CN107164425A - A kind of preparation method of flocculation decoloration dyeing waste water bacteria cellulose based composites - Google Patents

A kind of preparation method of flocculation decoloration dyeing waste water bacteria cellulose based composites Download PDF

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Publication number
CN107164425A
CN107164425A CN201710220197.3A CN201710220197A CN107164425A CN 107164425 A CN107164425 A CN 107164425A CN 201710220197 A CN201710220197 A CN 201710220197A CN 107164425 A CN107164425 A CN 107164425A
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China
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bacteria cellulose
waste water
dyeing waste
based composites
flocculation decoloration
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CN201710220197.3A
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Chinese (zh)
Inventor
邵蓉蓉
郑菲菲
张勇
姚菊明
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Zhejiang Sci Tech University ZSTU
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Zhejiang Sci Tech University ZSTU
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    • CCHEMISTRY; METALLURGY
    • C12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12PFERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P19/00Preparation of compounds containing saccharide radicals
    • C12P19/04Polysaccharides, i.e. compounds containing more than five saccharide radicals attached to each other by glycosidic bonds
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/286Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/52Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • C02F1/54Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
    • C02F1/56Macromolecular compounds

Abstract

The invention discloses a kind of preparation method of flocculation decoloration dyeing waste water bacteria cellulose based composites.The method main points of use are, by dynamic fermentation culture, to obtain the bacteria cellulose of secretion in the medium by bacterium, then porous adsorbing material is carried on the bacteria cellulose after purification process, obtain flocculation decoloration dyeing waste water bacteria cellulose based composites.The method is simple to operate, and production cost is low, and the composite of acquisition can be efficiently applied to the flocculation decoloration processing of dyeing waste water etc., and material environmental protection itself, biodegradable, there is important application value in flocculation decoloration field.

