CN103100376B - Fiber natural polymeric adsorbent and application thereof - Google Patents

Fiber natural polymeric adsorbent and application thereof Download PDF

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Publication number
CN103100376B
CN103100376B CN201310059836.4A CN201310059836A CN103100376B CN 103100376 B CN103100376 B CN 103100376B CN 201310059836 A CN201310059836 A CN 201310059836A CN 103100376 B CN103100376 B CN 103100376B
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natural polymeric
polymeric adsorbent
adsorbent
fiber natural
fiber
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CN103100376A (en
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王荣民
李慧茹
何玉凤
黄一君
张立佳
孟俞伟
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GANSU TIPTOP PLANT TECHNOLOGY CORP., LTD.
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Gansu Tiptop Plant Technology Corp Ltd
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Abstract

The invention provides a fiber natural polymeric adsorbent, and belongs to the technical field of wastewater treatment. The fiber natural polymer uses bean dregs as a fiber source. Fresh bean dregs are successively treated by distilled water, ethanol solution and sodium bicarbonate solution for processing, so as to remove water-soluble substances and small molecular substances; and then the bean dregs are subjected to drying, crushing and sieving through a 100 mesh screen. Adsorption tests prove that the fiber natural polymer adsorbent has excellent adsorption performance on wastewater containing heavy metal lead ions and copper ions, a dye methylene blue, malachite green, basic fuchsin and organic pollutant naphthol. Therefore, the fiber natural polymeric adsorbent can be used for industrial treatment on wastewater containing heavy metal ion, dyes and organics. At the same time, the adsorbent mainly comprises components including cellulose, lignin and a small amount of glycoprotein, and is a non-toxic, pollution-free edible natural polymer with good compatibility; therefore, the adsorbent can also be used as a rapid antidote for heavy metal poisoning.

