CN105692847B - A kind of method that unreacted monomer is recycled during synthetic cellulose base flocculation material - Google Patents
A kind of method that unreacted monomer is recycled during synthetic cellulose base flocculation material Download PDFInfo
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- CN105692847B CN105692847B CN201610062655.0A CN201610062655A CN105692847B CN 105692847 B CN105692847 B CN 105692847B CN 201610062655 A CN201610062655 A CN 201610062655A CN 105692847 B CN105692847 B CN 105692847B
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- polyacrylamide
- cellulose base
- unreacted
- flocculation material
- unreacted monomer
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
- C02F1/56—Macromolecular compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- 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
- C02F1/547—Tensides
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- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
The invention discloses a kind of method that unreacted monomer is recycled during synthetic cellulose base flocculation material.Main points using method are to filter to separate unreacted monomer by filtered through gauze and Buchner funnel, and the absolute dry mass of unreacted monomer is detected using weight method, then add appropriate polyacrylamide, are re-used for the building-up process of cellulose base flocculation material.Offer technology of the present invention is recycling the unreacted monomer of production process, reduces building-up process raw material and production cost, reduces production link environmental pollution etc., can play the role of key.
Description
Technical field
It is more particularly to a kind of to flocculate in synthetic cellulose base the present invention relates to a kind of method for recycling unreacted monomer
The method that unreacted monomer is recycled in materials process, belongs to technical field of chemical engineering.
Background technology
Natural polymer flocculation material belongs to one kind in high molecular surfactant, have it is safe and non-toxic, can biology drop
The advantages that solving, be cheap.Cellulose has the characteristics that glucose cyclic structure, is prepare natural polymer flocculation material good
Good raw material；The semirigid structure of its molecule, molecule is not easy to crimp in water phase, so as to be not easy to form micella, has higher table
Face activity.In addition, cellulose hydroxyl group activity is higher, that is, have compared with strongly hydrophilic, the graft copolymer of synthesis, which has, easily to be prepared, kind
The advantages that more.
Cellulose base flocculation material, the product mainly formed by native cellulose and Polyacrylamide Grafted, has good
Good flocculating property.Relative to traditional polyacrylamide flocculant, cellulose base flocculation material also has good biology
Degradation property, raw material sources are extensively and can the advantage such as Natural re generation.But in synthetic cellulose base flocculation material after reaction
Solution product in also there are unreacted monomer, such monomer of circulating and recovering, can reduce building-up process raw material and production cost,
Reduction production link environmental pollution etc. is played the role of key.
In cellulose base flocculation material preparation field, Chinese patent（201210243734.3）" a kind of modified cellulose gives up
Water treatment flocculant and preparation method thereof " is first made by oneself epoxychloropropane and ethylenediamine using microwave technology using sawdust as raw material
Etherifying agent, continues to be acted on wood fiber element with etherifying agent with microwave, synthetic cellulose flocculant for treating waste water；Chinese patent
（ZL 200910063702.3）" composite type polymeric flocculant " is with elm leather and fur powder, cactus powder, sodium carboxymethylcellulose and gathers
Acrylamide raw material, which is mixed with, to be formed, and is mainly used in the fields such as wastewater treatment, sludge condensation, pulp recovery, oil exploitation,
It can be used under the conditions of higher temperature and wider pH value；United States Patent (USP)（US 8623966）“Process for preparing
Acrylamide copolymers by hofmann degradation reaction " are by acrylamide in alkaline condition
Under hoffman degradation reaction prepare cationic or amphoteric flocculant；United States Patent (USP)（US6316507）“Method for
Producing a high-molecular weight flocculant " provide a kind of side of synthetic polymeric flocculant
Method：Amino-compound is added in the high molecular material of cyano-containing and the obtained flocculant product of synthesis is hydrolyzed again.By mesh
Before, it yet there are no in the production process of synthetic cellulose base flocculation material, recycle the related process skill of unreacted monomer
Art occurs.
