CN101979328B - Chitosan composite gel water purifying agent, preparation method and uses thereof - Google Patents
Chitosan composite gel water purifying agent, preparation method and uses thereof Download PDFInfo
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- CN101979328B CN101979328B CN 201010523953 CN201010523953A CN101979328B CN 101979328 B CN101979328 B CN 101979328B CN 201010523953 CN201010523953 CN 201010523953 CN 201010523953 A CN201010523953 A CN 201010523953A CN 101979328 B CN101979328 B CN 101979328B
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Abstract
The invention discloses a chitosan composite gel water purifying agent, which is gel prepared from solution of chitosan, cellulose, silica gel and activated carbon according to the mass ratio of 1:1-2.5:2-3.5:3-5. The invention also discloses a method for preparing the chitosan composite gel water purifying agent, which comprises the following steps of: adding the cellulose, the silica gel and the activated carbon into the solution of chitosan in turn; fully stirring at a high speed until black and homogeneous semifluid gel is formed, and obtaining the chitosan composite gel water purifying agent. The water purifying agent is natural and nontoxic, has functions of high-efficiency adsorption and flocculation, can be used for deep purification of an underwater environment polluted by endocrine disruptors and also can be used for emergency treatment in public health water pollution emergency. Meanwhile, the preparation method makes operation simple, reduces cost and is environmentally-friendly and suitable for industrial production.
Description
Technical field
The present invention relates to the water purification agent field, be specifically related to a kind of chitosan plural gel water purification agent.
Background technology
In recent years, external internal secretion interferon activity to the environmental chemistry thing has launched extensive investigations and research.A large amount of epizootiology data show, many environmental chemistry thing interfere animal's endocrine function are characteristic with dysgenesia, inborn defect, heteroplasia, metabolism disorder and some cancer then clinically.The human epidemiology studies demonstration, and human reproduction's obstacle, heteroplasia and some cancer such as mammary cancer, carcinoma of testis, ovarian cancer etc. are disturbed relevant with internal secretion.The chemicals that have been proved to be endocrine disrupter reach hundreds of more than.Japanese investigation to water pollutant in 1998 shows, mainly contains eight types of endocrine disruptors in the water, comprises phthalate, phenols (alkylphenol, dihydroxyphenyl propane and chlorophenol etc.), epoxy chloropropane and organic pesticide (like weedicide, agrochemical).The water body investigation result of other countries shows that also environment incretion interferent has got into water body, and pollution range can also can get into human body through the bioconcentration of food chain through directly drinking contaminated water also in progressively expansion.
To the pollution of the environment incretion interferent matter of increasingly sharpening, traditional coagulation-deposition-filtration-sterilization four-part form water technology can not have been tackled present water and pollute a difficult problem.Must develop a kind of water purification agent, so that the environment incretion interferent matter of polluting in the water is carried out advanced treatment with coacervation and adsorption dual effect for this reason.
Summary of the invention
The invention provides a kind of Nantural non-toxic and have efficient absorption and the chitosan plural gel water purification agent of floculation dual-use function.
The present invention also provides a kind of preparation method of chitosan plural gel water purification agent, and this method is simple to operate, is suitable for suitability for industrialized production.
A kind of chitosan plural gel water purification agent is the gelifying agent of being processed by chitosan solution, Mierocrystalline cellulose, silica gel and gac; The mass ratio of described chitosan, Mierocrystalline cellulose, silica gel and gac is 1: 1-2.5: 2-3.5: 3-5.
The aboundresources of chitosan has the various biological activity, also is a kind of good flocculation agent, and multiple harmful organic substance is had the good adsorption effect.Gac is a kind of conventional sorbent material of using, and receives the influence of factors such as matter property in itself characteristic and the water, and can not remove the organism in the water separately effectively.The present invention finds chitosan gel rubber and gac and has the compound type purifying agent that other etcetera of the dual function of reinforcement coacervation and absorption are processed, can a kind of new technology platform and new water purification product be provided for environment incretion interferent in the advanced water treatment.
The preferred deacetylation of described chitosan is greater than 90% chitosan, and viscosity is generally 150mpaS-550mpaS during 25 ℃ of this type chitosans, can reach better effect, and its dissolving power and flocculating property in diluted acid is better in addition.
The deacetylation of chitosan is meant that the saccharide residue number that removes acetoxyl in the chitosan molecule accounts for the per-cent of saccharide residue number total in the chitosan molecule among the present invention.
