3 times, 70 DEG C of vacuum drying, the cotton fiber being acidified;The cotton fiber of 1.5g acidification is put into 2% ferric chloride solution of 30mL In, it is placed into vacuum plant, room temperature keeps 8h, after cotton fiber is taken out, washs 3 times, 70 DEG C of vacuum drying obtain load chlorine Change the cotton fiber of iron;Above-mentioned cotton fiber is put into 2% potassium ferrocyanide solution of 60mL, is quickly stirred, stands 4 hours, solution System becomes blue;Into above-mentioned solution, 5% ferric chloride solution of 50mL is added, quickly stirring 20 minutes, stands 4 hours;It will Cotton fiber takes out, and it is colorless and transparent for being washed with deionized to cleaning solution, and 70 DEG C of vacuum drying obtain dyefunctionalized cotton fiber Composite material.It after tested, is 88.3% to the eliminating rate of absorption of cesium ion.
Embodiment 5
5g cotton fiber is put into 50mL 1M sulfuric acid solution, is heated to 60 DEG C, stirs 1 hour, is washed with deionized 3 times, 70 DEG C of vacuum drying, the cotton fiber being acidified;The cotton fiber of 0.5g acidification is put into 2% ferric chloride solution of 50mL In, it is placed into vacuum plant, room temperature keeps 8h, after cotton fiber is taken out, washs 3 times, 70 DEG C of vacuum drying obtain load chlorine Change the cotton fiber of iron;Above-mentioned cotton fiber is put into 2% potassium ferrocyanide solution of 50mL, is quickly stirred, stands 4 hours, solution System becomes blue;Cotton fiber is taken out, it is colorless and transparent for being washed with deionized to cleaning solution, and 70 DEG C of vacuum drying obtain Dyefunctionalized cotton fiber composite material.It after tested, is 57.8% to the eliminating rate of absorption of cesium ion.
Embodiment 6
1g cotton fiber is put into 2% ferric chloride solution of 50mL, is placed into vacuum plant, room temperature keeps 8h, by cotton It after fiber takes out, washs 3 times, 70 DEG C of vacuum drying obtain the cotton fiber of load iron chloride;Above-mentioned cotton fiber is put into 50mL It in 2% potassium ferrocyanide solution, quickly stirs, stands 4 hours, solution system becomes blue;Into above-mentioned solution, 50mL is added 4% ferric chloride solution, quickly stirring 20 minutes, stand 4 hours;Cotton fiber is taken out, is washed with deionized to cleaning solution and is Colorless and transparent, 70 DEG C of vacuum drying obtain dyefunctionalized cotton fiber composite material.After tested, the absorption of cesium ion is gone Except rate is 62.2%.
Above-described embodiment shows that dyefunctionalized cotton fiber composite material prepared by the present invention has good absorption Performance has broad prospect of application in field of waste water treatment.
Above embodiments not do limitation in any form to the present invention, any without departing from technical solution of the present invention Hold, according to the technical essence of the invention any simple modification, equivalent change and modification to the above embodiments, belongs to this The range of inventive technique scheme.

Claims (5)

1. a kind of preparation method of dyefunctionalized cotton fiber composite material, which is characterized in that specific step is as follows:
(1) cotton fiber is put into sulfuric acid solution, is heated to 60 DEG C, stirred 1 hour, is washed with deionized 3 times, 70 DEG C of vacuum are dry Cotton fiber that is dry, being acidified;
(2) cotton fiber of acidification is put into ferric chloride solution, is placed into vacuum plant, room temperature keeps 8h, by cotton It after fiber takes out, washs 3 times, 70 DEG C of vacuum drying obtain the cotton fiber of load iron chloride;
(3) above-mentioned cotton fiber is put into potassium ferrocyanide solution, is quickly stirred, stand 4 hours, solution system becomes blue;
(4) in Xiang Shangshu solution, ferric chloride solution is added, quickly stirring 20 minutes, stands 4 hours;
(5) cotton fiber is taken out, it is colorless and transparent for being washed with deionized to cleaning solution, and 70 DEG C of vacuum drying obtain dyestuff function Cotton fiber composite material can be changed.
2. a kind of preparation method of dyefunctionalized cotton fiber composite material according to claim 1, which is characterized in that step 1) concentration of the sulfuric acid solution is 0.1-1M.
3. a kind of preparation method of dyefunctionalized cotton fiber composite material according to claim 1, which is characterized in that step 2) mass ratio of the iron chloride, acidification cotton fiber and deionized water is 1:0.5-1:50.
4. a kind of preparation method of dyefunctionalized cotton fiber composite material according to claim 1, which is characterized in that step 3) mass ratio of the potassium ferrocyanide, load iron chloride cotton fiber and deionized water is 1:0.2-0.5:50.
5. a kind of preparation method of dyefunctionalized cotton fiber composite material according to claim 1, which is characterized in that step 4) mass ratio of the iron chloride and potassium ferrocyanide is 1:0.3-0.6.
CN201910056167.2A 2019-01-19 2019-01-19 A kind of preparation method of dyefunctionalized cotton fiber composite material Pending CN109797579A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114749157A (en) * 2022-05-11 2022-07-15 四川大学 Cesium adsorption material with prussian blue compounds loaded on collagen fibers, and preparation method and application thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114749157A (en) * 2022-05-11 2022-07-15 四川大学 Cesium adsorption material with prussian blue compounds loaded on collagen fibers, and preparation method and application thereof

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