CN100999352A - Konjaku graft acrylamide non ionic polymer flocculant and its preparation method - Google Patents

Konjaku graft acrylamide non ionic polymer flocculant and its preparation method Download PDF

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Publication number
CN100999352A
CN100999352A CN 200610022521 CN200610022521A CN100999352A CN 100999352 A CN100999352 A CN 100999352A CN 200610022521 CN200610022521 CN 200610022521 CN 200610022521 A CN200610022521 A CN 200610022521A CN 100999352 A CN100999352 A CN 100999352A
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konjaku
acrylamide
polymer flocculant
ionic polymer
non ionic
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冯玉军
谢陈鑫
操卫平
夏雨
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Chengdu Organic Chemicals Co Ltd of CAS
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Chengdu Organic Chemicals Co Ltd of CAS
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Abstract

This invention relates to an Amorphophallus konjac stem grafting acrylamide non-ion high polymer flocculating agent and its preparation method. This flocculating agent is made up of following raw materials: Amorphophallus konjac glue, acrylamide, catalytic agent, removing metal chelating agent, and solvent. At certain condition, Amorphophallus konjac glue and acrylamide react to prepare it. This flocculating agent has good water solubility. Dissolving rate is quicker than traditional synthesized flocculating agent such as poly-propionamide. It overcomes flaws of slow dissolving rate and inconvenient field using of traditional poly-propionamide; because of copolymerizing with natural product Amorphophallus konjac, it has advantage of strong natural product biodegradation. After be used, it do not cause secondary pollution. It can be used in process of city domestic sewage and industrial sewage.