The mass percentage concentration of chitosan is preferably 1%-8% in the described chitosan solution, the righttest gel of processing of its viscosity.
Solvent is preferably acetic acid aqueous solution or aqueous hydrochloric acid in the described chitosan solution.
The concentration expressed in percentage by volume of described acetic acid aqueous solution or aqueous hydrochloric acid all is preferably 1%-6% (the pH value is 5-6).
The granularity of described gac is preferably 80 orders-120 order, and the granularity of described silica gel is preferably 50 orders-80 order; The gel that this granularity is processed is the most stable.
Described gelifying agent has the reticulated structure that the white circular spherical particle is formed, and has the gac of irregular bulk between its network.
The preparation method of described chitosan plural gel water purification agent comprises step:
(1) preparing chitosan solution (its pH value is preferably 5-6, can regulate the pH value of chitosan solution through the solvent in the chitosan solution) adds Mierocrystalline cellulose in chitosan solution, stirs and makes cellulose dissolution, obtains solution;
(2) in the solution of step (1), add silica gel, mix, obtain dispersion liquid;
(3) in the dispersion liquid of step (2), add gac, mix, obtain the chitosan plural gel water purification agent until forming even black gel.
Described chitosan plural gel water purification agent is the application in the environment incretion interferent matter in removing water.
Described environment incretion interferent matter is representative with in (DDT) one or both of Witophen N, (2,2-two (rubigan)-1.1.1-trichloroethane).
Chitosan plural gel water purification agent of the present invention to the detection method of the clearance of environment incretion interferent matter is: certain amount of chitosan plural gel water purification agent is joined in the environment incretion interferent matter simulating pollution water body of certain volume; Constant-temperature shaking certain hour in water-bath; After centrifugal; Get supernatant and measure solution absorbency, go out the concentration of environment incretion interferent matter in the detected solution by the working curve regression equation calculation.
Calculate loading capacity q (mg/g), q=(C according to formula (I)
0-C
t) V/m
1--formula (I), wherein C
0(mg/L) be the starting point concentration of environment incretion interferent matter, C
t(mg/L) be the concentration of environment incretion interferent matter in the solution when adsorption time is t, V (L) is the volume of environment incretion interferent matter simulating pollution water body, m
1(g) be the quality of chitosan plural gel water purification agent.
Calculate clearance f (%), f=qm according to formula (II)
1/ m
2100%--formula (II), wherein m
2(g) be the quality of environment incretion interferent matter in the environment incretion interferent matter simulating pollution water body.
The present invention has the following advantages:
Chitosan plural gel water purification agent of the present invention is a kind of black semi-fluid chitosan plural gel, and kinetic viscosity is 5000mpaS-10000mpaS in the time of 25 ℃.Opticmicroscope shows that down chitosan plural gel water purification agent of the present invention has the reticulated structure that the white circular spherical particle is formed, and has the atrament (being gac) of irregular bulk between its network; The particle size range of white circular spherical particle wherein distributes generally at the 0.2-50 micron.
Mostly existing water purification agent is the granular solids mixture, and chitosan plural gel water purification agent of the present invention is a gel composite, has overcome to use the uneven shortcoming of preparation; Promptly join and promptly use effect good, Nantural non-toxic, tasteless; Excellent in physical and chemical performance; The drinking water emergency pre-treatment that advanced treatment or sudden water pollution incident cause that can be used for drinking water, environmentally friendly, pollution-free.
Chitosan plural gel water purification agent of the present invention is a kind of have efficient absorption and bifunctional composite water purifying agent of floculation, can efficiently remove environment incretion interferent matter in the water.Clarification time to environment incretion interferent in the water is very fast; Balance can reach capacity in 20 minutes; Clearance to environment incretion interferent is high, particularly environment incretion interferent matter in the water (like Witophen N, DDT and polychlorobiphenyl etc.) is had obviously Water purification efficiently, can reach 98.8% like the clearance to Witophen N; Clearance to DDT can reach 96%, and practicality is stronger.
The aboundresources such as raw materials of chitosan that the present invention is used, preparation technology's flow process of water purification agent is simple, with short production cycle, easy and simple to handle, and production cost is low, is suitable for suitability for industrialized production.
