CN106519285A - Preparation method for three-dimensional network structure flocculation material structured by bacterial cellulose - Google Patents
Preparation method for three-dimensional network structure flocculation material structured by bacterial cellulose Download PDFInfo
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- CN106519285A CN106519285A CN201610843285.4A CN201610843285A CN106519285A CN 106519285 A CN106519285 A CN 106519285A CN 201610843285 A CN201610843285 A CN 201610843285A CN 106519285 A CN106519285 A CN 106519285A
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- bacterial cellulose
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/28—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
-
- 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
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B15/00—Preparation of other cellulose derivatives or modified cellulose, e.g. complexes
- C08B15/02—Oxycellulose; Hydrocellulose; Cellulosehydrate, e.g. microcrystalline cellulose
- C08B15/04—Carboxycellulose, e.g. prepared by oxidation with nitrogen dioxide
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/11—Turbidity
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/04—Oxycellulose; Hydrocellulose
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
- Materials Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Water Supply & Treatment (AREA)
- Environmental & Geological Engineering (AREA)
- Hydrology & Water Resources (AREA)
- Biochemistry (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
Abstract
The invention discloses a preparation method for a three-dimensional network structure flocculation material structured by bacterial cellulose. The preparation method comprises the steps that a bacterial cellulose material is dissolved and is modified after sodium periodate and ethylene glycol are added, and carboxyl cellulose is generated; then the three-dimensional network structure flocculation material is obtained after processing and drying; and then the three-dimensional network structure flocculation material is added into waste water to conduct a flocculation application experiment. The preparation method has the advantages that operation is easy, material sources are extensive and cost is low, and the application range is wide. According to the preparation method, the bacterial cellulose is used as a raw material of the flocculation material, so that the bio-degradable material is fully utilized and secondary pollution to the environment is reduced; and meanwhile, material-dependence on oil resources is reduced greatly. The prepared three-dimensional network structure flocculation material can be applied to waste water treatment such as industrial waste water and domestic waste water treatment, and has important economy and social environment benefits.
Description
Technical field
The invention belongs to field of environment engineering technology, especially belongs to cellulose flocculant preparation method field, especially
It is related to a kind of preparation method of the tridimensional network flocculation material that Bacterial cellulose builds.
Background technology
At present, the method for processing waste water includes physical-chemical process and biochemical process.Wherein physical-chemical process mainly removes useless
Float, colloidal particle, color and toxic compounds in water, mainly has floatation and Coagulation Method etc..Coagulation Method is to pre- mistake
Chemicals are added to make organic impuritiess that coagulation to occur in the waste water of filter, the method is simple to operate, low cost, and treatment effeciency is high.
According to different sources and property, flocculant mainly includes mineral-type, organic synthesiss class, natural organic high-molecular class
And microbiology class.Inorganic flocculating agent mainly has iron salt class and an aluminium salt class, and its usage amount is larger and with certain corrosivity, to ring
Border and human health are adversely affected；And organic polymer coargulator consumption is few, and flocculation rate is very fast, and flocculation molecule has
Various hydrophilic radicals and structure, flocculating effect are preferable.But organic synthesiss high polymer coagulant (such as polyacrylamide etc.) itself
Or its hydrolysis, catabolite it is poisonous, due to the enhancing of the environmentally safe consciousness of the mankind, its application enjoy restriction.By contrast, certain
A little natural organic matter high polymer coagulant biodegradables, environmentally safe, and containing hydrophilic groups such as more-COOH,
Flocculating property is excellent, and can be introduced more active groups and be reached by chemical modification strengthens the purpose of flocculating property.Microorganism
Flocculant is the Organic substances such as the glycoprotein, mucopolysaccharide and the nucleic acid that are produced by microorganism, and its flocculating effect is excellent, there is no secondary dirt
Dye, easy to use, but production cost is higher, and not easy to maintain.With mankind's environmental protection and the enhancing of safety consciousness, flocculant is at place
The aspects such as reason effect, Environmental Safety require more and more higher.Therefore, find a kind of the natural of efficient, economic and practical, green non-pollution
High polymer coagulant has important realistic meaning.