Description

Konjaku graft acrylamide non ionic polymer flocculant and preparation method thereof
Technical field
The present invention relates to a kind of konjaku graft acrylamide non ionic polymer flocculant and preparation method thereof.
Background technology
At present, the pollution of China's water surrounding is relatively more serious, and water pollution and water source crisis are the major issues that is related to national economy.City domestic sewage and trade effluent must be through handling before being discharged into natural water body, to remove suspended substance in anhydrating, impurity, particle etc.In wastewater treatment process, flocculation sedimentation is a kind of not only economy but also easy water conditioning method of the processing waste water that generally adopts at present both at home and abroad, and organic polymer coargulator is the most widely used flocculation agent at present.
Organic polymer coargulator is broadly divided into synthetic and natural macromolecule flocculating agent, and synthetic series polymeric flocculant is main representative with the polyacrylamide, accounts for 86% of whole synthetic organic polymer flocculation agent.Synthetic polymeric flocculant has and is easy to by molecular designing, utilizes different synthesizing means " to cut out " molecular structure and can regulate and control the advantage of its performance as required flexibly.On flocculating effect, synthetic series polymeric flocculant has that flocculation rate is fast, and consumption is few, and the little characteristics of the salt that coexisted, PH and temperature effect.But exist following shortcoming simultaneously: cause secondary pollution thereby remain in to be difficult in the water body degrade; Residual acrylamide monomer is a kind of very strong material of nervosa of poisoning, and has very strong carinogenicity, and HUMAN HEALTH is enough become great threat.Natural macromolecule flocculating agent have readily biodegradable, good with Environmental compatibility, be difficult for causing advantage such as secondary pollution.
Therefore, in order to have the characteristic of natural polymer and synthetic macromolecule simultaneously, can adopt the method for natural polymer graft acrylamide to prepare novel organic polymer coargulator.
Summary of the invention
The objective of the invention is to prepare the natural modified polymeric flocculant of a kind of non-ionic type, adopt natural product konjaku and acrylamide monomer, copolymerization under certain condition forms.After connecting inflexible polyacrylamide long-chain by natural polymer, can form more effectively, shear more stable and have the flocculation agent of biological degradability in flexibility.
Flocculation agent of the present invention is made up of following raw material:
(1) 0.5~0.7% (weight) konjaku: selecting KGM content for use is more than 95%, and fineness is 200 purpose konjak gums
(2) 4%~8% (weight) acrylamide: select technical grade for use
(3) 0.1%~0.2% (weight) catalyzer: select ceric ammonium nitrate for use
(4) 0.04%~0.05% (weight) are removed metal chelating agent: select EDTA for use
(5) 90%~95% (weight) solvent: select deionized water for use
The present invention has following characteristics:
1, synthetic konjaku graft acrylamide non ionic polymer flocculant of the present invention has good water-solubility, can on-the-spot provisional configuration use.
2, synthetic konjaku graft acrylamide non ionic polymer flocculant of the present invention has good flocculating effect, can be widely used in municipal effluent and the Industrial Wastewater Treatment.
3, synthetic konjaku graft acrylamide non ionic polymer flocculant of the present invention has good biodegradable.
Description of drawings
Fig. 1 is the flocculating effect of natural unmodified konjak gum when handling the kaolin simulated sewage for konjaku graft acrylamide non ionic polymer flocculant of the present invention contrasts.
Fig. 2,3 comparative illustration the good biodegradable that has of konjaku graft acrylamide non ionic polymer flocculant of the present invention.Fig. 2 is the relative viscosity of konjaku in an aqueous solution change curve in time.Fig. 3 is the relative viscosity of this konjaku graft acrylamide non ionic polymer flocculant in an aqueous solution change curve in time.
Embodiment
The present technique invention realizes by following measure:
Konjaku graft acrylamide non ionic polymer flocculant is the polymkeric substance that is formed by konjaku and acrylamide copolymerization.Wherein below preferred 200 orders of konjaku, KGM content is more than 95%, and the general structure of konjaku is as follows; The preferred technical grade of acrylamide; The preferred ceric ammonium nitrate of catalyzer; Go metal chelating agent to select EDTA for use.
Building-up process is initiator system with the cerium ion.Reaction process is as follows:
Figure A20061002252100051
With the cerium ion is initiator, and reaction mechanism is as follows:
KOH+Ce 4+→KO.+Ce 3++H + (1)
KO.+M→KGM-OM. (2)
M+Ce 4+→M.+Ce 3++H + (3)
KOM.+M→KOM 2. (4)
KOM n-1.+M→KOM n. (5)
M n-1.+M→M n. (6)
KOM n-1.+M→KM n-1+M. (7)
KOM n-1.+KOH→KOM n-1+KO.+H + (8)
KOM n.+KOM n. → graft copolymer (9)
KOM n.+Ce 4+→ graft copolymer+Ce 3++ H +(10)
Wherein KOH is a konjak gum, and M is an acrylamide, and Ce is a cerium ion
Polymeric flocculant is generally linear structure, and the big more hydrocarbon chain that has of molecular weight is long more, and effectively functional group is also many more, and flocculation agent of the present invention is a non-ionic type, plays throwing out by intermolecular adsorption bridging effect.
The present invention takes solution polymerization process synthetic, and concrete steps are as follows:
In reaction vessel, to drop into the acrylamide monomer reaction after konjak gum and the gelatinization of deionized water elder generation, add the ceric ammonium nitrate catalyzer again and remove metal complex ionic agent EDTA, wherein konjaku and acrylamide monomer consumption are 4.5%~9.5%, initiator amount is 0.2%~1%, removing metal complex ionic agent consumption is 0.1%~0.5%, gets final product discharging in reaction under 40~70 ℃ after 5~10 hours, finishes to continue to feed high purity nitrogen in the reaction process from beginning to testing.Discharging is for gluing shape solution, and reaction utilizes acetone soln repetitive scrubbing discharging gained to glue shape solution after finishing, and the solid that is settled out gets pure graft product after dry 48 hours under 40~70 ℃ in vacuum drying oven.
The invention will be further described below in conjunction with embodiment.
Embodiment 1
1g konjak gum and 125ml deionized water added in the reactor that whipping appts is housed gelatinization 1 hour, add 8.52g acrylamide reaction 0.5 hour, add 0.10275g ceric ammonium nitrate catalyzer and 0.073g again and go metal complex ionic agent EDTA, from beginning to testing, finish to continue to feed high purity nitrogen in the reaction process 60 ℃ of reaction dischargings after 24 hours down.After reaction finishes, utilize the discharging of acetone soln repetitive scrubbing glue shape solution, the solid that is settled out is 60 ℃ of dryings 48 hours down in vacuum drying oven.
Embodiment 2
1g konjak gum and 125ml deionized water added in the reactor that whipping appts is housed gelatinization 1 hour, add 8.52g acrylamide reaction 0.5 hour, add 0.137g ceric ammonium nitrate catalyzer and 0.073g again and go metal complex ionic agent EDTA, from beginning to testing, finish to continue to feed high purity nitrogen in the reaction process 50 ℃ of reaction dischargings after 24 hours down.After reaction finishes, utilize the discharging of acetone soln repetitive scrubbing glue shape solution, the solid that is settled out is 70 ℃ of dryings 48 hours down in vacuum drying oven.
Embodiment 3
1g konjak gum and 125ml deionized water added in the reactor that whipping appts is housed gelatinization 1 hour, add 8.52g acrylamide reaction 0.5 hour, add 0.274g ceric ammonium nitrate catalyzer and 0.073g again and go metal complex ionic agent EDTA, from beginning to testing, finish to continue to feed high purity nitrogen in the reaction process 70 ℃ of reaction dischargings after 24 hours down.After reaction finishes, utilize the discharging of acetone soln repetitive scrubbing glue shape solution, the solid that is settled out is 50 ℃ of dryings 24 hours down in vacuum drying oven.
Embodiment 4
1g konjak gum and 125ml deionized water added in the reactor that whipping appts is housed gelatinization 1 hour, add 17.04g acrylamide reaction 0.5 hour, add 0.10275g ceric ammonium nitrate catalyzer and 0.073g again and go metal complex ionic agent EDTA, from beginning to testing, finish to continue to feed high purity nitrogen in the reaction process 40 ℃ of reaction dischargings after 24 hours down.After reaction finishes, utilize the discharging of acetone soln repetitive scrubbing glue shape solution, the solid that is settled out is 60 ℃ of dryings 36 hours down in vacuum drying oven.
Embodiment 5
1g konjak gum and 125ml deionized water added in the reactor that whipping appts is housed gelatinization 1 hour, add 5.68g acrylamide reaction 0.5 hour, add 0.10275g ceric ammonium nitrate catalyzer and 0.073g again and go metal complex ionic agent EDTA, from beginning to testing, finish to continue to feed high purity nitrogen in the reaction process 60 ℃ of reaction dischargings after 24 hours down.After reaction finishes, utilize the discharging of acetone soln repetitive scrubbing glue shape solution, the solid that is settled out is 40 ℃ of dryings 48 hours down in vacuum drying oven.

