CN101270179A - Process for synthesizing modified starch series polymeric flocculant - Google Patents
Process for synthesizing modified starch series polymeric flocculant Download PDFInfo
- Publication number
- CN101270179A CN101270179A CNA2008100506732A CN200810050673A CN101270179A CN 101270179 A CN101270179 A CN 101270179A CN A2008100506732 A CNA2008100506732 A CN A2008100506732A CN 200810050673 A CN200810050673 A CN 200810050673A CN 101270179 A CN101270179 A CN 101270179A
- Authority
- CN
- China
- Prior art keywords
- product
- reaction
- neutralizer
- polymeric flocculant
- add
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Landscapes
- Separation Of Suspended Particles By Flocculating Agents (AREA)
Abstract
The invention discloses a synthetic method of a modified starch polymeric flocculant. The flocculant takes starch, peat and acrylic acid as main materials and adopts a novel production process to deploy neutralizer, graft copolymerization and conduct post-treatment to the product, etc; the whole reaction is completed in the same reactor by exothermic reaction without heating, nitrogen protection and starch gelatinization; the production process is simple, all materials added in become products; the reaction process does not produce any side-product and waste, is conducted under mild conditions and easily controllable. The flocculant is characterized by strong adsorption capacity, small consumption, fast settlement, easiness in separation, capability of biodegradation, etc., being applicable to all water quality, in particular to treatment of urban sewage and industrial wastewater.
Description
Technical field
The invention belongs to the preparation method of polymeric flocculant.Being specifically related to a kind of is main raw material with Semen Maydis powder, peat and vinylformic acid etc., adopts the modified starch series flocculation agent of novel production process.
Background technology
Flocculation agent is widely used in sewage disposal, mainly can be divided into inorganic flocculating agent, synthetic organic polymer coargulator and natural organic high-molecular flocculant three major types by its raw material.Wherein inorganic flocculating agent and synthetic polymeric flocculant are owing to can have certain potential hazard to people and other animals and plants in production, use and subsequent processes, and inorganic flocculating agent is subjected to the variation of temperature, water temperature easily and influences flocculating effect, therefore is very limited in the use.
Modified starch flocculant is the natural modified polymeric flocculant of a class, characteristics such as raw material is easy to get because it has, cheap, nontoxic, readily biodegradable, environmentally safe are having broad application prospects aspect the purifying treatment of tap water and various industrial sewages.Particularly along with the improving constantly of people's environmental consciousness, this research also comes into one's own day by day.The modified starch flocculant kind of exploitation is a lot of at present, mainly is divided into starch graft copolymer class flocculation agent, starch ethers flocculation agent and several classes of starch xanthate class flocculation agent.The novel environment friendly flocculation agent that we developed belongs to the starch graft copolymer class, existing starch graft copolymer series polymeric flocculant exists complex manufacturing, condition control to require high, shortcomings such as reaction yield is low, product postprocessing complexity, these shortcomings cause producing difficulty, cost is too high, be unfavorable for environmental protection, industrial production and practical application are made a big impact.
According to the introduction of existing patent CN 1792854A CN166707A CN 1597549CN 1554592A etc., the main preparation technology of starch graft copolymer series polymeric flocculant graft copolymerization now is:
W-Gum → high temperature gelatinization → adding polymerization single polymerization monomer → adding initiator and linking agent → (under the nitrogen protection) → heating, maintenance isothermal reaction → starch graft copolymer
Following shortcoming is arranged on the tradition starch conversion polymeric flocculant synthetic method:
(1) starch needs gelatinization, reaction process to need nitrogen protection, the waste resource.
(2) because monomer concentration is lower, and rate of polymerization is slower, plant factor and throughput are lower.
(3) because the existence of solvent must be adopted retrieving arrangement, the product needed that reaction obtains is filtered, washing, causes the loss of raw material, also produces the waste water, waste residue etc. that environment there are pollution in the reaction process.
(4) equipment is many, complex process, and the productive rate of product is low.