Description

A kind of preparation method of flocculation decoloration dyeing waste water bacteria cellulose based composites
Technical field
The present invention relates to a kind of preparation method of flocculation decoloration composite, more particularly to a kind of flocculation decoloration dyeing waste water With the preparation method of bacteria cellulose based composites, belong to high-molecular organic material preparing technical field.
Background technology
In recent years, the problem of water environment pollution is always restriction and puzzlement human development, wherein dyeing waste water are arranged due to it It is high-volume big, the features such as composition is complicated, organic pollution content is big, colourity is high, as one of most intractable industrial wastewater.Cause This, realizing the efficient process of dyeing waste water turns into the most important thing for administering water environment pollution.
Flocculation decoloration technology because of it efficiently, low cost the features such as, particulate matter, dyestuff, heavy metal in water body Played an important role always in terms of removing.Dyeing waste water complicated component, existing flocculant is difficult to will be complicated various in waste water Pollutant effectively remove.At present, polyacrylamide as high polymer coagulant representative, although product stability is good, flocculation Effect is good, but it synthesizes that cost is high, monomer harm is big and raw material is non-renewable, and biodegradation is difficult to after use, to environment and There are many potential safety hazards in the mankind.Therefore, the novel flocculation decoloring material of exploitation green high-efficient is led to the processing of current water environment Domain has important practical significance.
In flocculation decoloration field of material preparation, a kind of Chinese patent (CN201610059898.9) " dendroid cellulose base Both sexes flocculating decoloring agent and preparation method thereof " utilizes sodium periodate oxidation cellulose using cellulosic material as molecular skeleton Material formation dialdehyde cellulose, is then bonded grafting polyethylene imine and is formed using aldehyde radical and amino progress schiff base structure, with Water is that successively prepared by addition cellulosic material, sodium metaperiodate and polyethyleneimine for solvent progress, by changing fiber material The mass ratio of material and polyethyleneimine regulates and controls the surface charge properties and avtive spot of the flocculating decoloring agent, is prepared for flocculation effect Can height, effect stability, environment-friendly flocculation material." one kind utilizes cellulose base to Chinese patent (CN201510115930.6) Dyeing waste water is introduced waste water storage pond by the method for flocculant coagulation decoloration dyeing waste water " using method, first aggregated aluminum sulfate De- steady pretreatment, then put into cellulose base flocculant and a certain amount of flocculation aid, is stirred, stands and precipitates, finally give compared with For limpid supernatant and flocculate precipitate, supernatant can contemplate reuse printing and dyeing workshop section or further biochemical treatment, simplify The handling process of decolorizing printing and dyeing waste water, further increases dyeing waste water purification efficiency, with important production and environment protection significance. Chinese patent (CN201610362998.9) be " a kind of bamboo pulp fiber element & polyvinylformamide composite flocculation decoloring materials Bamboo pulp pulpboard is passed through cutting, washing, dry, pulverization process comminuted cellulosic by preparation method ", molten using sodium hydroxide and urea Liquid freezing processing dissolves cellulose, triggers through free radical and polyvinylformamide graft copolymerization is made a kind of composite flocculation and taken off Color material product.United States Patent (USP) (A1 of US 20130256218) " Printing and dyeing wastewater Treatment and reuse apparatus and method therefor " provide a kind of by desulfurization, catalytic electrolysis, wadding What solidifying, biochemical treatment, two catalytic electrolysis, filtering and UF membrane were combined is used for treatment of dyeing wastewater and reuse method, effectively drop The low COD of waste water, reduces the consumption of chemical agent, reduces the formation of sludge, realizes the high recycling of water Rate.So far, it yet there are no to prepare with porous material using the bacteria cellulose of dynamic fermentation culture and wadded a quilt with cotton for dyeing waste water The related process technologies of the solidifying composite decolourized occur.
Bacteria cellulose as one kind have ultra-fine, ultrapure, superelevation mechanical strength, high-crystallinity, high water-holding capacity and compared with The natural biological recyclable materials of the characteristics such as good biocompatibility, the bacteria cellulose-base flocculation decoloration material prepared will Produce huge economic and social benefit.
The content of the invention
In order to overcome Flocculants exist it is not biodegradable, production cost is high the problems such as, prepare operating method Simply, production cost is low, environmental protection, biodegradable bacteria cellulose based composites, the wadding applied to dyeing waste water It is solidifying to decolourize.It is an object of the invention to provide a kind of preparation side of flocculation decoloration dyeing waste water bacteria cellulose based composites Method.
