CN106587296A - Bamboo pulp cellulose based flocculation decolorization composite functional material and preparation method thereof - Google Patents
Bamboo pulp cellulose based flocculation decolorization composite functional material and preparation method thereof Download PDFInfo
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- CN106587296A CN106587296A CN201611061275.1A CN201611061275A CN106587296A CN 106587296 A CN106587296 A CN 106587296A CN 201611061275 A CN201611061275 A CN 201611061275A CN 106587296 A CN106587296 A CN 106587296A
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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
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G81/00—Macromolecular compounds obtained by interreacting polymers in the absence of monomers, e.g. block polymers
- C08G81/02—Macromolecular compounds obtained by interreacting polymers in the absence of monomers, e.g. block polymers at least one of the polymers being obtained by reactions involving only carbon-to-carbon unsaturated bonds
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- General Chemical & Material Sciences (AREA)
- Polymers & Plastics (AREA)
- Medicinal Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
Abstract
The invention discloses a bamboo pulp cellulose based flocculation decolorization composite functional material and a preparation method thereof. The method mainly includes the steps of cutting a bamboo pulp board, washing the bamboo pulp board with water, drying the bamboo pulp board, crushing the bamboo pulp board into pulverized cellulose, dissolving the cellulose powder with sodium hydroxide and a urea frozen solution, adding an initiator, allowing the cellulose to be grafted and polymerized with polyacrylamide, adding activated carbon, and mixing the mixture fully to prepare the flocculation decolorization composite functional material. By adding the activated carbon in the flocculation decolorization composite functional material preparation process, a good flocculation effect is ensured, at the same time, the decolorization ability of the material is improved, the composite function that the decolorization effect and the flocculation effect is achieved at the same time is enhanced, the processes with flocculation first and decolorization second in a factory are partially simplified, the effect that solid suspended substances and soluble pollutants are removed by one step is achieved, the processing cost is reduced, the economic efficiency is improved, at the same time, the application field of bamboo fibers is expanded, the added value of a product is improved, and the application range of the flocculation decolorization product is expanded.
Description
Technical field
The invention belongs to technical field of polymer materials, the compound work(of more particularly to a kind of bamboo pulp fiber element base flocculation decoloration
Energy material and preparation method thereof.
Background technology
Flocculation technique is to be used to both at home and abroad improve a kind of not only economic but also water process skill of simplicity of waste water treatment efficiency at present
Art, has been widely used in the fields such as feedwater and drinking water treatment, Industrial Wastewater Treatment and food fermentation industry.Flocculant exists
With occupying an important position in solid-liquid separation of the water with wastewater treatment and production process, the selection of flocculant with use direct relation
The quality of flocculating effect.In recent years, as people are required more environmentally friendly and sustainable development, natural macromolecule flocculating agent
Receive more and more attention.
But at present, in organic polymer flocculation decoloration field, flocculant can not take into account flocculation and two kinds of effects of decolourizing, and
There are problems that to secondary environmental pollution and sludge degradation.In the preparation field of flocculation decoloration material, Chinese patent (CN
During 101307119B) " a kind of preparation method of amphiprotic chitosan flocculant " dissolves chitosan in acrylic acid aqueous solution,
The mass percentage concentration of acrylic acid solution is 0.1-1%, is configured to the solution of the mass percentage concentration for 1-3% of shitosan,
Ammonium ceric nitrate initiator is added in the solution for obtaining, acrylamide is added, acrylamide is 1 with the mass ratio of shitosan:1-
8:1,2-4 hours are reacted at 45-65 DEG C, amphiprotic chitosan flocculant is prepared, and its flocculating property is characterized；
Chinese patent (CN105504161A) " a kind of Anionic High-molecular Flocculant and preparation method thereof " by deionized water, chelating
Agent, chain-transferring agent and acrylamide sodium benzoate is added in reactor, and adjusts pH value to add ethyl acrylate after 5-9
Sour sodium, leads to N2After add initiator, then cause polymerization, obtain clear viscous copolymer, be cooled to after room temperature washing, be dried,
Anionic High-molecular Flocculant is obtained, for processing oil field waste；A kind of Chinese patent (CN101143743B) " cationic
The preparation method of high polymer coagulant " is with acrylamide, dimethylaminoethyl methacrylate, quaternizing agent, deionized water
For raw material, using different initiator systems, reactant concentration is strictly controlled, at ambient pressure aqueous solution polymerization, and it is flocculated
Performance is characterized；United States Patent (USP) (US 20140158633A1) " Particle suspensions of
Flocculating polymer powders and powder flocculant polymer blends " are with polycyclic oxygen second
Alkane and polyacrylamide are obtained mixture of powders flocculant, and mixture of powders flocculant is used for purification of waste water and fiber is dehydrated；It is beautiful
State's patent (US20150076070A1) " Advanced treatment method for biochemical tail water
Of coking wastewater " using bodied ferric sulfate (PFS) and polyacrylamide (PAM) as flocculant, at biology
The pretreatment of reason waste water, and can extensively be answered as being used to regenerate the desorbing reagent of nano composite material using sodium hydroxide solution
For the advanced process and comprehensive utilization of coking chemical waste water.Up to now, yet there are no using bamboo pulp fiber element and polyacrylamide
As raw material, while adding activated carbon, occur to the related process technologies for preparing flocculation decoloration composite functional material.