In flocculant preparation field, Chinese patent (CN 201610462430.4) " a kind of sewage flocculant and its preparation side
Sodium silicate is proportionally mixed by method " with magnesium chloride, is subsequently adding ethanol and is stirred；By polyacrylamide, titanium tetrachloride, silicon
Diatomaceous earth and aluminum sulfate co-grinding are powdered, add water mix homogeneously；By the product mixing for obtaining, while being continuously added hydrochloric acid
Stir.The flocculant proportioning science of the present invention, prepares simple, easy to use, the organic contamination that effectively can be gone in eliminating water
Thing and float, so as to lift water treatment capacity, improve the quality for processing water.Chinese patent (CN 201610406101.8) " one
Plant and prepare flocculant of pure water and preparation method thereof " a kind of flocculant for preparing pure water is provided, by weight portion
Raw material is made：Ferrous sulfate 40-60 parts, ferric ammonium sulfate 0.6-1 parts, TMS mesylate 0.2-0.4 parts, 2- ammonia
Base -1,3-PD 3-5 parts etc., flocculating effect of the present invention is good and easy to use.Chinese patent (CN 201610390665.7)
" a kind of preparation method and applications of low temperature resistant glycan microbial flocculant " are by Klebsiella oxytoca GS-4-08
Strain is used for the synchronization process of sucrose waste water and nitrile waste water；The waste water for obtaining after using process carries out the collection steps such as precipitate with ethanol
Extracellular polymeric secreted by bacterial strain is microbial flocculant.United States Patent (USP) (US9403704) " Water treatment
Method and water treatment flocculant " provide a kind of alkali of use flocculant process containing phenolic resin
Property solution reduce the method for treating water of secondary pollution, including addition flocculant and membrane separation.United States Patent (USP)
(US7666916)“Flocculant,manufacturing method therefor,and flocculation method
Using the flocculant " provide one kind can easy, safety, quickly process waterworks, sewage treatment plant, industry etc.
The preparation method of the flocculant of waste water, flocculant are obtained by colloidal silica solution Jing dilution gelations, are then tied with float gel
Conjunction carries out flocculation treatment.At present, yet there are no Bacterial cellulose as raw material, carboxycellulose is generated by chemical modification and is entered
The related process technologies of one-step synthesis tridimensional network flocculation material occur.
The content of the invention
For overcoming the deficiencies in the prior art, the present invention to provide a kind of simple to operate, applied range, do not result in secondary dirt
Dye, and reduce production cost Bacterial cellulose build tridimensional network flocculation material preparation method.
The technical solution adopted for the present invention to solve the technical problems is：The three-dimensional netted knot that a kind of Bacterial cellulose builds
The preparation method of structure flocculation material, it is characterised in that comprise the following steps：
1) bacteria cellulose material is added in sodium hydroxide and carbamide mixed solution, after being sufficiently stirred for, freezes 60-
80min, taking-up obtain bacterial cellulose solution；
2) by step 1) in the bacterial cellulose solution that obtains at 30-40 DEG C, under dark conditions, stirring adds periodic acid
After sodium oxidation 90-110min, glycol reaction 30-90min is added, remaining sodium metaperiodate is removed；Remove shading device to exist
It is stirred for reacting 6-8h under room temperature, obtains carboxycellulose solution；
3) by step 2) in the carboxycellulose solution that obtains of reaction carry out centrifugal treating, wash to neutrality, lyophilization
The tridimensional network flocculation material of Bacterial cellulose structure is obtained afterwards.
Preferably, the step 1) in sodium hydroxide and carbamide mixed solution with the mass ratio of bacteria cellulose material be
10-20:1。
Preferably, the step 1) mass fraction point of sodium hydroxide and carbamide in sodium hydroxide and carbamide mixed solution
Wei not 8wt% and 10wt%.
Preferably, the step 2) mass ratio of meso-periodic acid sodium and bacteria cellulose material is 0.1-0.2:1.
Preferably, the step 2) in the mass ratio of ethylene glycol and bacteria cellulose material be 1-3:1.
Preferably, the step 1) in be placed on -10 DEG C under the conditions of freezed.
Preferably, Bacterial cellulose source strain is the one kind in sarcina, edaphic bacilluss or root nodule bacteria.
The tridimensional network flocculation material that the present invention is provided, is to dissolve bacteria cellulose material, adds sodium metaperiodate
Be modified with ethylene glycol, generate carboxycellulose, then tridimensional network flocculation material is obtained after processing and being dried, then
Flocculation application is carried out in putting into waste water.The preparation method is easy to operate, material source extensive and low cost, applied range
It is wealthy.The present invention makes full use of biodegradable natural material, reduces environment using Bacterial cellulose as flocculation material raw material
Secondary pollution, while substantially reduce the raw material to petroleum resources rely on.The tridimensional network flocculation material of preparation is applied to work
The wastewater treatment such as industry and life, with important economy and social environment benefit.
