CN108217892A - A kind of preparation method of cellulose-chitosan green flocculation material for the processing fabric dyeing waste water of multicomponent containing silk - Google Patents
A kind of preparation method of cellulose-chitosan green flocculation material for the processing fabric dyeing waste water of multicomponent containing silk Download PDFInfo
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- CN108217892A CN108217892A CN201810009076.9A CN201810009076A CN108217892A CN 108217892 A CN108217892 A CN 108217892A CN 201810009076 A CN201810009076 A CN 201810009076A CN 108217892 A CN108217892 A CN 108217892A
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- chitosan
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5263—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using natural chemical compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
- C02F1/56—Macromolecular compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/30—Nature of the water, waste water, sewage or sludge to be treated from the textile industry
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- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
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- General Chemical & Material Sciences (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention discloses a kind of for handling the preparation method of the cellulose chitosan green flocculation material of the fabric dyeing waste water of multicomponent containing silk.Main points using method are that cellulose and chitosan are dissolved in sodium hydroxide and urea mixed solution, are crosslinked the two by glutaraldehyde, are washed through deionized water, and environmental-friendly, efficient flocculating cellulose chitosan green flocculation material is finally made.The cellulose and chitosan that the present invention uses are natural polymer organic matter, biodegradable.Simultaneously, the raw material range for preparing flocculation material has been expanded in the introducing of chitosan, the application field of chitosan is opened up, it proposes and a kind of prepares opening one's minds for novel green flocculation material, it can effectively solve that traditional flocculation material difficulty is biodegradable, easily causes secondary pollution problems, have important practical significance.
Description
Technical field
It is more particularly to a kind of for processing multicomponent containing silk the present invention relates to a kind of preparation method of green flocculation material
The preparation method of the cellulose of fabric dyeing waste water-chitosan green flocculation material, belongs to field of environment engineering technology.
Background technology
With the rapid development of the printing and dyeing industry, the type and quantity of dyeing waste water rapidly increase, to the pollution of water body also day
Become extensive and serious, threaten the health and safety of the mankind.The flocculation material for being presently used for processing dyeing waste water is mainly polypropylene
Acyl class compound, but such flocculation material cannot be effectively biodegradable, and catabolite acrylamide monomer is toxic to human body,
Secondary pollution can be caused to water body.Therefore, the present invention is i.e. based on natural origin, biodegradable cellulose and chitosan
Raw material prepares a kind of environmental-friendly, efficient flocculating green flocculation material.
Cellulose is the natural polymer that content is most abundant on the earth, by single D-Glucose unit by β-
1,4- glycosidic bond chains are formed by connecting.Cellulose is not soluble in water and common organic solvents, is the main component of plant cell wall.Shell
Glycan is to be obtained by the chitin that nature is widely present through deacetylation, biological functionality and compatibility, blood phase
The excellent performances such as capacitive, safety, microbic resolvability are by extensive concern.
At present, widely used traditional flocculant faces difficult for biological degradation, and secondary pollution is caused to water body, and flocculating effect is poor
The problems such as.In flocculant preparation field, a kind of Chinese patent (CN201410798666.6) " Cellulose/Chitosan composite pellets
And preparation method and application " be dissolved in cellulose and chitosan in ionic liquid respectively, heat cross-linking simultaneously obtains in coagulating bath
It is characterized to gel state composite pellets, and to its adsorptivity;A kind of Chinese patent (CN201110242033.3) " macromolecule wadding
The preparation method and application of solidifying agent " is crosslinked, acrylamide graft, xanthogenation using konjaku flour as raw material using epoxychloropropane
Obtain final products konjaku graft type xanthate;Chinese patent (CN201510389451.3) is " a kind of for coking wastewater
Composite type polymeric flocculant and preparation method thereof " is using a variety of modified starches as raw material, and more under initiator and mild acid conditions
Kind monomer carries out graft copolymerization, modified starch graft copolymer is prepared, and be made again with the blending of a variety of inorganic flocculating agents
Mould assembly high polymer coagulant;United States Patent (USP) (US 20150197439A1) " a kind of mud dewatering method " mixes sludge and cellulose
Conjunction obtains modified sewage sludge, then modified sewage sludge is mixed with coagulating agent is modified sludge condensation.So far, it yet there are no while sharp
It is basic raw material with cellulose and chitosan, is used to prepare the related process skill of the environmental-friendly green flocculation material of efficient flocculating
Art occurs.
