CN106832987A - A kind of preparation method of cellulose silk gum degradable flocculation material - Google Patents
A kind of preparation method of cellulose silk gum degradable flocculation material Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L97/00—Compositions of lignin-containing materials
- C08L97/02—Lignocellulosic material, e.g. wood, straw or bagasse
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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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- 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
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
- C08J3/246—Intercrosslinking of at least two polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L89/00—Compositions of proteins; Compositions of derivatives thereof
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- C—CHEMISTRY; METALLURGY
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2389/00—Characterised by the use of proteins; Derivatives thereof
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- 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
- C08J2397/00—Characterised by the use of lignin-containing materials
- C08J2397/02—Lignocellulosic material, e.g. wood, straw or bagasse
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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
- C08J2489/00—Characterised by the use of proteins; Derivatives thereof
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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
- C08J2497/00—Characterised by the use of lignin-containing materials
- C08J2497/02—Lignocellulosic material, e.g. wood, straw or bagasse
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/06—Biodegradable
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
- C08L2205/16—Fibres; Fibrils
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- Separation Of Suspended Particles By Flocculating Agents (AREA)
Abstract
The invention discloses a kind of preparation method of cellulose silk gum degradable flocculation material.It is using bamboo cellulose and sericin, to be crosslinked by glutaraldehyde chemical modification using the main points of method, prepares that flocculating effect is excellent, the cellulose silk gum degradable flocculation material of biodegradable.The preparation method is simple to operate, excellent effect and flocculation material Product environment is pollution-free.Be incorporated into the raw material for preparing flocculation material for bamboo fiber element and sericin by the present invention, increased the raw material range for preparing flocculation material, reduces production cost, while increased flocculation material environment friendly in itself, has important practical significance.
Description
Technical field
The present invention relates to a kind of preparation method of flocculation material, more particularly to a kind of cellulose-silk gum degradable flocculation material
The preparation method of material, belongs to high-molecular organic material technical field.
Background technology
Flocculation is a highly important link in water process.Flocculant is in consolidating with water and wastewater treatment and production process
Liquid occupies an important position in separating, the quality for selecting with using direct relation flocculating effect of flocculant.From last century six
The seventies rise, organic polymer coargulator progressively replaces inorganic metal class flocculant, be widely used in chemical industry, metallurgy, coal,
The production fields such as weaving, papermaking, oil, environmental protection.As the research and development and people of high polymer coagulant are to more environmentally friendly
With the demand of sustainable chemistry technology, natural macromolecule flocculating agent is by society and scholars more and more concern.
At present, the natural resources species that can prepare natural macromolecule flocculating agent is enriched, such as starch, cellulose and its derivative
Thing, shitosan, alginic acid etc., or even some protein, plant colloid etc., these natural macromolecular materials assign natural polymer
Flocculant is nontoxic, biodegradable excellent properties so that the exploitation of such flocculant is widely closed with research by academia
Note.
The present invention proposes a kind of preparation technology of cellulose-silk gum degradable flocculation material.Using cheap, source
Extensive bamboo pulp and sericin are raw material, and scattered fiber fines are turned into after mashing, and through glutaraldehyde cross-linking after dissolving, grafting is altogether
Poly- sericin, obtains a kind of cellulose-silk gum degradable flocculation material.The preparation technology advantage is mainly manifested in：One is system
For a kind of environmentally friendly, fully biodegradable novel flocculant, degradation cycle is shortened；Two ensure that it is good
Flocculating effect, and the use of bamboo pulp fiber element and sericin is raw material, production cost can be not only reduced, increase economic efficiency,
The application field of bamboo pulp fiber can be also expanded, added value of product is improved；Sericin is the waste eggshell for extracting fibroin process simultaneously
In vain, it is cheap, it is capable of achieving the recycling of discarded object.