Description of drawings
Fig. 1 is 200 times of opticmicroscope pictures of the chitosan plural gel water purification agent of the embodiment of the invention 1 preparation;
Fig. 2 is 200 times of opticmicroscope pictures after the chitosan plural gel water purification agent of the embodiment of the invention 1 preparation flocculates.
Embodiment
Embodiment 1
(1) takes by weighing 3g chitosan (deacetylation is 99%); To wherein adding concentration expressed in percentage by volume is 3% aqueous acetic acid 100ml; All dissolve to chitosan, obtain the pH value and be 5 chitosan solution, according to chitosan: the mass ratio of Mierocrystalline cellulose=1: 1.5 adds Mierocrystalline cellulose; Make cellulose dissolution in 3 hours with 500 rev/mins of stirrings, obtain solution.
(2) according to chitosan: the mass ratio of silica gel (granularity is 50 orders)=1: 2 adds silica gel in the solution of step (1), stirs with 800 rev/mins and makes the silica gel homodisperse in 1 hour, obtains dispersion liquid.
(3) according to chitosan: the mass ratio of gac=1: 3.5 adds granularity in the dispersion liquid of step (2) be 80 purpose gacs; Stir 4 hours until processing even black gel with 500 rev/mins; Obtain the chitosan plural gel water purification agent, kinetic viscosity is 10000mpaS in the time of its 25 ℃.
Above-mentioned chitosan plural gel water purification agent is added in the water body that contains Witophen N (PCP-Na) 100ppm (mass ratio) pollution; Wherein, The quality of chitosan plural gel water purification agent is 1% of a water body quality; Regulate pH=5 with hydrochloric acid and stir after 20 minutes centrifugally, detect the mass content of PCP-Na in the gained liquid, calculate above-mentioned chitosan plural gel water purification agent and can reach 95% the clearance of PCP-Na.
200 times of opticmicroscope pictures of above-mentioned chitosan plural gel water purification agent such as Fig. 1 show that this chitosan plural gel water purification agent has the reticulated structure that the white circular spherical particle is formed, and exists the atrament (being gac) of irregular bulk between its network; The particle size range of white circular spherical particle wherein is distributed between the 0.2-50 micron, 7.878 microns of average out to, and wherein 90% particle is below 20.87 microns.When above-mentioned chitosan plural gel water purification agent after the water purification effect, 200 times of opticmicroscope pictures of centrifugal sediment such as Fig. 2, the reticulated structure that visible white circular spherical particle is formed disappears, rarely seen grain becomes big black gac deposition.
Embodiment 2
(1) takes by weighing 5g chitosan (deacetylation is 98%); To wherein adding concentration expressed in percentage by volume is 4% aqueous acetic acid 100ml; All dissolve to chitosan, obtain the pH value and be 6 chitosan solution, according to chitosan: the mass ratio of Mierocrystalline cellulose=1: 2 adds Mierocrystalline cellulose; Make cellulose dissolution in 2 hours with 600 rev/mins of stirrings, obtain solution.
(2) according to chitosan: the mass ratio of silica gel (granularity is 80 orders)=1: 3 adds silica gel in the solution of step (1), stirs with 700 rev/mins and makes the silica gel homodisperse in 1.5 hours, obtains dispersion liquid.
(3) according to chitosan: the mass ratio of gac=1: 5 adds granularity in the dispersion liquid of step (2) be 100 purpose gacs; Stir 3 hours until processing even black gel with 500 rev/mins; Obtain the chitosan plural gel water purification agent, kinetic viscosity is 6500mpaS in the time of 25 ℃.
Above-mentioned chitosan plural gel water purification agent is added in the water body that contains DDT 100ppm (mass ratio) pollution; Wherein, The quality of chitosan plural gel water purification agent is 1% of a water body quality; Regulate pH=5 with hydrochloric acid and stir after 20 minutes centrifugally, detect the mass content of DDT in the gained liquid, calculate above-mentioned chitosan plural gel water purification agent and can reach 94% the clearance of DDT.
200 times of opticmicroscope pictures of above-mentioned chitosan plural gel water purification agent show that this chitosan plural gel water purification agent has the reticulated structure that the white circular spherical particle is formed, and exists the atrament (being gac) of irregular bulk between its network; The particle size range of white circular spherical particle wherein is distributed between the 0.3-80 micron, 8.878 microns of average out to, and wherein 80% particle is below 30 microns.When above-mentioned chitosan plural gel water purification agent after the water purification effect, the reticulated structure that the visible white circular spherical particle of 200 times of opticmicroscope pictures of centrifugal sediment is formed disappears, rarely seen grain becomes big black gac deposition.