Summary of the invention
The objective of the invention is to overcome the weak point that exists in the existing production technology, a kind of novel production process is provided, it is simple to have production technique, and cost is low, reaction conditions is gentle, productive rate is high, need not heating and advantages such as nitrogen protection, non-pollutant discharge.This flocculation agent has characteristics such as flocculating effect is good, high adsorption capacity, the formation flco is big, settling velocity fast, be easy to separation, and is biodegradable, pollution-free in addition.
Technological process of the present invention:
(1) configuration neutralizer: take by weighing propenyl compound 40-60g, under continuous stirring condition, 26% sodium hydroxide solution joined carry out neutralization reaction in the propenyl compound, being configured to degree of neutralization is the vinylformic acid neutralizer of 60-90%.After question response is complete, stops stirring neutralizer is cooled off gradually.
(2) graft copolymerization: in the same container, under continuous agitation condition, the Semen Maydis powder of monomer total mass 10-20% and the peat dust of monomer total mass 10-20% are successively joined in the neutralizer that is cooled to 20-40 ℃.Steady temperature stirs 20-40min, and starch and peat dust are uniformly dispersed.Add monomer total mass 0.5-2.0% initiator (Potassium Persulphate) and monomer total mass 0.1-0.5% linking agent (NMBA-----N, N-methylene-bisacrylamide) more slowly, constant temperature 0.5-3.0h.Question response liquid fades to translucent viscous fluid, adds 25% ammoniacal liquor 10-20ml, and the pH value of system is transferred to 7-8.Behind the static 10-30min, system reacts completely, and emits gas to finishing.
(3) aftertreatment of product: product is processed into little bulk, is placed in the baking oven, under 100-130 ℃, be dried to constant weight.Through broken, pulverizing, obtain particle or pulverous polymeric flocculant.
Similar flocculation agent with other is compared the principal feature of this product:
(1) from the heat release crosslinking process
The reaction carry out adopted in the process from the crosslinked technology of heat release, be reflected under the relatively mild temperature and carry out, need not additionally heat up to system, avoided the loss of energy, make the cross-linking effect of system better, this technology has been simplified reactions steps greatly, and level at home is in a leading position.
(2) flocculation agent functionalization
Macromolecule modified flocculation agent great majority are to adopt acrylamide graft starch, and we adopt the direct and Semen Maydis powder reaction of the mixture of vinylformic acid and peat.Owing to added active peat, strengthen some poisonous ionic absorption properties, improved the function of flocculation agent.This method yet there are no report at home and abroad, has guaranteed the novelty of our projects.
The peat incomplete decomposing that is the marsh plant remains in crossing wet and anaerobic environment and the hover ground plastid that contains organic matter, humic acid, mineral substance and colloid that forms.We select peat some characteristics of peat of having made prepared using itself, have improved the part character of flocculation agent.The organic matter of peat, content of humic acid height, fibre content is abundant, and loose porous, ventilating permeable is good, and specific surface area is big, and the absorption sequestering power is strong, and this has improved the adsorptive power of product flocculation agent greatly.It provides big molecular skeleton for flocculation agent in addition, the utilization ratio of flocculation agent and flocculation rate is improved, and more help forming big flocculating body, is convenient to rapid subsidence and separates.
(3) technical process is simplified
Our invented technology is compared with traditional production method; do not need nitrogen protection and starch pasting process; product is one-step synthesis in process of production; utilization is finished the heat cross-linking reaction from heat release; technology advanced person; without processes such as saponification, filtration, washings, equipment is simple, reaction is continuous, has improved usage ratio of equipment and throughput.The raw material that adds all generates product, does not have by product, and productive rate improves greatly.In reaction process, reduced the loss of raw material.Equipment and raw material domesticize fully, make that cost reduces, scale operation is easier, more feasible.
(4) environment friendly and pollution-free
There is not industrial waste to produce in the production process, three waste discharges such as no waste water,waste gas and industrial residue, pollution-free, help the protection of environment, be a kind of free of contamination production technique that cleans.
In the use, product stability is good, and is nontoxic, safe and reliable, and to equipment and pipeline non-corrosiveness all, non-scaling uses and is not subjected to season, region limits, is convenient to deposit and transport.