In organic polymer flocculation material preparation field, " a kind of vegetable source natural is high for Chinese patent (CN106044984A)
The preparation method of molecular flocculant " extracts Aloe Vera Gel with aloe as raw material through base exchange method auxiliary alcohol precipitation, then by Aloe Vera Gel
It is first modified through soya-bean milk and microorganism in konjak starch compounding, then microwave modification is etherified, suction filtration alcohol is obtained natural polymer wadding after washing
Solidifying agent, and its flocculating property is characterized；A kind of Chinese patent (CN105001381A) " paper mill sludge base Amphiphatic high polymer
The preparation method of flocculant " is separated with paper mill sludge raw material and dimethyl diallyl ammonium chloride as raw material from paper mill sludge
Go out supernatant, adjust supernatant pH, cooling adds anhydrous sodium sulfite, adds initiator and dimethyl diallyl chlorination
Ammonium, agitated reaction, mixture adds acetone stirring, separates out product, through vacuum filtration, drying, obtains final product both sexes high score
Sub- flocculant product；United States Patent (USP) (US 20120241377) " Water treatment method and water
Treatment flocculant " react prepared thermoplastic phenolic resin in the presence of acidic using phenol and formaldehyde
Prepare flocculation material.So far, yet there are no using bamboo pulp fiber element and sericin glycerol polymerization, to prepare degradable wadding
The related process technologies of gel material occur.
The invention provides a kind of preparation method of cellulose-silk gum degradable flocculation material, using bamboo cellulose and silk
Glue protein, is crosslinked by glutaraldehyde chemical modification, prepares that flocculating effect is excellent, and the cellulose-silk gum of biodegradable is complete
Degraded flocculation material.The preparation method is simple to operate, excellent effect and flocculation material Product environment is pollution-free.The present invention is by bamboo
Subbundle element and sericin are incorporated into the raw material for preparing flocculation material, increased the raw material range for preparing flocculation material, are dropped
Low production cost, while increased flocculation material environment friendly in itself, has important practical significance.
The content of the invention
In order to overcome traditional inorganic flocculating agent and Syn-Organic flocculants low, easily secondary in the efficiency using process
Pollution, it is not biodegradable the problems such as, non-pollution discharge is realized, while renewable, the degradable biological material of recycling
Material, by simple glutaraldehyde cross-linking, excellent effect, soft preparation process synthesize flocculating effect substantially, complete biodegradable, nothing
The degradable flocculation material of secondary pollution.It is an object of the invention to provide a kind of system of cellulose-silk gum degradable flocculation material
Preparation Method.
To achieve the above object, the technical scheme is that using following steps：
1) after by the cutting of bamboo pulpboard, washing, dried in convection oven, then smashed with microphyte pulverizer, through 80-
100 mesh sieve net filtrations, obtain bamboo pulp fiber element powder of the particle diameter between 150-200 μm；
2) by step 1) bamboo pulp fiber that obtains element powder weighs certain mass and is dissolved in the water of certain volume and is added to
In beaker, immersion 12-36h is stirred in sealing under magnetic stirring apparatus effect, is obtained through swelling cellulose solution；
3) silk gum that certain mass molecular weight is 2000-100000 is weighed, is fully dissolved in the water for adding 5-15mL,
Be added to step 2) obtain through swelling cellulose solution in, and adjust its pH to 4-7, obtain cellulose-silk gum mixture
Solution；
4) to step 3) glutaraldehyde solution of certain mass is added in cellulose-silk gum mixture solution for obtaining, it is placed in
3-12h, product dialysis 7d, freeze-dried, as cellulose-silk gum degradable flocculation are reacted in 30-45 DEG C of thermostat
Material.
Described water is 90-120 with bamboo pulpboard mass ratio:1；Silk gum is 0.5-2 with bamboo pulpboard mass ratio:1；Penta 2
Aldehyde is the glutaraldehyde solution that content is 25%, and glutaraldehyde solution is 0.5-2 with bamboo pulpboard mass ratio:1.
Described bamboo pulpboard is the one kind in cizu pulpboard, fishscale bamboo pulpboard, bamboo pulpboard and square bamboo pulp plate.