To achieve the above object, technical scheme uses following implementation steps:
1) aseptically, bacterium is accessed in 100mL liquid fermentation mediums with oese, constant-temperature table shake is placed in Culture is swung, 29-34 DEG C of cultivation temperature, rotating speed 50-110r/min, incubation time 6-9d obtain a large amount of cotton-shaped scattered without pure The bacteria cellulose of change;
2) by step 1) obtained a large amount of cotton-shaped scattered not purified bacteria celluloses filter culture with 2 layers of gauze Base, is immersed in temperature for 70-90 DEG C, concentration in 0.1mol/L NaOH solution, wash away remained on surface bacterioprotein and Medium component inside cellulose, a NaOH solution is changed per 15-25min, and the thin of purifying is filtrated to get after circulating 3-5 times Fungin, then by magnetic agitation 5-15min in its acetic acid solution as 0.1%, filter off acetic acid solution, be placed on Bu Shi In funnel, pouring pouring deionized water, suction filtration, up to filtrate pH is neutrality, is freeze-dried, the bacteria cellulose purified repeatedly;
3) by step 2) the obtained bacteria cellulose of purifying divides equally 3-4 parts to be added to 100mL concentration is 3mol/L's In NaOH solution, magnetic agitation 20-40min forms it into dispersed system, and 0.5-0.8g porous adsorbing materials are added Into 30mL deionized waters, it is respectively added slowly to after magnetic agitation 5-15min in the NaOH aqueous solution of cellulose, mixed system 70-80 DEG C, 90-110r/min reaction 1-2h, separation of solid and liquid are carried out with centrifuge, then be washed with deionized water to neutrality, 60-80 DEG C Dry and disperse grinding, that is, obtain flocculation decoloration dyeing waste water bacteria cellulose based composites.
Described bacteria culture is one kind in gluconobacter sp (ATCC 49306), gluconobacter sp (CGMCC1671).
The formula of described liquid fermentation medium is:30-40g/L glucose, 30-40g/L fructose, 2.5-3.5g/L ferment Female powder, 4.5-5.5g/L tryptones, 0.8-1.2g/L sodium citrates, pH 4-6, sterilize through 110 DEG C of high temperature and high pressure steams 30min。
Described porous adsorbing material is one kind in activated carbon, diatomite, atlapulgite.
The beneficial benefit that the present invention has is:
The present invention is utilized respectively two kinds of strains of gluconobacter sp (ATCC 49306) and gluconobacter sp (CGMCC1671) and dynamically trained The bacteria cellulose material obtained is supported, is nanometer porous bacteria cellulose material, is more beneficial for loading it compared with plant cellulose His porous particle or powdered rubber, realize efficient flocculating decoloring effect, the composite of preparation compared with conventional polymer flocculant, With advantages such as biodegradable, raw material recyclabilities, and there is good flocculating decoloring effect to dyeing waste water, with weight The application value and social benefit wanted.
Brief description of the drawings
Fig. 1 is the field emission scanning electron microscope photo of bacteria cellulose prepared by the dynamic fermentation culture of embodiment 1.
Embodiment explanation
Embodiment 1:
1) gluconobacter sp (ATCC 49306) aseptically, is accessed into 100mL liquid fermentation mediums with oese (35g/L glucose, 30g/L fructose, 3.0g/L dusty yeasts, 5.5g/L tryptones, 1.2g/L sodium citrates, pH 5 pass through 110 DEG C of high temperature and high pressure steams sterilize 30min) in, it is placed in constant-temperature table concussion and cultivate, 29 DEG C of cultivation temperature, rotating speed 80r/min, Incubation time 6d, obtains a large amount of cotton-shaped scattered not purified bacteria celluloses;
2) by step 1) obtained a large amount of cotton-shaped scattered not purified bacteria celluloses filter culture with 2 layers of gauze Base, is immersed in temperature for 70 DEG C, and concentration is in 0.1mol/L NaOH solution, washes away the bacterioprotein and fiber of remained on surface Medium component inside element, a NaOH solution is changed per 20min, and the bacteria cellulose of purifying is filtrated to get after circulating 3 times, Again by magnetic agitation 10min in its acetic acid solution as 0.1%, acetic acid solution is filtered off, is placed in Buchner funnel, pours pouring Deionized water repeatedly suction filtration until filtrate pH for neutrality, freeze-drying, the bacteria cellulose purified;
3) by step 2) the obtained bacteria cellulose of purifying divides equally 4 parts to be added to 100mL concentration molten for 3mol/LNaOH In liquid, magnetic agitation 30min forms it into dispersed system, 0.5g activated carbons is added in 30mL deionized waters, magnetic It is respectively added slowly to after power stirring 10min in the NaOH aqueous solution of cellulose, 80 DEG C of mixed system, 100r/min reaction 1h, Separation of solid and liquid is carried out with centrifuge, then is washed with deionized water to neutrality, 70 DEG C dry and scattered grinding, that is, obtain flocculation decoloration print Contaminate waste water bacteria cellulose-base composite A.
Embodiment 2:
1) gluconobacter sp (CGMCC 1671) aseptically, is accessed into 100mL liquid fermentation mediums with oese (40g/L glucose, 35g/L fructose, 2.5g/L dusty yeasts, 5.0g/L tryptones, 0.8g/L sodium citrates, pH 4 pass through 110 DEG C of high temperature and high pressure steams sterilize 30min) in, it is placed in constant-temperature table concussion and cultivate, 32 DEG C of cultivation temperature, rotating speed 50r/min, Incubation time 9d, obtains a large amount of cotton-shaped scattered not purified bacteria celluloses;
2) by step 1) obtained a large amount of cotton-shaped scattered not purified bacteria celluloses filter culture with 2 layers of gauze Base, is immersed in temperature for 90 DEG C, during concentration is 0.1mol/LNaOH solution, washes away the bacterioprotein and cellulose of remained on surface Internal medium component, a NaOH solution is changed per 15min, and the bacteria cellulose of purifying is filtrated to get after circulating 4 times, then By magnetic agitation 5min in its acetic acid solution as 0.1%, acetic acid solution is filtered off, is placed in Buchner funnel, is poured pouring and go Ionized water repeatedly suction filtration until filtrate pH for neutrality, freeze-drying, the bacteria cellulose purified;
3) by step 2) the obtained bacteria cellulose of purifying divides equally 4 parts to be added to 100mL concentration molten for 3mol/LNaOH In liquid, magnetic agitation 20min forms it into dispersed system, 0.8g diatomite is added in 30mL deionized waters, magnetic It is respectively added slowly to after power stirring 15min in the NaOH aqueous solution of cellulose, 70 DEG C of mixed system, 90r/min reaction 1.5h, Separation of solid and liquid is carried out with centrifuge, then is washed with deionized water to neutrality, 60 DEG C dry and scattered grinding, that is, obtain flocculation decoloration print Contaminate waste water bacteria cellulose based composites B.
Embodiment 3:
1) gluconobacter sp (ATCC 49306) aseptically, is accessed into 100mL liquid fermentation mediums with oese (30g/L glucose, 40g/L fructose, 3.5g/L dusty yeasts, 4.5g/L tryptones, 1.0g/L sodium citrates, pH 6 pass through 110 DEG C of high temperature and high pressure steams sterilize 30min) in, it is placed in constant-temperature table concussion and cultivate, 34 DEG C of cultivation temperature, rotating speed 110r/min, Incubation time 8d, obtains a large amount of cotton-shaped scattered not purified bacteria celluloses;
2) by step 1) obtained a large amount of cotton-shaped scattered not purified bacteria celluloses filter culture with 2 layers of gauze Base, is immersed in temperature for 80 DEG C, during concentration is 0.1mol/LNaOH solution, washes away the bacterioprotein and cellulose of remained on surface Internal medium component, a NaOH solution is changed per 25min, and the bacteria cellulose of purifying is filtrated to get after circulating 5 times, then By magnetic agitation 15min in its acetic acid solution as 0.1%, acetic acid solution is filtered off, is placed in Buchner funnel, is poured pouring and go Ionized water repeatedly suction filtration until filtrate pH for neutrality, freeze-drying, the bacteria cellulose purified;
3) by step 2) the obtained bacteria cellulose of purifying divides equally 3 parts to be added to 100mL concentration molten for 3mol/LNaOH In liquid, magnetic agitation 40min forms it into dispersed system, and 0.8g atlapulgites are added in 30mL deionized waters, It is respectively added slowly to after magnetic agitation 5min in the NaOH aqueous solution of cellulose, 75 DEG C of mixed system, 110r/min reaction 2h, Separation of solid and liquid is carried out with centrifuge, then is washed with deionized water to neutrality, 80 DEG C dry and scattered grinding, that is, obtain flocculation decoloration print Contaminate waste water bacteria cellulose based composites C.
Flocculation decoloration dyeing waste water bacteria cellulose based composites prepared by embodiment 1, embodiment 2, embodiment 3 A, flocculation decoloration dyeing waste water bacteria cellulose based composites B, flocculation decoloration dyeing waste water bacteria cellulose-base are combined Material C is applied to the treatment effect of dyeing waste water flocculation decoloration process, and measure and calculation its chroma removal rate, turbidity removal rate, CODCrClearance.Table 1 is that flocculation decoloration dyeing waste water bacteria cellulose based composites are applied to dyeing waste water flocculation decoloration Chroma removal rate, turbidity removal rate, the COD of processCrThe results of measuring of clearance.The data in table 1, using institute of the present invention The bacteria cellulose based composites that the preparation method stated is obtained are applied to the flocculation treatment of dyeing waste water, waste water clearance rate Up to 86.3-90.2%, turbidity removal rate reaches 78.5-87.6%, CODCrClearance is 35.7-54.9%, illustrates the wadding prepared Solidifying decolouring dyeing waste water bacteria cellulose based composites have good flocculation sediment and decolorizing effect to dyeing waste water.
Such as Fig. 1, the field emission scanning electron microscope photo of the bacteria cellulose prepared from the dynamic fermentation culture of embodiment 1 can Go out, bacteria cellulose is very thin, filament diameter belongs to nanometer range, with porous network structure, be conducive to other porous masses Load.
Table 1
Listed above is only the specific embodiment of the present invention.The invention is not restricted to above example, there can also be many Deformation.All deformations that one of ordinary skill in the art directly can export or associate from present disclosure, all should It is considered protection scope of the present invention.