Bamboo pulp fiber element base flocculation decoloration composite functional material adopts natural bamboo cellulose for framework material, grafting poly- third
Acrylamide, adds activated carbon, processes slightly soluble and soluble pollutants in waste water, and flocculation sediment reduces colourity, takes into account flocculation and takes off
Color performance, can reach float in waste water and removes with while dissolubility pollutant, it is adaptable to dyeing waste water and municipal wastewater etc.
Sewage disposal, the important realistic meaning with environment and economy.
The content of the invention
In order to overcome the deficiencies in the prior art, the present invention to provide a kind of bamboo pulp fiber for strengthening and decolourizing with flocculation composite effect
The preparation method of plain base flocculation decoloration composite functional material.
For achieving the above object, the technical scheme is that and adopt following steps：
1) bamboo pulp pulpboard is cut into into bulk, smashed with microphyte pulverizer, Jing 220-320 mesh sieve net filtrations obtain grain
Footpath is the bamboo pulp fiber element powder of 0.042-0.068mm；
2) weigh step 1) in obtain bamboo pulp fiber element powder, be dissolved in the sodium hydroxide/carbamide of 5 DEG C of precooling 90min
In mixed solution, magnetic agitation 5-15min, diaphragm seal is put in -10--15 DEG C of refrigerator and freezes 50-80min, is freezed
Cellulose solution；
3) by step 2) the freezing cellulose solution that obtains under magnetic agitation effect, is passed through nitrogen 60min, and 35-45 DEG C
Add initiator to cause 30-60min, add polyacrylamide to carry out glycerol polymerization, polyacrylamide and bamboo pulp fiber element powder
Mass ratio be 1.5-2.5:1, it is placed in 35-45 DEG C of temperature and reacts 90-150min, obtain sticky polymers liquid；
4) in step 3) activated carbon, magnetic agitation 15-60min, reaction system are added in the sticky polymers liquid that obtains
35～45 DEG C of temperature are kept, bamboo pulp fiber element base flocculation decoloration composite functional material is obtained.
Further, the step 2) in sodium hydroxide/carbamide mixed solution, the wherein quality of sodium hydroxide and carbamide point
Number is respectively 5wt% and 14wt%, and sodium hydroxide/carbamide mixed solution is 25-35 with the mass ratio of bamboo pulp fiber element powder:1.
Further, the step 3) in initiator to be that oxidation-reduction that potassium peroxydisulfate/sodium sulfite is constituted is compound draw
Agent is sent out, oxidation-reduction composite initiator is 0.1-0.3 with the mass ratio of bamboo pulp fiber element powder:1, oxidation-reduction is compound to be caused
Potassium peroxydisulfate and the mass ratio of sodium sulfite are 1 in agent:1.5-3.
Further, the step 4) in activated carbon mesh number be 10-200 mesh, the matter of activated carbon and bamboo pulp fiber element powder
Amount is than being 1-3:1.