The unprocessed or incomplete nitrogen-containing pollutant of processing is discharged into natural environment and easily causes water body environment eutrophication
Pollution；Ammonia nitrogen can also gaining water-supplying disinfection and the chlorine dosage in industrial circulating water sterilisation process；The noble metals such as corrosion copper are set
It is standby.Therefore, the reduction technology of ammonia-nitrogen content has caused the great attention of field of environment protection in positive development ＆ production waste water.Using simple
Efficient reuse technology recycles unreacted nitrogen containing monomer during synthetic cellulose base flocculation material, you can reduces and closes
Into process raw material and production cost, production link environmental pollution is reduced, there is important production and social benefit.
The content of the invention
To reduce cellulose base flocculation material production cost, while realize not anti-in cellulose base flocculation material production process
The recycling and reuse of monomer are answered, production link environmental pollution are reduced, the object of the present invention is to provide one kind in synthetic cellulose
The method that unreacted monomer is recycled during base flocculation material.
To achieve the above object, the technical scheme is that using following steps：
1）30 mL of solution product of synthetic cellulose base flocculation material is added in 90-120 mL distilled water, stirs 4-
8 min obtain diluted solution product to uniform；
2）By step 1）Obtained diluted solution product, is filtered with double-deck hospital gauze, and filtrate is added to 60-90
In mL acetone solns, the quick 4-8 min that stir are filtered to uniform, then through Buchner funnel, obtain the solid through separating smoke filtrate；
3）By step 2）The obtained solid through separating smoke filtrate is placed in dry 6-8 h in 50-60 DEG C of convection oven, then will
Dry solid, which is put into pulverizer, to be crushed, and is obtained through particulate solids；
4）By step 3）Obtain through particulate solids, its absolute dry mass is measured with weight method；
5）According to step 4）The solid particle absolute dry mass of measure, supplements the polyacrylamide of corrresponding quality, adds together
In cellulose solution, the building-up process of cellulose base flocculation material is re-used for.
The solid and solid particle is respectively unreacted polyacrylamide and polyacrylamide particle.
The cellulosic material that the cellulose base flocculation material uses is birch pulp, yearning between lovers wood pulp, Scotland pine
One kind in paper pulp.
Compared with background technology, the invention has the advantages that：
Circulation profit of the technology provided by the present invention for the unreacted monomer during synthetic cellulose base flocculation material
With, and then reducing the raw material of building-up process and production cost, reducing production link environmental pollution etc., it can play key
Effect, meets the principles and policies of national development circular economy.
Brief description of the drawings
Fig. 1 is that standard kaolin solution is by the contrast photo before and after cellulose base flocculation material flocculation treatment, wherein a
Using photo after the cellulose base flocculation material flocculation treatment standard kaolin solution of initial monomer synthesis, b is using embodiment 1
The cellulose base flocculation material for recycling unreacted monomer synthesis handles photo after standard kaolin solution.
Embodiment
With reference to specific embodiment, the invention will be further described.
Embodiment 1:
1）30 mL of solution product for synthesizing birch pulp cellulose base flocculation material is added in 90 mL distilled water, is stirred
4 min are mixed to uniform, obtain diluted solution product；
2）By step 1）Obtained diluted solution product, is filtered with double-deck hospital gauze, and filtrate is added to 60 mL third
In ketone solution, quick 4 min that stir are filtered to uniform, then through Buchner funnel, obtain the polyacrylamide through separating smoke filtrate；
3）By step 2）The obtained polyacrylamide through separating smoke filtrate is placed in dry 6 h in 50 DEG C of convection ovens, then
Dry polyacrylamide is put into pulverizer and is crushed, obtains the polyacrylamide particle through crushing；
4）By step 3）The obtained polyacrylamide particle through crushing, its absolute dry mass is measured with weight method；
5）According to step 4）The polyacrylamide particle absolute dry mass of measure, supplements the polyacrylamide of corrresponding quality, and one
Rise and add in cellulose solution, be re-used for the building-up process of cellulose base flocculation material.