Description

A kind of fiber natural polymeric adsorbent and application thereof
Technical field
The invention belongs to water-treatment technology field, relate to a kind of preparation of fiber natural polymeric adsorbent; The present invention also relates to this adsorbent simultaneously and is containing heavy metal lead ion and copper ion, dyestuff methylene blue, malachite green, basic fuchsin and the application contained in the wastewater treatment of naphthols.
Background technology
In recent years, along with the increase gradually of industrial and agricultural wastewater and city domestic sewage discharge capacity, the river of China, river, lake, waters, storehouse are generally subject to pollution in various degree, and water quality, in continuous deterioration, causes serious harm to ecological environment and human health.Traditional method of wastewater treatment has ion-exchange, solvent extraction, chemical precipitation method, oxidation-reduction method, absorption method, electrochemical treatment and membrane technology method, but there is dosing greatly in most for the treatment of technology, somewhat expensive, effect is undesirable, easily produces secondary pollution problems.Absorption method is a kind of simple, cheap and efficient method.At present, to nontoxic, at a low price, efficiently and have the exploitation of the adsorbent of stronger complexing power to become study hotspot, with natural polymer, agriculture and forestry organic waste material and industrial by-products are applied to as adsorbent the concern that wastewater treatment has been subject to more and more people.
Cellulose is natural polymer the abundantest on the earth, is also inexhaustible, the nexhaustible resource of nature.In recent years, along with the rapidly soaring of oil equal energy source price and sustainable development in the urgent need to, cellulose more and more comes into one's own as eco-friendly renewable resource.Due to the stereospecificity high molecular polymer that cellulose is a kind of fibrous multiple capillary, there is porous and the large characteristic of specific area, and containing many hydrophilic hydroxyls in molecule, therefore there is certain adsorptivity.
The insoluble sludge produced in the process of bean products such as soya-bean milk, soya-bean milk and bean curd produced by bean dregs.Bean dregs are good fibrous raw materials, and main component is cellulose fiber peacekeeping lignin fibre, and wherein content of cellulose occupies the half of dry.Bean dregs are as the refuse produced in bean product manufacture craft, and output is very large, and about annual output is 80,000 tons, accounts for the 8%-10% of China's soybean annual production.But due to its perishability and the inconvenience that stores in transport, these bean dregs, only as feed, fertilizer or as offal treatment, do not realize its value, economic benefit is low, also result in environmental pollution to a certain degree simultaneously.In addition, containing abundant dietary fiber in bean dregs, also containing isoflavones, soybean protein, calcium, phosphorus, vitamin etc., there is abundant nutritive value, unique medical value and health care, discarded, also result in great waste, therefore, development and utilization bean dregs have wide market potential.It is raw material that CN102631896A provides with bean dregs, is used for the absorption of formaldehyde by the sorbing material that growth of microorganism legal system is standby.CN102687668A, CN102687669A disclose respectively with dry, wet bean dregs for cat litter prepared by raw material.But these adsorbents do not relate to the research containing heavy metal ion, the wastewater treatment of dye well naphthols.
Summary of the invention
The object of the invention is for problems of the prior art, provide a kind of and not only may be used for water treatment but also can as the fiber natural polymeric adsorbent of edible rapid detoxification agent.
(1) preparation of fiber natural polymeric adsorbent
Fiber natural polymeric adsorbent of the present invention, is first washed with distilled water by fresh bean dregs, crosses and filter water-soluble substances; Use the alcohol solution dipping 1 ~ 10h of mass percent 50 ~ 80% again, filter, distilled water washs; Then the sodium bicarbonate solution of pH=8 ~ 11 is used to soak 1 ~ 10h; Filter, respectively with ethanol, distilled water washing, removing small-molecule substance; Last vacuum drying at 35 ~ 65 DEG C, pulverizes, and crosses 100 mesh sieves, both must this fiber natural polymeric adsorbent (SHR).
Described fresh bean dregs are the insoluble sludge that bean product processing industry produces soya-bean milk, bean curd, soya-bean milk gained.
(2) structure of fiber natural polymeric adsorbent
Below by characterization methods such as Fourier infrared spectrum (FT-IR), X-ray photoelectron spectroscopic analysis (XPS), elementary analyses, analytic explanation is carried out to the structure of adsorbent prepared by the present invention.
1, FT-IR spectrum analysis
Adsorbent (SHR) FT-IR spectrum analysis as shown in Figure 1, as can be seen from Figure 1, adsorbent (SHR) major absorbance peak 3422 cm -1it is the stretching vibration absworption peak of alcohol, Fen – OH; 2925 and 2855cm -1it is the stretching vibration peak of CH; 1061 and 794 cm -1c – O – C and the C – H vibration absorption peak of fiber prime ring respectively; 1744 and 1647 cm -1the characteristic absorption peak of carbonyl, 1417 cm -1it is the stretching vibration peak of C – O in carboxyl.As can be seen here, in this adsorbent, Han You – OH, C – O and-C=O isoreactivity group, can carry out complexing with metal ion, dyestuff and organic matter, thus have suction-operated to the metal ion in sewage, dyestuff and organic matter.