Compared with background technology, the invention has the advantages that：
The recycling of the present invention bamboo resource of China's abundant, during prepare flocculation decoloration composite functional material
Cheap, wide material sources bamboo pulp fibers are introduced, as molecule basic framework, original macromolecular material is partly substituted.Add
Activated carbon is combined, and processes slightly soluble and soluble pollutants in waste water, while keeping good flocculation ability, strengthens its decolouring energy
Power, realizes the one-step removal of solid suspension and dissolubility pollutant, reduces wastewater treatment working section cost, it is adaptable to which printing and dyeing are useless
The process of water and municipal wastewater, with important environment and economic benefit.
Description of the drawings
Fig. 1 is the digital photograph of bamboo pulp fiber element base flocculation decoloration composite functional material product prepared by embodiment 1：A is
The sticky polymers liquid before activated carbon is added, b is to add the bamboo pulp fiber element base flocculation decoloration complex function after activated carbon
Material product.
Fig. 2 is that bamboo pulp fiber element base flocculation decoloration composite functional material product flocculation decoloration prepared by embodiment 1 processes mould
Intend the effect photo of dye solution：A is the simulation dye solution photo of flocculation decoloration before processing, and b is after flocculation decoloration process
Simulation dye solution photo.
Fig. 3 is that bamboo pulp fiber element base flocculation decoloration composite functional material product flocculation decoloration prepared by embodiment 1 processes real
The effect photo of border dyeing waste water：A is the actual dying photo of flocculation decoloration before processing, and b is after flocculation decoloration process
Actual dying photo.
Specific embodiment
With reference to specific embodiment, the invention will be further described.
Embodiment 1：
1) bamboo pulp pulpboard is cut into into bulk, smashed with microphyte pulverizer, the mesh sieve net filtrations of Jing 220, obtaining particle diameter is
The bamboo pulp fiber element powder of 0.068mm；
2) weigh step 1) in the bamboo pulp fiber element powder that obtains, be dissolved in 5% sodium hydroxide of 5 DEG C of precooling 90min/
In 14% carbamide mixed solution, 5% sodium hydroxide/14% carbamide mixed solution is 25 with the mass ratio of bamboo pulp fiber element powder:
1, magnetic agitation 5min, diaphragm seal is put in -15 DEG C of refrigerator and freezes 80min, obtains freezing cellulose solution；
3) by step 2) the freezing cellulose solution that obtains under magnetic agitation effect, is passed through nitrogen 60min, 45 DEG C of additions
Potassium peroxydisulfate/sodium sulfite composite initiator causes 30min, oxidation-reduction composite initiator and bamboo pulp fiber element powder
Mass ratio is 0.3:1, potassium peroxydisulfate and the mass ratio of sodium sulfite are 1 in oxidation-reduction composite initiator:1.5, add poly-
Acrylamide carries out glycerol polymerization, and polyacrylamide is 1.5 with the mass ratio of bamboo pulp fiber element powder:1, in being placed in 45 DEG C of temperature
Reaction 150min, obtains sticky polymers liquid；
4) in step 3) 200 mesh activated carbons, activated carbon and bamboo pulp fiber element powder are added in the sticky polymers liquid that obtains
The mass ratio at end is 1:1, magnetic agitation 15min, whole temperature of reaction system is kept for 45 DEG C, obtains bamboo pulp fiber element base flocculation de-
Color composite functional material (a).
Embodiment 2：
1) bamboo pulp pulpboard is cut into into bulk, smashed with microphyte pulverizer, the mesh sieve net filtrations of Jing 280, obtaining particle diameter is
The bamboo pulp fiber element powder of 0.056mm；
2) weigh step 1) in the bamboo pulp fiber element powder that obtains, be dissolved in 5% sodium hydroxide of 5 DEG C of precooling 90min/
In 14% carbamide mixed solution, 5% sodium hydroxide/14% carbamide mixed solution is 30 with the mass ratio of bamboo pulp fiber element powder:
1, magnetic agitation 10min, diaphragm seal is put in -13 DEG C of refrigerator and freezes 70min, obtains freezing cellulose solution；
3) by step 2) the freezing cellulose solution that obtains under magnetic agitation effect, is passed through nitrogen 60min, 40 DEG C of additions
Potassium peroxydisulfate/sodium sulfite composite initiator causes 40min, oxidation-reduction composite initiator and bamboo pulp fiber element powder
Mass ratio is 0.25:1, potassium peroxydisulfate and the mass ratio of sodium sulfite are 1 in oxidation-reduction composite initiator:2, add poly-
Acrylamide carries out glycerol polymerization, and polyacrylamide is 2 with the mass ratio of bamboo pulp fiber element powder:1, it is placed in 40 DEG C of temperature anti-
130min is answered, sticky polymers liquid is obtained；
4) in step 3) 50 mesh activated carbons, activated carbon and bamboo pulp fiber element powder are added in the sticky polymers liquid that obtains
Mass ratio be 2:1, magnetic agitation 20min, whole temperature of reaction system is kept for 40 DEG C, obtains bamboo pulp fiber element base flocculation decoloration
Composite functional material (b).