This product adopts starch to make up macromolecular scaffold, uses the back biodegradable, environmentally safe.This product has all embodied environment friendly and pollution-free characteristics in production, use and post-processed process.
This product can also be composite with other multiple organic or inorganic flocculation agent except that above characteristics, can bring into play good flocculating effect equally, enlarged the range of application of product.
Description of drawings
Accompanying drawing is the synthesis process flow diagram of modified starch series polymeric flocculant
Embodiment
Embodiment 1
At normal temperatures, compound concentration is 26% sodium hydroxide solution 85ml, slowly joins behind the cool to room temperature in the propenyl monomer of 60g, constantly stirs to make to react completely, and is cooled to 35 ℃.Successively add the peat dust of 11g Semen Maydis powder, 12g under continuous stirring condition, Semen Maydis powder, peat dust are uniformly dispersed, constant temperature stirred 30 minutes.The initiator, the 0.2g linking agent that add 0.7g more slowly successively, constant temperature stirring reaction 3 hours.Add 17ml ammoniacal liquor, the pH value of system is transferred to 7, reaction system left standstill 20 minutes, and reaction is after finish, and 120 ℃ of oven dry down, fragmentation, pulverizing obtain flaxen powdery product the product that obtains.
Embodiment 2
At normal temperatures, compound concentration is 26% sodium hydroxide solution 40ml, slowly joins behind the cool to room temperature in the propenyl monomer of 40g, constantly stirs to make to react completely, and is cooled to 25 ℃.Successively add the peat dust of 8g Semen Maydis powder, 6g under continuous stirring condition, Semen Maydis powder, peat dust are uniformly dispersed, constant temperature stirred 20 minutes.The initiator, the 0.05g linking agent that add 0.2g more slowly successively, constant temperature stirring reaction 1 hour.Add 10ml ammoniacal liquor, the pH value of system is transferred to 8, reaction system left standstill 10 minutes, and reaction is after finish, and 100 ℃ of oven dry down, fragmentation, pulverizing obtain flaxen powdery product the product that obtains.
Embodiment 3
At normal temperatures, compound concentration is 26% sodium hydroxide solution 65ml, slowly joins behind the cool to room temperature in the propenyl monomer of 50g, constantly stirs to make to react completely, and is cooled to 40 ℃.Successively add the peat dust of 5g Semen Maydis powder, 10g under continuous stirring condition, Semen Maydis powder, peat dust are uniformly dispersed, constant temperature stirred 40 minutes.The initiator, the 0.1g linking agent that add 1.0g more slowly successively, constant temperature stirring reaction 2 hours.Add 14ml ammoniacal liquor, the pH value of system is transferred to 8, reaction system left standstill 15 minutes, and reaction is after finish, and 120 ℃ of oven dry down, fragmentation, pulverizing obtain flaxen powdery product the product that obtains.
Claims (2)
1. the synthetic method of modified starch series polymeric flocculant is characterized in that:
(1) configuration neutralizer: take by weighing propenyl compound 40-60g, under continuous stirring condition, 26% sodium hydroxide solution joined carry out neutralization reaction in the propenyl compound, being configured to degree of neutralization is the vinylformic acid neutralizer of 60-90%, after question response is complete, stops stirring neutralizer is cooled off gradually;
(2) graft copolymerization: in the same container, under continuous agitation condition, the Semen Maydis powder of monomer total mass 10-20% and the peat dust of monomer total mass 10-20% are successively joined in the neutralizer that is cooled to 20-40 ℃, steady temperature, stir 20-40min, starch and peat dust are uniformly dispersed, add monomer total mass 0.5-2.0% initiator potassium persulfate and monomer total mass 0.1-0.5% linking agent NMBA-----N more slowly, the N-methylene-bisacrylamide, constant temperature 0.5-3.0h, question response liquid fades to translucent viscous fluid, the ammoniacal liquor 10-20ml of adding 25% transfers to 7-8 to the pH value of system, behind the static 10-30min, system reacts completely, and emits gas to finishing;
(3) aftertreatment of product: product is processed into little bulk, is placed in the baking oven, under 100-130 ℃, be dried to constant weight,, obtain particle or pulverous polymeric flocculant through broken, pulverizing.