Cellulose and chitosan are natural polymer, derive from a wealth of sources, is biodegradable, is cheap, by it
A kind of novel green flocculation material is prepared as basic raw material, the advantages that biodegradable, added value of product is high is will be provided with, is new
The preparation of type green flocculation material provides one and opens one's minds.
Invention content
The problems such as in order to overcome the flocculation material prepared at present biodegradable, while recycling cellulose and shell
Glycan, to prepare the biodegradable green flocculation material of high added value, the object of the present invention is to provide one kind for handling print
Contaminate the preparation method of cellulose-chitosan green flocculation material of waste water.
To achieve the above object, the technical scheme is that using following steps:
1) cellulose powder is dissolved in the 6wt% sodium hydroxides and 14wt% urea liquids of -10~-15 DEG C of precoolings,
Obtain colourless, transparent cellulose solution;
2) it dissolving chitosan in 1wt% acetic acid solutions, magnetic stirring apparatus 250r/min stirs 1~2h at normal temperatures,
By the protonated amino of chitosan, chitosan turbid solution is obtained;
3) the chitosan turbid solution that will be obtained in step 2) is dissolved in 7wt% sodium hydroxides and 10wt% urea liquids,
Through 3 freeze cycles, colourless, transparent chitosan solution is obtained;
4) by the chitosan solution obtained in the cellulose solution and step 3) that are obtained in step 1) at 25~80 DEG C by
It is mixed under 200r/min magnetic agitations according to certain mass ratio, adds in a certain amount of 20wt% glutaraldehyde solutions, stirring is anti-
25~150min is answered, obtains gum-like product;
5) gum-like product obtained in step 4) is washed with deionized to neutrality, is washed away with absolute ethyl alcohol unreacted
Glutaraldehyde, then cleaned product with deionized water, it is dried under room temperature to constant weight, obtains cellulose-chitosan green flocculation material.
3 freeze cycles stir 1h at normal temperatures for chitosan solution is freezed 30min at -10 DEG C.
The cellulose and the mass ratio of chitosan are 1:0.2~5;The addition of 20wt% glutaraldehyde solutions is 0.20
~1.20g/g.
Compared with background technology, the invention has the advantages that:
The present invention introduces chitosan in green flocculation material is prepared, and has expanded the raw material model for preparing green flocculation material
It encloses, opened up the application field of chitosan and is conducive to accelerate the limitation that breakthrough prepares flocculated material source;It proposes simultaneously high
Value is opened one's minds using one of cellulose and chitosan, meets national development circular economy policy.
With reference to specific embodiment, the invention will be further described.
Embodiment 1:
1) cellulose powder is dissolved in the 6wt% sodium hydroxides and 14wt% urea liquids of -10 DEG C of precoolings, obtains nothing
Color, transparent cellulose solution;
2) it dissolves chitosan in 1wt% acetic acid solutions, magnetic stirring apparatus 250r/min stirs 1.5h at normal temperatures, will
Protonated amino in chitosan obtains chitosan turbid solution;
3) the chitosan turbid solution that will be obtained in step 2) is dissolved in 7wt% sodium hydroxides and 10wt% urea liquids,
Chitosan solution is freezed into 30min at -10 DEG C, stirs 1h at normal temperatures, through 3 freeze cycles, obtains colourless, transparent shell
Glycan solution;
4) by the chitosan solution obtained in the cellulose solution and step 3) that are obtained in step 1) at 40 DEG C according to fibre
Dimension element and chitosan 1:5 mass ratio is mixed under 200r/min magnetic agitations, adds in 0.20g/g 20wt% glutaraldehydes
Solution is stirred to react 25min, obtains gum-like product;
5) gum-like product obtained in step 4) is washed with deionized to neutrality, is washed away with absolute ethyl alcohol unreacted
Glutaraldehyde, then be washed till product totally with deionized water, it dries at normal temperatures to constant weight, obtains cellulose-chitosan green wadding
Gel material (a).