Embodiment 3
1) bamboo pulp pulpboard is cut into into bulk, smashed with microphyte pulverizer, the mesh sieve net filtrations of Jing 320, obtaining particle diameter is
The bamboo pulp fiber element powder of 0.042mm；
2) weigh step 1) in the bamboo pulp fiber element powder that obtains, be dissolved in 5% sodium hydroxide of 5 DEG C of precooling 90min/
In 14% carbamide mixed solution, 5% sodium hydroxide/14% carbamide mixed solution is 35 with the mass ratio of bamboo pulp fiber element powder:
1, magnetic agitation 15min, diaphragm seal is put in -10 DEG C of refrigerator and freezes 50min, obtains freezing cellulose solution；
3) by step 2) the freezing cellulose solution that obtains under magnetic agitation effect, is passed through nitrogen 60min, 35 DEG C of additions
Potassium peroxydisulfate/sodium sulfite composite initiator causes 60min, oxidation-reduction composite initiator and bamboo pulp fiber element powder
Mass ratio is 0.1:1, potassium peroxydisulfate and the mass ratio of sodium sulfite are 1 in oxidation-reduction composite initiator:3, add poly- third
Acrylamide carries out glycerol polymerization, and polyacrylamide is 2.5 with the mass ratio of bamboo pulp fiber element powder:1, it is placed in 35 DEG C of temperature anti-
90min is answered, sticky polymers liquid is obtained；
4) in step 3) 10 mesh activated carbons, activated carbon and bamboo pulp fiber element powder are added in the sticky polymers liquid that obtains
Mass ratio be 3:1, magnetic agitation 60min, whole temperature of reaction system is kept for 35 DEG C, obtains bamboo pulp fiber element base flocculation decoloration
Composite functional material (c).
The percent grafting of three kinds of bamboo pulp fibers element base flocculation decoloration composite functional material prepared by embodiment 1,2,3 is determined, together
When determine and be applied to turbidity removal rate, the chroma removal rate of actual dying.Table 1 is three kinds of bamboos prepared by embodiment 1,2,3
The percent grafting measurement result of pulp cellulose base flocculation decoloration composite functional material and it is applied to actual dying flocculation decoloration mistake
The turbidity removal rate of journey, chroma removal rate measurement result.
From data in table 1, the bamboo pulp fiber element base flocculation decoloration obtained using preparation method of the present invention is answered
Functional material (a), (b), (c) percent grafting are closed 34.6～47.2%, glycerol polymerization is ideal.It is applied to actual printing and dyeing
The flocculation decoloration of waste water is processed, color degree of dyeing waste water clearance 75.2～89.5%, turbidity removal rate 76.5～87.0%,
The bamboo pulp fiber element base flocculation decoloration composite functional material for illustrating present invention preparation has preferably flocculation to actual dying
Decolorizing effect.
Such as Fig. 1, the digital photograph of the cellulose base complex function flocculation decoloration material product prepared from embodiment 1 can
Go out, product design is sticky, be suitable to be diluted to desired concn with aqueous solution, being added in actual dying is carried out at flocculation decoloration
Reason；Such as Fig. 2 and Fig. 3, the bamboo pulp fiber element base flocculation decoloration composite functional material prepared from embodiment 1 is processed simulates dye solution
Flocculating effect is can be seen that with actual dying effect photo significantly, decolorizing effect is good, the effect taken into account of decolourizing and flocculate
Preferably.
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.One of ordinary skill in the art does not make all deformations directly derived under the premise of creative work or associate,
It is considered as the scope of the present invention.