Claims (5)

1. a konjaku graft acrylamide prepares the method for non ionic polymer flocculant, it is characterized in that: adopt copolyreaction, a certain amount of konjaku and deionized water added in the reactor that whipping appts is housed gelatinization 1~2 hour, add acrylamide reaction 0.5~1 hour, add a certain amount of catalyzer again and remove metal chelating agent, reaction got final product discharging in 5~10 hours under 40~70 ℃, obtain sticking shape solution, after reaction finishes, utilize acetone soln repetitive scrubbing discharging gained to glue shape solution, the solid that is settled out obtains pure graft product after dry 24~48 hours under 50~70 ℃ in vacuum drying oven.
2. a kind of konjaku graft acrylamide as claimed in claim 1 prepares the method for non ionic polymer flocculant, it is characterized in that: konjaku accounts for 0.5~0.7% of raw material total mass, acrylamide accounts for 4%~8%, catalyzer accounts for 0.1%~0.2%, go metal chelating agent to account for 0.04%~0.05%, deionized water accounts for 90%~95%.
3. konjaku graft acrylamide as claimed in claim 1 prepares the method for non ionic polymer flocculant, it is characterized in that: the preferred fineness of konjaku is below 200 orders, and KGM (Rhizoma amorphophalli glucomannan) content is at the konjak gum more than 95%.
4. konjaku graft acrylamide as claimed in claim 1 prepares the method for non ionic polymer flocculant, it is characterized in that: the preferred ceric ammonium nitrate of catalyzer.
5. konjaku graft acrylamide as claimed in claim 1 prepares the method for non ionic polymer flocculant, it is characterized in that: preferred EDTA is as removing metal chelating agent.
CN 200610022521 2006-12-18 2006-12-18 Konjaku graft acrylamide non ionic polymer flocculant and its preparation method Pending CN100999352A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102876312A (en) * 2012-09-26 2013-01-16 西南石油大学 Acrylamide graft copolymer oil-displacing agent and preparation method thereof
CN102952238A (en) * 2011-08-21 2013-03-06 华中农业大学 Preparation method and application of polymeric flocculant
CN103421454A (en) * 2013-08-22 2013-12-04 四川魔力科技有限公司 Konjac adhesive and preparation method thereof
CN107758826A (en) * 2017-12-20 2018-03-06 葛延瑱 A kind of preparation method of sewage treatment flocculating agent
CN110054434A (en) * 2019-06-05 2019-07-26 杭州中齐新材料科技有限公司 A kind of non-dispersible underwater concrete flocculant

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102952238A (en) * 2011-08-21 2013-03-06 华中农业大学 Preparation method and application of polymeric flocculant
CN102876312A (en) * 2012-09-26 2013-01-16 西南石油大学 Acrylamide graft copolymer oil-displacing agent and preparation method thereof
CN102876312B (en) * 2012-09-26 2015-01-07 西南石油大学 Acrylamide graft copolymer oil-displacing agent and preparation method thereof
CN103421454A (en) * 2013-08-22 2013-12-04 四川魔力科技有限公司 Konjac adhesive and preparation method thereof
CN107758826A (en) * 2017-12-20 2018-03-06 葛延瑱 A kind of preparation method of sewage treatment flocculating agent
CN107758826B (en) * 2017-12-20 2018-08-31 北京荣士都生物科技有限公司 A kind of preparation method of sewage treatment flocculating agent
CN110054434A (en) * 2019-06-05 2019-07-26 杭州中齐新材料科技有限公司 A kind of non-dispersible underwater concrete flocculant

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