Compared with background technology, the invention has the advantages that：
The present invention uses the Protein filament discarded during bamboo pulp fiber element and extraction fibroin while flocculating effect is good
Glue is raw material, overcome traditional inorganic flocculating agent and Syn-Organic flocculants the efficiency using process it is low, cause secondary
Pollution, it is not biodegradable the problems such as, non-pollution discharge is realized, while recycling is renewable, degradable biological material
Material, by simple glutaraldehyde cross-linking, excellent effect, soft preparation process synthesize flocculating effect substantially, complete biodegradable,
The degradable flocculation material of non-secondary pollution, increased flocculation material environment friendly in itself, have important practical significance.
Brief description of the drawings
Fig. 1 is to contrasting before and after the cellulose-silk gum degradable flocculation material treatment industrial wastewater prepared by embodiment 1
Piece：(a1) undressed industrial wastewater digital photograph, (a2) through the Industry Waste of cellulose-silk gum degradable flocculation material treatment
Water digital photograph.
Specific embodiment
With reference to specific embodiment, the invention will be further described.
Embodiment 1:
1) after by the cutting of cizu pulpboard, washing, dried in convection oven, then smashed with microphyte pulverizer, through 80-
100 mesh sieve net filtrations, obtain cizu cellulose powder of the particle diameter between 150-200 μm；
2) by step 1) the cizu cellulose powder that obtains weighs 1g and is dissolved in 90mL water and is added in beaker, seal,
Immersion 24h is stirred under magnetic stirring apparatus effect, is obtained through swelling cellulose solution；
3) silk gum that 1.5g molecular weight is 8000 is weighed, is fully dissolved in the water for adding 10mL, be added to step 2)
Obtain through swelling cellulose solution in, and adjust its pH to 4, obtain cellulose-silk gum mixture solution；
4) to step 3) glutaraldehyde that adds 1.5g contents to be 25% in cellulose-silk gum mixture solution for obtaining is molten
Liquid, is placed in and 9h is reacted in 35 DEG C of thermostats, product dialysis 7d, freeze-dried, as cellulose-silk gum degradable flocculation
Material (a).
Embodiment 2:
1) after by the cutting of fishscale bamboo pulpboard, washing, dried in convection oven, then smashed with microphyte pulverizer, through 80-
100 mesh sieve net filtrations, obtain fishscale bamboo cellulose powder of the particle diameter between 150-200 μm；
2) by step 1) in the fishscale bamboo cellulose powder that obtains weigh 1g and be dissolved in 100mL water and be added in beaker, seal
Mouthful, immersion 36h is stirred under magnetic stirring apparatus effect, obtain through swelling cellulose solution；
3) silk gum that 0.5g molecular weight is 2000 is weighed, is fully dissolved in the water for adding 5mL, be added to step 2)
To through swelling cellulose solution in, and adjust its pH to 5, obtain cellulose-silk gum mixture solution；
4) to step 3) glutaraldehyde that adds 0.5g contents to be 25% in cellulose-silk gum mixture solution for obtaining is molten
Liquid, is placed in and 3h is reacted in 45 DEG C of thermostats, product dialysis 7d, freeze-dried, as cellulose-silk gum degradable flocculation
Material (b).
Embodiment 3:
1) after by the cutting of bamboo pulpboard, washing, dried in convection oven, then smashed with microphyte pulverizer, through 80-
100 mesh sieve net filtrations, obtain bamboo cellulose powder of the particle diameter between 150-200 μm；
2) by step 1) in the bamboo cellulose powder that obtains weigh 1g and be dissolved in 110mL water and be added in beaker, seal
Mouthful, immersion 24h is stirred under magnetic stirring apparatus effect, obtain through swelling cellulose solution；
3) silk gum that 1g molecular weight is 20000 is weighed, is fully dissolved in the water for adding 10mL, be added to step 2)
To through swelling cellulose solution in, and adjust its pH to 6, obtain cellulose-silk gum mixture solution；
4) to step 3) glutaraldehyde solution that 1g contents are 25% is added in cellulose-silk gum mixture solution for obtaining,
It is placed in and 6h is reacted in 40 DEG C of thermostats, product dialysis 7d is freeze-dried, as cellulose-silk gum degradable flocculation material
Material (c).