Claims (4)

1. a kind of flocculation decoloration dyeing waste water preparation method of bacteria cellulose based composites, is mainly included the following steps that:
1) aseptically, bacterium is accessed in 100mL liquid fermentation mediums with oese, constant-temperature table concussion training is placed in Support, 29-34 DEG C of cultivation temperature, rotating speed 50-110r/min, incubation time 6-9d, obtain a large amount of cotton-shaped scattered not purified Bacteria cellulose;
2) by step 1) obtained a large amount of cotton-shaped scattered not purified bacteria celluloses filter culture medium with 2 layers of gauze, soak Bubble temperature be 70-90 DEG C, concentration for 0.1mol/L NaOH solution in, wash away the bacterioprotein and cellulose of remained on surface Internal medium component, a NaOH solution is changed per 15-25min, and the bacterial fibers of purifying are filtrated to get after circulating 3-5 times Element, then by magnetic agitation 5-15min in its acetic acid solution as 0.1%, filter off acetic acid solution, be placed on Buchner funnel In, pouring pouring deionized water, suction filtration, up to filtrate pH is neutrality, is freeze-dried, the bacteria cellulose purified repeatedly;
3) by step 2) the obtained bacteria cellulose of purifying divides equally 3-4 parts to be added to the NaOH that 100mL concentration is 3mol/L molten In liquid, magnetic agitation 20-40min forms it into dispersed system, and 0.5-0.8g porous adsorbing materials are added into 30mL In deionized water, it is respectively added slowly to after magnetic agitation 5-15min in the NaOH aqueous solution of cellulose, mixed system 70-80 DEG C, 90-110r/min reaction 1-2h, carries out separation of solid and liquid with centrifuge, then be washed with deionized water to neutrality, 60-80 DEG C dries And scattered grinding, that is, obtain flocculation decoloration dyeing waste water bacteria cellulose based composites.
2. a kind of preparation side of flocculation decoloration dyeing waste water bacteria cellulose based composites according to claim 1 Method, it is characterised in that:Described bacteria culture is one in gluconobacter sp (ATCC 49306), gluconobacter sp (CGMCC 1671) Kind.
3. a kind of preparation side of flocculation decoloration dyeing waste water bacteria cellulose based composites according to claim 1 Method, it is characterised in that:The formula of described liquid fermentation medium is:30-40g/L glucose, 30-40g/L fructose, 2.5- 3.5g/L dusty yeasts, 4.5-5.5g/L tryptones, 0.8-1.2g/L sodium citrates, pH 4-6, through 110 DEG C of high temperature and high pressure steams Sterilize 30min.
4. a kind of preparation side of flocculation decoloration dyeing waste water bacteria cellulose based composites according to claim 1 Method, it is characterised in that:Described porous adsorbing material is one kind in activated carbon, diatomite, atlapulgite.
CN201710220197.3A 2017-04-06 2017-04-06 A kind of preparation method of flocculation decoloration dyeing waste water bacteria cellulose based composites Pending CN107164425A (en)

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CN109115848A (en) * 2018-07-17 2019-01-01 浙江理工大学 A kind of determination sensor preparation method of microorganism BOD
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Application publication date: 20170915