The invention has the beneficial effects as follows：Petroleum resources will not be excessively relied on, reduce production cost, simplify operation side
Method, expands range of application, and flocculation material is biodegradable to reduce secondary pollution, the tridimensional network flocculation material of preparation
Suitable for the wastewater treatment such as industry and life, with important economy and social meaning.
Description of the drawings
Fig. 1 is that the tridimensional network flocculation material that Bacterial cellulose prepared by embodiment 1 builds is former with Bacterial cellulose
The infrared spectrum of material.
Fig. 2 is applied to Kaolin for the tridimensional network flocculation material that Bacterial cellulose prepared by embodiment 1 builds and gives up
Before and after water process and the effect photo that processes of contrast traditional flocculant polyacrylamide.
Specific embodiment
In order that those skilled in the art are better understood from the present invention program, below in conjunction with the embodiment of the present invention
Accompanying drawing, carries out clear, complete description to the technical scheme in inventive embodiments, it is clear that described embodiment is only this
A part of embodiment of invention, rather than the embodiment of whole.Based on the embodiment in the present invention, those of ordinary skill in the art
The every other embodiment obtained under the premise of creative work is not made, should all belong to the scope of protection of the invention.
Embodiment 1:
1) bacteria cellulose material that sarcina produces is pressed into sodium hydroxide and carbamide mixed solution and Bacterial cellulose
Material 15:During 1 mass ratio adds 8wt% sodium hydroxide and 10wt% carbamide mixed solutions, -10 DEG C of bars after being sufficiently stirred for, are placed
80min is freezed under part, and taking-up obtains bacterial cellulose solution；
2) by step 1) bacterial cellulose solution that obtains at 35 DEG C, under dark conditions, by sodium metaperiodate and cellulose
Material 0.2:After 1 mass ratio stirring adds sodium periodate oxidation 110min, then by ethylene glycol and bacteria cellulose material 2:1
Mass ratio adds glycol reaction 60min, removes remaining sodium metaperiodate；Remove shading device and be stirred for reaction at room temperature
6h, obtains carboxycellulose solution；
3) by step 2) in the carboxycellulose solution that obtains of reaction carry out centrifugal treating, wash to neutrality, lyophilization
Tridimensional network flocculation material (a) of Bacterial cellulose structure is obtained afterwards.
Embodiment 2:
1) bacteria cellulose material that root nodule bacteria produce is pressed into sodium hydroxide and carbamide mixed solution and bacterial fibers material
Material 20:During 1 mass ratio adds 8wt% sodium hydroxide and 10wt% carbamide mixed solutions, -10 DEG C of conditions after being sufficiently stirred for, are placed
Lower freezing 70min, taking-up obtain bacterial cellulose solution；
2) by step 1) bacterial cellulose solution that obtains at 40 DEG C, under dark conditions, by sodium metaperiodate and cellulose
Material 0.1:After 1 mass ratio stirring adds sodium periodate oxidation 90min, then by ethylene glycol and bacteria cellulose material 1:1
Mass ratio adds glycol reaction 30min, removes remaining sodium metaperiodate；Remove shading device and be stirred for reaction at room temperature
7h, obtains carboxycellulose solution；
3) by step 2) in the carboxycellulose solution that obtains of reaction carry out centrifugal treating, wash to neutrality, lyophilization
Tridimensional network flocculation material (b) of Bacterial cellulose structure is obtained afterwards.
Embodiment 3:
1) bacteria cellulose material that sarcina produces is pressed into sodium hydroxide and carbamide mixed solution and Bacterial cellulose
Material 18:During 1 mass ratio adds 8wt% sodium hydroxide and 10wt% carbamide mixed solutions, -10 DEG C of bars after being sufficiently stirred for, are placed
65min is freezed under part, and taking-up obtains bacterial cellulose solution；
2) by step 1) bacterial cellulose solution that obtains is at 40 DEG C, under dark conditions, fine with antibacterial by sodium metaperiodate
Dimension cellulosic material 0.18:After 1 mass ratio stirring adds sodium periodate oxidation 105min, then by ethylene glycol and cellulosic material 1.5:
1 mass ratio adds glycol reaction 70min, removes remaining sodium metaperiodate；Remove shading device to be stirred at room temperature instead
7h is answered, carboxycellulose solution is obtained；
3) by step 2) in the carboxycellulose solution that obtains of reaction carry out centrifugal treating, wash to neutrality, lyophilization
Tridimensional network flocculation material (c) of Bacterial cellulose structure is obtained afterwards.