2. the synthetic method of modified starch series polymeric flocculant as claimed in claim 1, it is characterized in that: at normal temperatures, compound concentration is 26% sodium hydroxide solution 85ml, slowly joins behind the cool to room temperature in the propenyl monomer of 60g, constantly stirring makes and reacts completely, and is cooled to 35 ℃; Successively add the peat dust of 11g Semen Maydis powder, 12g under continuous stirring condition, Semen Maydis powder, peat dust are uniformly dispersed, constant temperature stirred 30 minutes; The initiator, the 0.2g linking agent that add 0.7g more slowly successively, constant temperature stirring reaction 3 hours; Add 17ml ammoniacal liquor, reaction system left standstill 20 minutes, and reaction is after finish, and 120 ℃ of oven dry down, broken, pulverizing obtains flaxen powdery product the product that obtains.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008100506732A CN101270179A (en) | 2008-04-30 | 2008-04-30 | Process for synthesizing modified starch series polymeric flocculant |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008100506732A CN101270179A (en) | 2008-04-30 | 2008-04-30 | Process for synthesizing modified starch series polymeric flocculant |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101270179A true CN101270179A (en) | 2008-09-24 |
Family
ID=40004428
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2008100506732A Pending CN101270179A (en) | 2008-04-30 | 2008-04-30 | Process for synthesizing modified starch series polymeric flocculant |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101270179A (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101704928B (en) * | 2009-11-26 | 2011-10-05 | 广州大学 | Preparation method of starch grafted acrylamide flocculating agent |
| CN102432090A (en) * | 2011-10-27 | 2012-05-02 | 常州大学 | Method for preparing flocculation aid for pretreating blue algae biogas slurry |
| CN102974470A (en) * | 2012-12-11 | 2013-03-20 | 中国地质科学院矿产综合利用研究所 | Oolitic hematite flocculant and oolitic hematite selective dispersion agglomeration separation method |
| CN103739784A (en) * | 2014-01-15 | 2014-04-23 | 东北师范大学 | Diatomite composite super-absorbent resin material and preparation method thereof |
| CN106718061A (en) * | 2016-12-27 | 2017-05-31 | 中国林业科学研究院亚热带林业研究所 | The composite cultivation method of dictyophora phalloidea is planted under a kind of mao bamboon |
| CN107585844A (en) * | 2017-09-30 | 2018-01-16 | 铜陵家宴生态农业发展有限公司 | A kind of preparation method of lactic modified banana tegument extract composite starch coagulant |
| CN108101180A (en) * | 2017-12-29 | 2018-06-01 | 天津德清科技有限公司 | A kind of sewage-treating agent and preparation method thereof |
| CN112086635A (en) * | 2020-08-31 | 2020-12-15 | 佛山市德方纳米科技有限公司 | Preparation method of lithium iron phosphate positive electrode active material |
-
2008
- 2008-04-30 CN CNA2008100506732A patent/CN101270179A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101704928B (en) * | 2009-11-26 | 2011-10-05 | 广州大学 | Preparation method of starch grafted acrylamide flocculating agent |
| CN102432090A (en) * | 2011-10-27 | 2012-05-02 | 常州大学 | Method for preparing flocculation aid for pretreating blue algae biogas slurry |
| CN102432090B (en) * | 2011-10-27 | 2013-06-19 | 常州大学 | Method for preparing flocculation aid for pretreating blue algae biogas slurry |
| CN102974470A (en) * | 2012-12-11 | 2013-03-20 | 中国地质科学院矿产综合利用研究所 | Oolitic hematite flocculant and oolitic hematite selective dispersion agglomeration separation method |
| CN102974470B (en) * | 2012-12-11 | 2014-06-04 | 中国地质科学院矿产综合利用研究所 | Oolitic hematite flocculant and oolitic hematite selective dispersion agglomeration separation method |
| CN103739784A (en) * | 2014-01-15 | 2014-04-23 | 东北师范大学 | Diatomite composite super-absorbent resin material and preparation method thereof |
| CN106718061A (en) * | 2016-12-27 | 2017-05-31 | 中国林业科学研究院亚热带林业研究所 | The composite cultivation method of dictyophora phalloidea is planted under a kind of mao bamboon |