Embodiment 2:
1) cellulose powder is dissolved in the 6wt% sodium hydroxides and 14wt% urea liquids of -15 DEG C of precoolings, obtains nothing
Color, transparent cellulose solution;
2) it dissolves chitosan in 1wt% acetic acid solutions, magnetic stirring apparatus 250r/min stirs 2h at normal temperatures, by shell
Protonated amino in glycan obtains chitosan turbid solution;
3) the chitosan turbid solution that will be obtained in step 2) is dissolved in 7wt% sodium hydroxides and 10wt% urea liquids,
Chitosan solution is freezed into 30min at -10 DEG C, stirs 1h at normal temperatures, through 3 freeze cycles, obtains colourless, transparent shell
Glycan solution;
4) by the chitosan solution obtained in the cellulose solution and step 3) that are obtained in step 1) at 55 DEG C according to fibre
Dimension element and chitosan 1:0.8 mass ratio is mixed under 200r/min magnetic agitations, adds in 1.20g/g 20wt% penta 2
Aldehyde solution, is stirred to react 65min, obtains gum-like product;
5) gum-like product obtained in step 4) is washed with deionized to neutrality, is washed away with absolute ethyl alcohol unreacted
Glutaraldehyde, then be washed till product totally with deionized water, it dries at normal temperatures to constant weight, obtains cellulose-chitosan green wadding
Gel material (b).
Embodiment 3:
1) cellulose powder is dissolved in the 6wt% sodium hydroxides and 14wt% urea liquids of -12 DEG C of precoolings, obtains nothing
Color, transparent cellulose solution;
2) it dissolves chitosan in 1wt% acetic acid solutions, magnetic stirring apparatus 250r/min stirs 1h at normal temperatures, by shell
Protonated amino in glycan obtains chitosan turbid solution;
3) the chitosan turbid solution that will be obtained in step 2) is dissolved in 7wt% sodium hydroxides and 10wt% urea liquids,
Chitosan solution is freezed into 30min at -10 DEG C, stirs 1h at normal temperatures, through 3 freeze cycles, obtains colourless, transparent shell
Glycan solution;
4) by the chitosan solution obtained in the cellulose solution and step 3) that are obtained in step 1) at 25 DEG C according to fibre
Dimension element and chitosan 1:0.2 mass ratio is mixed under 200r/min magnetic agitations, adds in 0.50g/g 20wt% penta 2
Aldehyde solution, is stirred to react 100min, obtains gum-like product;
5) gum-like product obtained in step 4) is washed with deionized to neutrality, is washed away with absolute ethyl alcohol unreacted
Glutaraldehyde, then be washed till product totally with deionized water, it dries at normal temperatures to constant weight, obtains cellulose-chitosan green wadding
Gel material (c).
Embodiment 4:
1) cellulose powder is dissolved in the 6wt% sodium hydroxides and 14wt% urea liquids of -13 DEG C of precoolings, obtains nothing
Color, transparent cellulose solution;
2) it dissolves chitosan in 1wt% acetic acid solutions, magnetic stirring apparatus 250r/min stirs 1.5h at normal temperatures, will
Protonated amino in chitosan obtains chitosan turbid solution;
3) the chitosan turbid solution that will be obtained in step 2) is dissolved in 7wt% sodium hydroxides and 10wt% urea liquids,
Chitosan solution is freezed into 30min at -10 DEG C, stirs 1h at normal temperatures, through 3 freeze cycles, obtains colourless, transparent shell
Glycan solution;
4) by the chitosan solution obtained in the cellulose solution and step 3) that are obtained in step 1) at 80 DEG C according to fibre
Dimension element and chitosan 1:1 mass ratio is mixed under 200r/min magnetic agitations, adds in 0.80g/g 20wt% glutaraldehydes
Solution is stirred to react 150min, obtains gum-like product;
5) gum-like product obtained in step 4) is washed with deionized to neutrality, is washed away with absolute ethyl alcohol unreacted
Glutaraldehyde, then be washed till product totally with deionized water, it dries at normal temperatures to constant weight, obtains cellulose-chitosan green wadding
Gel material (d).