Embodiment 2:
1）30 mL of solution product for synthesizing birch pulp cellulose base flocculation material is added in 100 mL distilled water,
5 min are stirred to uniform, obtain diluted solution product；
2）By step 1）Obtained diluted solution product, is filtered with double-deck hospital gauze, and filtrate is added to 70 mL third
In ketone solution, quick 5 min that stir are filtered to uniform, then through Buchner funnel, obtain the polyacrylamide through separating smoke filtrate；
3）By step 2）The obtained polyacrylamide through separating smoke filtrate is placed in dry 7 h in 50 DEG C of convection ovens, then
Dry polyacrylamide is put into pulverizer and is crushed, obtains the polyacrylamide particle through crushing；
4）By step 3）The obtained polyacrylamide particle through crushing, its absolute dry mass is measured with weight method；
5）According to step 4）The polyacrylamide particle absolute dry mass of measure, supplements the polyacrylamide of corrresponding quality, and one
Rise and add in cellulose solution, be re-used for the building-up process of cellulose base flocculation material.
Embodiment 3:
1）30 mL of solution product for synthesizing Acacia paper cellulose base flocculation material is added to 110 mL distilled water
In, 7 min are to uniform for stirring, obtain diluted solution product；
2）By step 1）Obtained diluted solution product, is filtered with double-deck hospital gauze, and filtrate is added to 80 mL third
In ketone solution, quick 7 min that stir are filtered to uniform, then through Buchner funnel, obtain the polyacrylamide through separating smoke filtrate；
3）By step 2）The obtained polyacrylamide through separating smoke filtrate is placed in dry 7 h in 60 DEG C of convection ovens, then
Dry polyacrylamide is put into pulverizer and is crushed, obtains the polyacrylamide particle through crushing；
4）By step 3）The obtained polyacrylamide particle through crushing, its absolute dry mass is measured with weight method；
5）According to step 4）The polyacrylamide particle absolute dry mass of measure, supplements the polyacrylamide of corrresponding quality, and one
Rise and add in cellulose solution, be re-used for the building-up process of cellulose base flocculation material.
Embodiment 4:
1）30 mL of solution product for synthesizing Scotland pine paper cellulose base flocculation material is added to 120 mL distilled water
In, 8 min are to uniform for stirring, obtain diluted solution product；
2）By step 1）Obtained diluted solution product, is filtered with double-deck hospital gauze, and filtrate is added to 90 mL third
In ketone solution, quick 8 min that stir are filtered to uniform, then through Buchner funnel, obtain the polyacrylamide through separating smoke filtrate；
3）By step 2）The obtained polyacrylamide through separating smoke filtrate is placed in dry 8 h in 60 DEG C of convection ovens, then
Dry polyacrylamide is put into pulverizer and is crushed, obtains the polyacrylamide particle through crushing；
4）By step 3）The obtained polyacrylamide particle through crushing, its absolute dry mass is measured with weight method；
5）According to step 4）The polyacrylamide particle absolute dry mass of measure, supplements the polyacrylamide of corrresponding quality, and one
Rise and add in cellulose solution, be re-used for the building-up process of cellulose base flocculation material.
The cellulose base flocculation material of unreacted monomer synthesis will be recycled using initial monomer and embodiment 1,2,3,4
Material, is respectively applied to standard kaolin solution flocculation treatment, kaolin solution turbidity before and after measure flocculation.Table 1 is by initial single
Turbidity change before and after the cellulose base flocculation material flocculation standard kaolin solution that body and embodiment 1,2,3,4 synthesize.By table 1
Middle data are understood, using turbidity after the cellulose base flocculation material flocculation treatment kaolin solution synthesized by offer technology of the present invention
Between 10.6-12.3 NTU, the flocculating property of the cellulose base flocculation material synthesized with initial monomer（11.2 NTU）More
It is close, illustrate to recycle unreacted monomer by technology provided by the invention, to the production process of cellulose base flocculation material
It will not be adversely affected with properties of product.
Such as Fig. 1, embodiment 1 is recycled to the cellulose base flocculation material of unreacted monomer synthesis, for flocculation treatment
Standard kaolin solution effect, the cellulose base flocculation material flocculation treatment effect synthesized with using initial monomer is very close,
Kaolin solution is more clarified after flocculation treatment.