Embodiment 4:
1) bacteria cellulose material that edaphic bacilluss are produced is pressed into sodium hydroxide and carbamide mixed solution and Bacterial cellulose
Material 10:During 1 mass ratio adds 8wt% sodium hydroxide and 10wt% carbamide mixed solutions, -10 DEG C of bars after being sufficiently stirred for, are placed
60min is freezed under part, and taking-up obtains bacterial cellulose solution；
2) by step 1) bacterial cellulose solution that obtains at 30 DEG C, under dark conditions, by sodium metaperiodate and cellulose
Material 0.15:After 1 mass ratio stirring adds sodium periodate oxidation 100min, then by ethylene glycol and bacteria cellulose material 3:1
Mass ratio add glycol reaction 90min, remove remaining sodium metaperiodate；Remove shading device and be stirred for reaction at room temperature
8h, obtains carboxycellulose solution；
3) by step 2) in the carboxycellulose solution that obtains of reaction carry out centrifugal treating, wash to neutrality, lyophilization
Tridimensional network flocculation material (d) of Bacterial cellulose structure is obtained afterwards.
By the preparation of infrared spectrum measurement embodiment 1, embodiment 2, embodiment 3 and embodiment 4 by three kinds of different bacteriums
Tridimensional network flocculation material (a) of cellulose preparation, tridimensional network flocculation material (b), tridimensional network flocculation
The carboxyl-content change of material (c) and tridimensional network flocculation material (d).
Table 1 be embodiment 1, embodiment 2, embodiment 3 and embodiment 4 prepare tridimensional network flocculation material (a), three
Dimension network structure flocculation material (b), tridimensional network flocculation material (c) and tridimensional network flocculation material (d) process high
Ridge soil coagulating waste water effect.From the data in table 1, it can be seen that tridimensional network flocculation material is applied at the coagulation of Kaolin waste water
Reason, the turbidity removal rate of waste water illustrate 4 kinds of tridimensional network flocculation materials prepared by the process in 94.1-95.2%
There is good coagulating sedimentation effect to Kaolin waste water.
As shown in figure 1, the infrared spectrum of the tridimensional network flocculation material prepared from embodiment 1 can be seen,
3403cm-1It is the stretching vibration absworption peak of O-H, 1637cm-1For the absworption peak of C=O stretching vibrations, 1384cm-1It is flexible for C-O
Vibration absorption peak, characteristic peak of these absworption peaks for carboxyl.All there is carboxyl after before modified in sample, but pass through oxidation modification
Afterwards, the V in tridimensional network flocculation materialO-HAbsworption peak substantially weakens, the V in carboxylC-OAbsworption peak has strengthened, and this shows
After oxidation reaction, part of hydroxyl is oxidized to carboxyl, and the carboxyl-content in tridimensional network flocculation material increases, and has
Beneficial to flocculation sediment.As shown in Fig. 2 the tridimensional network flocculation material prepared from embodiment 1 is applied at Kaolin waste water
Before and after reason and the effect photo that processes of contrast traditional flocculant can be seen that, the three-dimensional that polyacrylamide and Bacterial cellulose build
Network structure flocculation material is equally matched using the flocculating effect of the use PROCESS FOR TREATMENT waste water after optimization, all with more excellent
Coagulation effect.Kaolin waste water raw water is muddy, and liquid is in pistac substantially, and supernatant after treatment becomes clarification thoroughly
It is bright, and colourity and turbidity have obvious reduction；Larger floc particle is formed after flocculation material absorption impurities in water, with supernatant
Liquid separates sedimentation, and coagulation effect is obvious.
Table 1
Above-mentioned specific embodiment is used for illustrating the present invention, rather than limits the invention, the present invention's
In spirit and scope of the claims, any modifications and changes made to the present invention both fall within the protection model of the present invention
Enclose.