2, XPS analysis
Fig. 2, Fig. 3, Fig. 4 are respectively XPS spectrum figure, C1s spectrogram and the O1s spectrogram of fiber natural polymeric adsorbent of the present invention.As can be seen from Figure 2, SHR, primarily of C, H, O composition, also has a small amount of N element.As can be seen from Fig. 3,284.7,286.5,288.3eV is respectively C-C in SHR C1s, the characteristic peak of C-O (alcohol, phenolic hydroxyl group) and C=O (carboxyl), illustrates in SHR containing carbon-carbon single bond and carbon-carbon double bond and the carbon atom that is connected with alcohol, phenolic hydroxyl group and carboxyl.As shown in Figure 4,531.9 are respectively C=O in O1s (carboxyl) and C-O (carboxyl oxygen, hydroxyl) with 533.6eV, illustrate that the oxygen atom in SHR mainly exists with carboxyl and OH-form, in SHR, contained atom N then exists with the form of protein.From the above analysis, cellulose, lignin and protein is comprised in SHR.This result is consistent with results of elemental analyses.
3, elementary analysis
By elementary analysis, fiber natural polymeric adsorbent finds that the content distribution of elements is as follows in SHR: C:50.22%, H:7.58 %, N:5.71 %, S:0.49%.Other elements do not found in addition to oxygen are analyzed, so the content of oxygen is 36% according to XPS.And the atomic ratio of contained element is C/O=1.86/1 in SHR; C/N=10.21/1; H/C=1.82/1.Usually in cellulose and lignin, C/O is respectively 1:1 and 2:1, there is not N and S element, and in SHR the ratio of C/O between 1:1 and 2:1, illustrate in SHR that namely comprising lignin also comprises cellulose, also containing a small amount of protein, in preparation process, most of protein is by washing removing, so protein exists with the form of glycoprotein in SHR.Show that SHR is primarily of lignin, cellulose composition thus, also containing a small amount of glycoprotein, nontoxic, pollution-free, be the good edibility natural polymer of a kind of bio-compatible.
(3)the absorption property of fiber natural polymeric adsorbent
1, the adsorption experiment of heavy metal lead ion
Method of testing: getting 50 mL concentration is 200 mg/L lead ion solution, pH=5.0.In this solution, add adsorbent SHR of the present invention, the addition of adsorbent is 0.3 g, with rotating speed 150r/min under room temperature, mixed liquor 60 min of constant temperature oscillation lead solution and this adsorbent, leaves standstill, suction filtration, filtrate, by the concentration of determination of color residual heavy metal lead ion, calculates clearance.
Test result: the clearance of heavy metal lead ion is 99.11%.
2, the adsorption experiment of heavy metal copper ion
Method of testing: getting 50 mL concentration is 100 mg/L copper ion solutions, pH=4.7.In this solution, add adsorbent SHR of the present invention, the addition of adsorbent is 0.1 g, with rotating speed 150r/min under room temperature, mixed liquor 60 min of constant temperature oscillation copper solution and this adsorbent, leaves standstill, suction filtration, filtrate, by the concentration of determination of color residual heavy metal copper ion, calculates clearance.
Test result: the clearance of heavy metal copper ion is 82.55%.
3, to the adsorption experiment of wastewater containing methylene blue
Method of testing: getting 50 mL concentration is the waste water of 100 mg/L containing methylene blue.Adsorbent SHR of the present invention is added in this waste water, the addition of adsorbent is 0.05 g, with rotating speed 150r/min under room temperature, mixed liquor 30 min of constant temperature oscillation waste water and this adsorbent, leave standstill, suction filtration, filtrate measures the concentration of remaining methylene blue with ultraviolet-visible spectrophotometry, calculates percent of decolourization.
Test result: to being 98.54% containing the percent of decolourization of methylene blue.
4, to the adsorption experiment containing malachite green wastewater
Method of testing: getting 50 mL concentration is the waste water of 50 mg/L containing malachite green.In this waste water, add adsorbent SHR of the present invention, the addition of adsorbent is 0.3 g, with rotating speed 150r/min under room temperature, mixed liquor 30 min of constant temperature oscillation waste water and this adsorbent, leaves standstill, suction filtration, filtrate measures the concentration of remaining malachite green with ultraviolet-visible spectrophotometry, calculates percent of decolourization.
Test result: to being 98% containing the percent of decolourization of malachite green.
5, to the adsorption experiment containing basic fuchsin waste water
Method of testing: getting 50 mL concentration is the waste water of 100 mg/L containing basic fuchsin.Adsorbent SHR of the present invention is added in this waste water, the addition of adsorbent is 0.05 g, with rotating speed 150r/min under room temperature, mixed liquor 30 min of constant temperature oscillation waste water and this adsorbent, leave standstill, suction filtration, filtrate measures the concentration of residual alkalinity magenta with ultraviolet-visible spectrophotometry, calculates percent of decolourization.
Test result: in waste water containing basic fuchsin percent of decolourization be 95.72%.
6, to the adsorption experiment containing naphthols waste water