Table 1
| Standard kaolin solution is original Turbidity（NTU） | Flocculated using the cellulose base flocculation material of initial monomer synthesis Standard kaolin solution turbidity afterwards（NTU） | Marked after recycling the cellulose base flocculation material flocculation of unreacted monomer synthesis Quasi- kaolin solution turbidity（NTU） | |
| Embodiment 1 | 546 | 11.2 | 11.5 |
| Embodiment 2 | 546 | 11.2 | 10.6 |
| Embodiment 3 | 546 | 11.2 | 12.3 |
| Embodiment 4 | 546 | 11.2 | 11.0 |
Listed above is only the specific embodiment of the present invention.The invention is not restricted to above example, can also there is many
Deformation.All deformations that those of ordinary skill in the art directly can export or associate from present disclosure, should all
It is considered protection scope of the present invention.
Claims (1)
- A kind of 1. method that unreacted monomer is recycled during synthetic cellulose base flocculation material, it is characterised in that bag Include following steps：1）By using one kind in birch pulp, yearning between lovers wood pulp, Scotland pine paper pulp as Material synthesis cellulose base flocculation material 30 mL of solution product be added in 90-120 mL distilled water, 4-8 min are to uniform for stirring, obtain diluted solution production Product；2）By step 1）Obtained diluted solution product, is filtered with double-deck hospital gauze, and filtrate is added to 60-90 mL third In ketone solution, the quick 4-8 min that stir are filtered to uniform, then through Buchner funnel, obtain the unreacted poly- third through separating smoke filtrate Acrylamide；3）By step 2）The obtained unreacted polyacrylamide through separating smoke filtrate is placed in dry 6- in 50-60 DEG C of convection oven 8 h, then dry unreacted polyacrylamide is put into pulverizer and is crushed, obtain the unreacted polyacrylamide through crushing Grain；4）By step 3）The obtained unreacted polyacrylamide particle through crushing, its absolute dry mass is measured with weight method；5）According to step 4）The unreacted polyacrylamide particle absolute dry mass of measure, supplements the polyacrylamide of corrresponding quality, Add together in cellulose solution, be re-used for the building-up process of cellulose base flocculation material.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4028290A (en) * | 1975-10-23 | 1977-06-07 | Hercules Incorporated | Highly absorbent modified polysaccharides |
| CN1196334A (en) * | 1997-04-11 | 1998-10-21 | 广州市环境保护科学研究所 | Method for preparing cation/amphoteric graft polyacrylamide flocculating agent |
| CN101633527A (en) * | 2009-08-26 | 2010-01-27 | 武汉金坡环境工程有限公司 | Composite type polymeric flocculant |
| CN103172790A (en) * | 2013-04-11 | 2013-06-26 | 南京大学 | Hydrolysis graft strengthened anionic carboxymethyl cellulose flocculating agent and preparation method thereof |
| CN103254443A (en) * | 2013-05-28 | 2013-08-21 | 浙江理工大学 | Preparation method of textile waste cellulose based sewage flocculant |
| CN103613707A (en) * | 2013-12-13 | 2014-03-05 | 山东大学 | Amphiprotic acrylamide copolymer with twin tail long chains and preparation method thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2010144575A1 (en) * | 2009-06-09 | 2010-12-16 | William Chambers | Biodegradable absorbent material and method of manufacture |
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2016
- 2016-01-29 CN CN201610062655.0A patent/CN105692847B/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4028290A (en) * | 1975-10-23 | 1977-06-07 | Hercules Incorporated | Highly absorbent modified polysaccharides |
| CN1196334A (en) * | 1997-04-11 | 1998-10-21 | 广州市环境保护科学研究所 | Method for preparing cation/amphoteric graft polyacrylamide flocculating agent |
| CN101633527A (en) * | 2009-08-26 | 2010-01-27 | 武汉金坡环境工程有限公司 | Composite type polymeric flocculant |
| CN103172790A (en) * | 2013-04-11 | 2013-06-26 | 南京大学 | Hydrolysis graft strengthened anionic carboxymethyl cellulose flocculating agent and preparation method thereof |
| CN103254443A (en) * | 2013-05-28 | 2013-08-21 | 浙江理工大学 | Preparation method of textile waste cellulose based sewage flocculant |
| CN103613707A (en) * | 2013-12-13 | 2014-03-05 | 山东大学 | Amphiprotic acrylamide copolymer with twin tail long chains and preparation method thereof |
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