| CN107585844A (en) * | 2017-09-30 | 2018-01-16 | 铜陵家宴生态农业发展有限公司 | A kind of preparation method of lactic modified banana tegument extract composite starch coagulant |
| CN108101180A (en) * | 2017-12-29 | 2018-06-01 | 天津德清科技有限公司 | A kind of sewage-treating agent and preparation method thereof |
| CN112086635A (en) * | 2020-08-31 | 2020-12-15 | 佛山市德方纳米科技有限公司 | Preparation method of lithium iron phosphate positive electrode active material |
| CN112086635B (en) * | 2020-08-31 | 2022-01-07 | 佛山市德方纳米科技有限公司 | Preparation method of lithium iron phosphate positive electrode active material |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101270179A (en) | Process for synthesizing modified starch series polymeric flocculant | |
| CN103159532B (en) | A kind of preparation method of porous lignin particle compound fertilizer | |
| CN105692850B (en) | A kind of preparation method of water process banana skin high-molecular coagulant adopting | |
| CN105713049A (en) | Method for producing humic acid and sodium salt thereof | |
| CN102225985B (en) | Preparation method of macroporous sodium carboxymethylcellulose grafted copolymer with rapid swelling absorption property | |
| CN102161562A (en) | Process for treating excess sludge by utilizing fly ash | |
| CN105800892A (en) | Blue-green algae and excess sludge resourceful treatment method | |
| CN110577433A (en) | Preparation method of kitchen waste-based composite gel slow-release fertilizer | |
| CN104743756A (en) | Method for recycling sludge with low energy consumption | |
| CN103769059A (en) | Plant straw surface imprint adsorption material and preparation method thereof | |
| CN108160044A (en) | A kind of preparation method of the polynary functional group's antibiotic property biogas residue adsorbent of tool for adsorbing heavy metal and anion | |
| CN109928603A (en) | A kind of preparation method and application method of sludge green Assistant | |
| CN106221849A (en) | Stalk fuel containing biomass sludge and preparation method thereof | |
| CN109052878A (en) | A kind of microorganism sludge solidification environment-friendly materials and its application | |
| CN112337033A (en) | Harmless treatment method of abamectin slag, product and application of product as sandy soil modifier | |
| CN111908745A (en) | Method for preparing potassium humate organic fertilizer by using sludge and simultaneously dehydrating | |
| CN105399963A (en) | Mechanical-activation solid-phase preparation method of lignocellulose ester group oxidation catalyst | |
| CN104229966B (en) | A kind of magnetic collagen aleurone modified cation flocculation agent and preparation method thereof | |
| CN109851726A (en) | A kind of biodegradable graft copolymerized polymer composite material and preparation method | |
| CN112759210B (en) | Sludge treatment system and method | |
| CN103936241B (en) | A kind of recycling sludge of sewage plant treatment process | |
| CN101161695B (en) | Method for preparing absorbent material by micro-wave radiation of potato fecula industry slag grafted polymeric acrylate | |
| CN105061698A (en) | Preparation method of rice husk char based water-retaining agent | |
| CN111996008B (en) | Method for immobilizing humic acid on surface of shell natural material | |
| CN101993516A (en) | Ultraviolet light initiation preparation method of polyacrylate type composite super absorbent resin |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C53 | Correction of patent for invention or patent application | ||
| CB03 | Change of inventor or designer information |
Inventor after: Lan Yaqian Inventor after: Su Zhongmin Inventor after: Li Lu Inventor before: Su Zhongmin Inventor before: Lan Yaqian Inventor before: Li Lu |
|
| COR | Change of bibliographic data |
Free format text: CORRECT: INVENTOR; FROM: SU ZHONGMIN LAN YAQIAN LI LU TO: LAN YAQIAN SU ZHONGMIN LI LU |
|
| C12 | Rejection of a patent application after its publication | ||
| RJ01 | Rejection of invention patent application after publication |
Open date: 20080924 |