Embodiment 4:
1) after by the cutting of square bamboo pulp plate, washing, dried in convection oven, then smashed with microphyte pulverizer, through 80-
100 mesh sieve net filtrations, obtain square bamboo cellulose powder of the particle diameter between 150-200 μm；
2) by step 1) in the square bamboo cellulose powder that obtains weigh 1g and be dissolved in 120mL water and be added in beaker, seal
Mouthful, immersion 12h is stirred under magnetic stirring apparatus effect, obtain through swelling cellulose solution；
3) silk gum that 2g molecular weight is 100000 is weighed, is fully dissolved in the water for adding 15mL, be added to step 2)
Obtain through swelling cellulose solution in, and adjust its pH to 7, obtain cellulose-silk gum mixture solution；
4) to step 3) glutaraldehyde solution that 2g contents are 25% is added in cellulose-silk gum mixture solution for obtaining,
It is placed in and 12h is reacted in 30 DEG C of thermostats, product dialysis 7d is freeze-dried, as cellulose-silk gum degradable flocculation material
Material (d).
Determine embodiment 1,2,3,4 and prepare 4 kinds of celluloses-yield of silk gum degradable flocculation material, zeta current potentials
And turbidity removal rate.Table 1 is cellulose-silk gum degradable flocculation material yield, the zeta current potentials prepared by embodiment 1,2,3,4
With the sign results of measuring of turbidity removal efficiency.From the data in table 1, it can be seen that the fiber obtained using preparation method of the present invention
Element-silk gum degradable flocculation material (a), cellulose-silk gum degradable flocculation material (b), cellulose-silk gum degradable flocculation material
Material (c), cellulose-silk gum degradable flocculation material (d) yield are more considerable in 43.81-62.49%；Zeta current potentials-
20.4--30.2mV, is anionic flocculation material；Turbidity removal rate is illustrated by offer technology of the present invention in 77.9-85.7%
The cellulose of preparation-silk gum degradable flocculation material has excellent flocculating property and turbidity of wastewater clearance higher.
Such as Fig. 1, the effect of the cellulose prepared using embodiment 1-silk gum degradable flocculation material (a) treatment industrial wastewater
Photo can be seen that the degradable flocculation material flocculation sediment effect of present invention preparation substantially, and the turbidity removal rate of waste water is higher.
Table 1
Listed above is only specific embodiment of the 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 can directly derive from present disclosure or associate, all should
It is considered protection scope of the present invention.
Claims (3)
1. the preparation method of a kind of cellulose-silk gum degradable flocculation material, it is characterised in that comprise the following steps：
1) after by the cutting of bamboo pulpboard, washing, dried in convection oven, then smashed with microphyte pulverizer, through 80-100 mesh
Screen filtration, obtains bamboo pulp fiber element powder of the particle diameter between 150-200 μm；
2) by step 1) bamboo pulp fiber that obtains element powder weighs certain mass and is dissolved in the water of certain volume and is added to beaker
In, immersion 12-36h is stirred in sealing under magnetic stirring apparatus effect, is obtained through swelling cellulose solution；
3) silk gum that certain mass molecular weight is 2000-100000 is weighed, is fully dissolved in the water for adding 5-15mL, added
To step 2) obtain through swelling cellulose solution in, and adjust its pH to 4-7, obtain cellulose-silk gum mixture solution；
4) to step 3) glutaraldehyde solution of certain mass is added in cellulose-silk gum mixture solution for obtaining, it is placed in 30-45
React 3-12h in DEG C thermostat, product dialysis 7d is freeze-dried, as cellulose-silk gum degradable flocculation material.
2. the preparation method of a kind of cellulose according to claim 1-silk gum degradable flocculation material, it is characterised in that：
Described water is 90-120 with bamboo pulpboard mass ratio:1；Silk gum is 0.5-2 with bamboo pulpboard mass ratio:1；Glutaraldehyde is content
It is 25% glutaraldehyde solution, glutaraldehyde solution is 0.5-2 with bamboo pulpboard mass ratio:1.