Measure 4 kinds of celluloses-chitosan green flocculation that embodiment 1, embodiment 2, embodiment 3, embodiment 4 are prepared
Material is to the treatment effect of the fabric dyeing waste water of multicomponent containing silk.Table 1 is by embodiment 1, embodiment 2, embodiment 3, embodiment 4
The cellulose of preparation-chitosan green flocculation material is respectively to the characterization knot of the fabric disposal effect of dyeing wastewater of multicomponent containing silk
Fruit.By data in table 1 it is found that prepared green flocculation material exists to the COD removal rates of the fabric dyeing waste water of multicomponent containing silk
69.0%-74.7%, for turbidity removal rate in 87.4%-93.7%, dyeing waste water COD and turbidity removal are with obvious effects.Illustrate according to
Cellulose-chitosan green flocculation material prepared by the technology is held in the palm to containing a multicomponent fabric dyeing waste water with good coagulation
Sedimentation effect can be applied to the coagulating sedimentation workshop section of the fabric dyeing waste water of multicomponent containing silk.
Table 1
Listed above is only specific embodiments of the present invention.The present invention is not limited to above example, can also there are many
Deformation.All deformations that those of ordinary skill in the art directly can export or associate from present disclosure, should all
It is considered protection scope of the present invention.
Claims (3)
1. a kind of preparation side of cellulose-chitosan green flocculation material for the processing fabric dyeing waste water of multicomponent containing silk
Method, which is characterized in that include the following steps:
1) cellulose powder is dissolved in the 6wt% sodium hydroxides and 14wt% urea liquids of -10~-15 DEG C of precoolings, obtained
Colourless, transparent cellulose solution;
2) it dissolves chitosan in 1wt% acetic acid solutions, magnetic stirring apparatus 250r/min stirs 1~2h at normal temperatures, by shell
The protonated amino of glycan obtains chitosan turbid solution;
3) the chitosan turbid solution that will be obtained in step 2) is dissolved in 7wt% sodium hydroxides and 10wt% urea liquids, through 3
Secondary freeze cycle obtains colourless, transparent chitosan solution;
4) by the chitosan solution obtained in the cellulose solution and step 3) that are obtained in step 1) at 25~80 DEG C according to one
Determine mass ratio to be mixed under 200r/min magnetic agitations, add in a certain amount of 20wt% glutaraldehyde solutions, be stirred to react 25
~150min, obtains gum-like product;
5) gum-like product obtained in step 4) is washed with deionized to neutrality, unreacted penta 2 is washed away with absolute ethyl alcohol
Aldehyde, then cleaned product with deionized water, it is dried under room temperature to constant weight, obtains cellulose-chitosan green flocculation material.
It is 2. according to claim 1 a kind of green for handling cellulose-chitosan of the fabric dyeing waste water of multicomponent containing silk
The preparation method of color flocculation material, it is characterised in that:Chitosan solution is is freezed by 3 freeze cycles at -10 DEG C
30min stirs 1h at normal temperatures.
It is 3. according to claim 1 a kind of green for handling cellulose-chitosan of the fabric dyeing waste water of multicomponent containing silk
The preparation method of color flocculation material, it is characterised in that:The cellulose and the mass ratio of chitosan are 1:0.2~5;20wt%
The addition of glutaraldehyde solution is 0.20~1.20g/g.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN111348755A (en) * | 2020-04-03 | 2020-06-30 | 姜文杰 | Sewage treatment agent for printing and dyeing textile industry and preparation method thereof |
CN112708170A (en) * | 2020-12-10 | 2021-04-27 | 东华理工大学 | Photochromic biomass-based flexible gel film |
CN114174387A (en) * | 2019-08-02 | 2022-03-11 | 株式会社大赛璐 | Porous cellulose particles and method for producing same |
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