Method of testing: getting 50 mL concentration is the waste water of 200 mg/L containing naphthols.In this waste water, add adsorbent SHR of the present invention, the addition of adsorbent is 0.15 g, with rotating speed 150r/min at 45 DEG C, mixed liquor 60 min of constant temperature oscillation waste water and this adsorbent, leaves standstill, suction filtration, filtrate, by the concentration of the remaining naphthols of determination of color, calculates clearance.
Test result: to being 69.36% containing the clearance of naphthols.
In sum, the fiber natural polymeric adsorbent SHR for preparing of the present invention has good absorption property to containing heavy metal lead ion and copper ion, dyestuff methylene blue, malachite green and basic fuchsin and organic pollution naphthols waste water.Therefore, can be used for industrial treatment and contain heavy metal ion, dyestuff and organic waste water.Simultaneously because the main component of this adsorbent is lignin, cellulose and a small amount of glycoprotein, nontoxic, pollution-free, be the good edibility natural polymer of a kind of bio-compatible, therefore, also can be used as the rapid detoxification agent of heavy metal poisoning.
Accompanying drawing explanation
Fig. 1 is the FT-IR spectrogram of fiber natural polymeric adsorbent of the present invention (SHR);
Fig. 2 is the XPS spectrum figure of fiber natural polymeric adsorbent of the present invention (SHR);
Fig. 3 is the C1s spectrogram of fiber natural polymeric adsorbent of the present invention (SHR);
Fig. 4 is the O1s spectrogram of fiber natural polymeric adsorbent of the present invention (SHR);
Fig. 5 is that fiber natural polymeric adsorbent of the present invention (SHR) absorption property to different material compares.
Detailed description of the invention
Below by specific embodiment prepared by works further instruction to fiber natural polymeric adsorbent of the present invention.
embodiment 1
Get fresh bean dregs 10 g, wash 3 times with distilled water, cross and filter water-soluble substances.Then use 60% alcohol immersion 3 h, filter, distilled water washs 1 time, then soaks 1 h with the sodium acid carbonate of pH=8, filters, and respectively with ethanol, distilled water washing, removes other small-molecule substance; 65 DEG C of vacuum drying, pulverize, and cross 100 mesh sieves, both obtain fiber natural polymeric adsorbent (SHR).
The absorption property of this fiber natural polymeric adsorbent: be 99.11% to the clearance of Pb In Exhausted Water ion; Be 82.55% to copper ion clearance; Be 98.54% to the percent of decolourization of methylene blue; Be 98% to the percent of decolourization of malachite green; Be 95.72% to the percent of decolourization of basic fuchsin; Be 69.36% to the clearance of naphthols.
embodiment 2
Get fresh bean dregs 30 g, wash 3 times with distilled water, cross and filter water-soluble substances.Then use 75% alcohol immersion 1 h, filter, distilled water washs 2 times, then soaks 5 h with the sodium acid carbonate of pH=8, filter, respectively with ethanol, distilled water washing, remove other small-molecule substance, 35 DEG C of vacuum drying, pulverizing, cross 100 mesh sieves, both fiber natural polymeric adsorbent (SHR).Its absorption property is with embodiment 1.
embodiment 3
Get fresh bean dregs 30 g, wash 5 times with distilled water, cross and filter water-soluble substances.Then use 75% alcohol immersion 5 h, filter, distilled water washs 2 times, then soaks 1 h with the sodium acid carbonate of pH=9, filter, respectively with ethanol, distilled water washing, remove other small-molecule substance, 45 DEG C of vacuum drying, pulverizing, cross 100 mesh sieves, both fiber natural polymeric adsorbent (SHR).Its absorption property is with embodiment 1.
embodiment 4
Get fresh bean dregs 50 g, wash 5 times with distilled water, cross and filter water-soluble substances.Then use 50% alcohol immersion 10 h, filter, distilled water washs 1 time, then soaks 1 h with the sodium acid carbonate of pH=10, filter, respectively with ethanol, distilled water washing, remove other small-molecule substance, 65 DEG C of vacuum drying, pulverizing, cross 100 mesh sieves, both fiber natural polymeric adsorbent (SHR).Its absorption property is with embodiment 1.
embodiment 5
Get fresh bean dregs 50 g, wash 10 times with distilled water, cross and filter water-soluble substances.Then use 80% alcohol immersion 5 h, filter, distilled water washs 1 time, then soaks 5 h with the sodium acid carbonate of pH=8, filter, respectively with ethanol, distilled water washing, remove other small-molecule substance, 65 DEG C of vacuum drying, pulverizing, cross 100 mesh sieves, both fiber natural polymeric adsorbent (SHR).Its absorption property is with embodiment 1.
embodiment 6
Get fresh bean dregs 100 g, wash 10 times with distilled water, cross and filter water-soluble substances.Then use 60% alcohol immersion 1 h, filter, distilled water washs 2 times, then soaks 10 h with the sodium acid carbonate of pH=10, filter, respectively with ethanol, distilled water washing, remove other small-molecule substance, 65 DEG C of vacuum drying, pulverizing, cross 100 mesh sieves, both fiber natural polymeric adsorbent (SHR).Its absorption property is with embodiment 1.
embodiment 7
Get fresh bean dregs 100 g, wash 3 times with distilled water, cross and filter water-soluble substances.Then use 75% alcohol immersion 5 h, filter, distilled water washs 2 times, then soaks 3 h with the sodium acid carbonate of pH=11, filter, respectively with ethanol, distilled water washing, remove other small-molecule substance, 65 DEG C of vacuum drying, pulverizing, cross 100 mesh sieves, both fiber natural polymeric adsorbent (SHR).Its absorption property is with embodiment 1.