Claims (7)
1. the preparation method of the tridimensional network flocculation material that a kind of Bacterial cellulose builds, it is characterised in that including following
Step：
1) bacteria cellulose material is added in sodium hydroxide and carbamide mixed solution, freezes 60-80min after being sufficiently stirred for, take
Go out to obtain bacterial cellulose solution；
2) by step 1) in the bacterial cellulose solution that obtains at 30-40 DEG C, under dark conditions, stirring adds sodium metaperiodate oxygen
After changing 90-110min, glycol reaction 30-90min is added, remove remaining sodium metaperiodate；Remove shading device in room temperature
Under be stirred for react 6-8h, obtain carboxycellulose solution；
3) by step 2) in the reaction carboxycellulose solution that obtains carry out centrifugal treating, wash to neutrality, after lyophilization
To the tridimensional network flocculation material that Bacterial cellulose builds.
2. the preparation method of the tridimensional network flocculation material that Bacterial cellulose according to claim 1 builds, which is special
Levy and be：The step 1) in sodium hydroxide and carbamide mixed solution be 10-20 with the mass ratio of bacteria cellulose material:1.
3. the preparation method of the tridimensional network flocculation material that Bacterial cellulose according to claim 1 builds, which is special
Levy and be：The step 1) mass fraction of sodium hydroxide and carbamide is respectively 8wt% in sodium hydroxide and carbamide mixed solution
And 10wt%.
4. the preparation method of the tridimensional network flocculation material that Bacterial cellulose according to claim 1 builds, which is special
Levy and be：The step 2) mass ratio of meso-periodic acid sodium and bacteria cellulose material is 0.1-0.2:1.
5. the preparation method of the tridimensional network flocculation material that Bacterial cellulose according to claim 1 builds, which is special
Levy and be：The step 2) in the mass ratio of ethylene glycol and bacteria cellulose material be 1-3:1.
6. the preparation method of the tridimensional network flocculation material that Bacterial cellulose according to claim 1 builds, which is special
Levy and be：The step 1) in be placed on -10 DEG C under the conditions of freezed.
7. the preparation method of the tridimensional network flocculation material that Bacterial cellulose according to claim 1 builds, which is special
Levy and be：Bacterial cellulose source strain is the one kind in sarcina, edaphic bacilluss or root nodule bacteria.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107033919A (en) * | 2017-05-14 | 2017-08-11 | 吴刚 | A kind of preparation method of sand-consolidating agent |
| CN110003499A (en) * | 2018-10-08 | 2019-07-12 | 天津科技大学 | A kind of anti-bacterial hydrogel and preparation method thereof |
| CN114835312A (en) * | 2022-04-29 | 2022-08-02 | 杭州珩钧环境工程有限公司 | Resourceful treatment method of liquid dye wastewater |
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|---|---|---|---|---|
| CN102924613A (en) * | 2012-11-01 | 2013-02-13 | 海南大学 | Preparation method of dialdehyde bacterial cellulose |
| CN102964625A (en) * | 2012-11-27 | 2013-03-13 | 海南大学 | Method for preparing hydrophobic block cellulose aerogel thermal insulation material |
| CN103980367A (en) * | 2014-05-19 | 2014-08-13 | 浙江理工大学 | Method for preparing carboxyl cellulose flocculant |
-
2016
- 2016-09-23 CN CN201610843285.4A patent/CN106519285A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102924613A (en) * | 2012-11-01 | 2013-02-13 | 海南大学 | Preparation method of dialdehyde bacterial cellulose |
| CN102964625A (en) * | 2012-11-27 | 2013-03-13 | 海南大学 | Method for preparing hydrophobic block cellulose aerogel thermal insulation material |
| CN103980367A (en) * | 2014-05-19 | 2014-08-13 | 浙江理工大学 | Method for preparing carboxyl cellulose flocculant |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107033919A (en) * | 2017-05-14 | 2017-08-11 | 吴刚 | A kind of preparation method of sand-consolidating agent |
| CN110003499A (en) * | 2018-10-08 | 2019-07-12 | 天津科技大学 | A kind of anti-bacterial hydrogel and preparation method thereof |
| CN114835312A (en) * | 2022-04-29 | 2022-08-02 | 杭州珩钧环境工程有限公司 | Resourceful treatment method of liquid dye wastewater |
| CN114835312B (en) * | 2022-04-29 | 2023-04-18 | 杭州珩钧环境工程有限公司 | Resourceful treatment method of liquid dye wastewater |
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