3. the preparation method of a kind of cellulose according to claim 1-silk gum degradable flocculation material, it is characterised in that：
Described bamboo pulpboard is the one kind in cizu pulpboard, fishscale bamboo pulpboard, bamboo pulpboard and square bamboo pulp plate.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108217892A (en) * | 2018-01-04 | 2018-06-29 | 浙江理工大学 | A kind of preparation method of cellulose-chitosan green flocculation material for the processing fabric dyeing waste water of multicomponent containing silk |
| CN109225170A (en) * | 2018-09-27 | 2019-01-18 | 陕西科技大学 | A kind of cellulose base adsorbent material and its preparation method and application of casein crosslinking |
| CN109553215A (en) * | 2018-11-19 | 2019-04-02 | 浙江海洋大学 | A kind of processing method of electroplating wastewater |
| CN109880182A (en) * | 2019-02-20 | 2019-06-14 | 西南大学 | Dialdehyde carboxymethyl cellulose/sericin composite membrane preparation method and application |
| CN111056669A (en) * | 2019-12-25 | 2020-04-24 | 浙江理工大学桐乡研究院有限公司 | Method for treating silk broadcloth refining wastewater |
| CN114958009A (en) * | 2022-05-24 | 2022-08-30 | 浙江理工大学 | Preparation method of silk-based high-strength ionic gel flexible sensing material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102505477A (en) * | 2011-11-02 | 2012-06-20 | 浙江理工大学 | Method for preparing fabric finishing agent from sericin recycled from silk processing wastewater |
| CN104722277A (en) * | 2015-02-16 | 2015-06-24 | 浙江理工大学 | Preparation method of green metal absorbing material with cellulose and sericin |
-
2017
- 2017-01-10 CN CN201710018167.4A patent/CN106832987A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102505477A (en) * | 2011-11-02 | 2012-06-20 | 浙江理工大学 | Method for preparing fabric finishing agent from sericin recycled from silk processing wastewater |
| CN104722277A (en) * | 2015-02-16 | 2015-06-24 | 浙江理工大学 | Preparation method of green metal absorbing material with cellulose and sericin |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108217892A (en) * | 2018-01-04 | 2018-06-29 | 浙江理工大学 | A kind of preparation method of cellulose-chitosan green flocculation material for the processing fabric dyeing waste water of multicomponent containing silk |
| CN109225170A (en) * | 2018-09-27 | 2019-01-18 | 陕西科技大学 | A kind of cellulose base adsorbent material and its preparation method and application of casein crosslinking |
| CN109225170B (en) * | 2018-09-27 | 2021-06-29 | 陕西科技大学 | Casein crosslinked cellulose-based adsorption material and preparation method and application thereof |
| CN109553215A (en) * | 2018-11-19 | 2019-04-02 | 浙江海洋大学 | A kind of processing method of electroplating wastewater |
| CN109553215B (en) * | 2018-11-19 | 2021-11-09 | 浙江海洋大学 | Method for treating electroplating wastewater |
| CN109880182A (en) * | 2019-02-20 | 2019-06-14 | 西南大学 | Dialdehyde carboxymethyl cellulose/sericin composite membrane preparation method and application |
| CN109880182B (en) * | 2019-02-20 | 2021-06-11 | 西南大学 | Preparation method and application of dialdehyde carboxymethyl cellulose/sericin composite membrane |
| CN111056669A (en) * | 2019-12-25 | 2020-04-24 | 浙江理工大学桐乡研究院有限公司 | Method for treating silk broadcloth refining wastewater |
| CN114958009A (en) * | 2022-05-24 | 2022-08-30 | 浙江理工大学 | Preparation method of silk-based high-strength ionic gel flexible sensing material |
| CN114958009B (en) * | 2022-05-24 | 2024-01-16 | 浙江理工大学 | Preparation method of silk-based high-strength ionic gel flexible sensing material |
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