Claims (4)
1. a kind of bamboo pulp fiber element base flocculation decoloration composite functional material and preparation method thereof, it is characterised in that including following step
Suddenly：
1) bamboo pulp pulpboard is cut into into bulk, smashed with microphyte pulverizer, Jing 220-320 mesh sieve net filtrations, obtaining particle diameter is
The bamboo pulp fiber element powder of 0.042-0.068mm；
2) weigh step 1) in the bamboo pulp fiber element powder that obtains, be dissolved in the sodium hydroxide of 5 DEG C of precooling 90min/carbamide mixing
In solution, magnetic agitation 5-15min, diaphragm seal is put in -10--15 DEG C of refrigerator and freezes 50-80min, obtains freezing fiber
Plain solution；
3) by step 2) the freezing cellulose solution that obtains under magnetic agitation effect, is passed through nitrogen 60min, 35-45 DEG C of addition
Initiator causes 30-60min, adds polyacrylamide to carry out the matter of glycerol polymerization, polyacrylamide and bamboo pulp fiber element powder
Amount is than being 1.5-2.5:1, it is placed in 35-45 DEG C of temperature and reacts 90-150min, obtain sticky polymers liquid；
4) in step 3) add activated carbon, magnetic agitation 15-60min, system to keep 35-45 in the sticky polymers liquid that obtains
DEG C temperature, obtains bamboo pulp fiber element base flocculation decoloration composite functional material.
2. a kind of cellulose base flocculation decoloration composite functional material according to claim 1 and preparation method thereof, its feature
It is：The step 2) in sodium hydroxide and carbamide mixed solution, the mass fraction of wherein sodium hydroxide and carbamide is respectively
5wt% and 14wt%, sodium hydroxide/carbamide mixed solution is 25-35 with the mass ratio of bamboo pulp fiber element powder:1.
3. bamboo pulp fiber element base flocculation decoloration composite functional material and preparation method thereof according to claim 1, its
It is characterised by：The step 3) in initiator be oxidation-reduction composite initiator that potassium peroxydisulfate/sodium sulfite is constituted, oxygen
The mass ratio for changing-reducing composite initiator with bamboo pulp fiber element powder is 0.1-0.3:1, mistake in oxidation-reduction composite initiator
Potassium sulfate is 1 with the mass ratio of sodium sulfite:1.5-3.
4. a kind of bamboo pulp fiber element base flocculation decoloration composite functional material according to claim 1 and preparation method thereof, its
It is characterised by：The step 4) in activated carbon mesh number be 10-200 mesh, the mass ratio of activated carbon and bamboo pulp fiber element powder is 1-
3:1。
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| CN201611061275.1A CN106587296A (en) | 2016-11-28 | 2016-11-28 | Bamboo pulp cellulose based flocculation decolorization composite functional material and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109126739A (en) * | 2018-08-21 | 2019-01-04 | 浙江理工大学 | It is a kind of for removing the preparation method of the Studies On Preparation And Properties of Cellulose-based Adsorbents of antimony ion in dyeing waste water |
| CN110117053A (en) * | 2019-04-15 | 2019-08-13 | 浙江理工大学 | A kind of preparation method of the environmentally friendly flocculation material based on regenerated paper pulp |
| CN114195235A (en) * | 2020-09-02 | 2022-03-18 | 上海昶法新材料有限公司 | Flocculating agent, raw material composition thereof, and preparation method and application thereof |
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| CN106006903A (en) * | 2016-05-27 | 2016-10-12 | 浙江理工大学 | Preparation method of bamboo-pulp cellulose and poly(N-vinylformamide) composite flocculating and decolorizing material |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109126739A (en) * | 2018-08-21 | 2019-01-04 | 浙江理工大学 | It is a kind of for removing the preparation method of the Studies On Preparation And Properties of Cellulose-based Adsorbents of antimony ion in dyeing waste water |
| CN110117053A (en) * | 2019-04-15 | 2019-08-13 | 浙江理工大学 | A kind of preparation method of the environmentally friendly flocculation material based on regenerated paper pulp |
| CN114195235A (en) * | 2020-09-02 | 2022-03-18 | 上海昶法新材料有限公司 | Flocculating agent, raw material composition thereof, and preparation method and application thereof |
| CN114195235B (en) * | 2020-09-02 | 2024-03-15 | 上海昶法新材料有限公司 | Flocculant, raw material composition thereof, and preparation method and application thereof |
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