Embodiment 3
(1) takes by weighing 7g chitosan (deacetylation is 91%); To wherein adding concentration expressed in percentage by volume is 5% aqueous acetic acid 100ml; All dissolve to chitosan, obtain the pH value and be 5.5 chitosan solution, according to chitosan: the mass ratio of Mierocrystalline cellulose=1: 2.5 adds Mierocrystalline cellulose; Make cellulose dissolution in 1 hour with 800 rev/mins of stirrings, obtain solution.
(2) according to chitosan: the mass ratio of silica gel (granularity is 60 orders)=1: 3.5 adds silica gel in the solution of step (1), stirs with 500 rev/mins and makes the silica gel homodisperse in 2 hours, obtains dispersion liquid.
(3) according to chitosan: the mass ratio of gac=1: 4 adds granularity in the dispersion liquid of step (2) be 120 purpose gacs; Stir 1 hour until processing even black gel with 800 rev/mins; Obtain the chitosan plural gel water purification agent, kinetic viscosity is 5000mpaS in the time of 25 ℃.
Above-mentioned chitosan plural gel water purification agent is added in the water body that contains Witophen N (PCP-Na) 100ppm (mass ratio) pollution; Wherein, The quality of chitosan plural gel water purification agent is 1% of a water body quality; Regulate pH=5 with hydrochloric acid and stir after 20 minutes centrifugally, detect the mass content of PCP-Na in the gained liquid, calculate above-mentioned chitosan plural gel water purification agent and can reach 97% the clearance of PCP-Na.Use with quadrat method and prove that the clearance to DDT in the water reaches 95.5%.
200 times of opticmicroscope pictures of above-mentioned chitosan plural gel water purification agent show that this chitosan plural gel water purification agent has the reticulated structure that the white circular spherical particle is formed, and exists the atrament (being gac) of irregular bulk between its network; The particle size range of white circular spherical particle wherein is distributed between the 0.5-90 micron, 9.035 microns of average out to, and wherein 80% particle is below 35 microns.When above-mentioned chitosan plural gel water purification agent after the water purification effect, the reticulated structure that the visible white circular spherical particle of 200 times of opticmicroscope pictures of centrifugal sediment is formed disappears, rarely seen grain becomes big black gac deposition.
Claims (10)
1. a chitosan plural gel water purification agent is characterized in that, is the gelifying agent of being processed by chitosan solution, Mierocrystalline cellulose, silica gel and gac; The mass ratio of described chitosan, Mierocrystalline cellulose, silica gel and gac is 1: 1-2.5: 2-3.5: 3-5.
2. chitosan plural gel water purification agent according to claim 1 is characterized in that the deacetylation of described chitosan is greater than 90%.
3. chitosan plural gel water purification agent according to claim 1 is characterized in that, the mass percentage concentration of chitosan is 1%-8% in the described chitosan solution.
4. chitosan plural gel water purification agent according to claim 1 is characterized in that, solvent is acetic acid aqueous solution or aqueous hydrochloric acid in the described chitosan solution.
5. chitosan plural gel water purification agent according to claim 4 is characterized in that, the concentration expressed in percentage by volume of described acetic acid aqueous solution or aqueous hydrochloric acid is 1%-6%.
6. chitosan plural gel water purification agent according to claim 1 is characterized in that, the granularity of described gac is 80 orders-120 orders; The granularity of described silica gel is 50 orders-80 orders.
7. chitosan plural gel water purification agent according to claim 1 is characterized in that, described gelifying agent has the reticulated structure that the white circular spherical particle is formed, and has the gac of irregular bulk between its network.
8. according to the preparation method of each described chitosan plural gel water purification agent of claim 1-7, comprise step:
(1) preparing chitosan solution adds Mierocrystalline cellulose in chitosan solution, stir and make cellulose dissolution, obtains solution;
(2) in the solution of step (1), add silica gel, mix, obtain dispersion liquid;
(3) in the dispersion liquid of step (2), add gac, mix, obtain the chitosan plural gel water purification agent until forming even black gel.
9. according to the application in the environment incretion interferent matter in removing water of each described chitosan plural gel water purification agent of claim 1-7.
10. application according to claim 9 is characterized in that, described environment incretion interferent matter is Witophen N, 2, one or both in two (the rubigan)-1 of 2-.
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