Claims (7)

1. a purposes for fiber natural polymeric adsorbent naphthols in absorption waste water, is characterized in that: described fiber natural polymeric adsorbent has following technique to be prepared from: by fresh bean dregs first with distilled water washing, cross and filter water-soluble substances; Use alcohol solution dipping again, filter, distilled water washs; Then soak with sodium bicarbonate solution; Filter, respectively with ethanol, distilled water washing, removing small-molecule substance; Last vacuum drying, pulverizes, and crosses 100 mesh sieves, both obtains fiber natural polymeric adsorbent.
2. fiber natural polymeric adsorbent, in the purposes of adsorbing naphthols in waste water, is characterized in that as claimed in claim 1: described bean dregs are the insoluble sludge that bean product processing industry produces soya-bean milk, bean curd, soya-bean milk gained.
3. fiber natural polymeric adsorbent, in the purposes of adsorbing naphthols in waste water, is characterized in that: the mass percent of described ethanolic solution is 50 ~ 80% as claimed in claim 1.
4. fiber natural polymeric adsorbent, in the purposes of adsorbing naphthols in waste water, is characterized in that: in described ethanolic solution, soak time is 1 ~ 10h as claimed in claim 1.
5. fiber natural polymeric adsorbent, in the purposes of adsorbing naphthols in waste water, is characterized in that: the time of soaking in described sodium bicarbonate solution is 1 ~ 10h as claimed in claim 1.
6. fiber natural polymeric adsorbent, in the purposes of adsorbing naphthols in waste water, is characterized in that: pH=8 ~ 11 of described sodium bicarbonate solution as claimed in claim 1.
7. fiber natural polymeric adsorbent, in the purposes of adsorbing naphthols in waste water, is characterized in that: described vacuum drying carries out at 35 ~ 65 DEG C as claimed in claim 1.
CN201310059836.4A 2013-02-26 2013-02-26 Fiber natural polymeric adsorbent and application thereof Expired - Fee Related CN103100376B (en)

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CN103447007A (en) * 2013-07-26 2013-12-18 北京工业大学 Modified bean dreg adsorbent and preparation method as well as application thereof
MX2017002004A (en) 2014-08-15 2017-05-12 Halosource Inc Granular filtration media mixture and uses in water purification.
CN105170077B (en) * 2015-09-30 2017-10-27 太仓碧奇新材料研发有限公司 The preparation method of pinkish red chalk powder composite material in a kind of removal dyeing waste water
CN105080514B (en) * 2015-10-09 2017-04-12 吉首大学 Preparation method of cellulose-base absorbent
CN105174354B (en) * 2015-10-12 2017-11-14 南阳师范学院 A kind of method that Wastewater Dyes are removed using waste edible fungus gurry
CN107497408B (en) * 2017-10-16 2020-10-02 西南大学 Preparation method and application of novel polycyclic aromatic hydrocarbon compound (PAHs) adsorbent
CN107865443A (en) * 2017-10-26 2018-04-03 吕燕强 A kind of preparation method of gomuti palm powder
CN109231348A (en) * 2018-11-20 2019-01-18 兰州城市学院 The application of Propiram mycelium pellet and its derivative in processing organic dye waste water

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CN101239305A (en) * 2008-03-06 2008-08-13 上海交通大学 Method for preparing modified plant fibrous sale price biological adsorption agent
CN101703921B (en) * 2009-10-31 2012-01-11 华南理工大学 Method for preparing adsorbent by modifying pineapple peel residues

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