CN104448133B - A kind of preparation method and application of PAMC - Google Patents
A kind of preparation method and application of PAMC Download PDFInfo
- Publication number
- CN104448133B CN104448133B CN201410767113.4A CN201410767113A CN104448133B CN 104448133 B CN104448133 B CN 104448133B CN 201410767113 A CN201410767113 A CN 201410767113A CN 104448133 B CN104448133 B CN 104448133B
- Authority
- CN
- China
- Prior art keywords
- pamc
- nano
- preparation
- meter sio
- container
- 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.)
- Active
Links
Abstract
The invention discloses a kind of preparation method and application of PAMC.The present invention is by the way of microwave heating, with Nano-meter SiO_22Dispersion liquid, dimethyl diallyl ammonium chloride and acrylamide monomer are raw material, and vegetable oil is continuous phase, uses redox initiator initiation reaction, it is passed through after nitrogen flooding oxygen, a period of time is reacted in microwave reactor, is then transferred in water-bath, continuous heating is carried out in reaction system.PAMC glue milky product is generated by emulsion polymerization, by acetone demulsification, absolute ethyl alcohol is washed after purification, and powdery PAMC product is obtained through drying, crushing, the Cr being applied in processing water body6+Ion, Hg2+When ion, phenol and repefral, its clearance reaches more than 40%.Preparation technology of the present invention is simple, and prepared product solubility property is good, can be widely used for multiple industries such as heavy metal containing wastewater treatment, treatment of Organic Wastewater, sludge dewatering.
Description
Technical field
The invention belongs to the preparation of water treatment agent and environment-friendly engineering technical field, and in particular to a kind of microwave radiation technology triggers new
The preparation method and application of type PAMC.
Background technology
Current China's water environment is by typical contamination, and wherein heavy metal and organic matter is the important pollutant of two classes, such
Pollutant property is stable, is not easily decomposed and can be enriched with vivo, with very strong carcinogenic, teratogenesis, mutagenesis,
Therefore it is necessary for the pollutant synthesis efficient water treatment agent of low energy.
At present, water treatment agent is broadly divided into inorganic flocculating agent, organic flocculant, biological flocculant and composite flocculation agent.But
It is the increasingly complexity with water environment, traditional flocculant can not meet needs well, therefore in water environment
Characteristic pollutant it is synthetically prepared go out not only have traditional flocculant effect, and with exclusive adsorption effect novel flocculation
Agent is significant.
PAMC is the important organic water treatment agent of a class, with dosage is small, high treating effect, application
Extensively the advantages of, but the method for conventional synthesis comes with some shortcomings, and such as generated time is longer, therefore prepares generated time
It is short, and be at water for the heavy metal ion and organic pollution high treating effect, water treatment agent with low cost in water environment
Science and engineering author's urgent problem.
The content of the invention
First purpose of the present invention be for existing polyacrylamide amine product exist not enough there is provided a kind of dissolubility
Preferably, the heavy metal ion and organic matter in water environment can be effectively removed simultaneously, and is easy to the cation of industrialized production gathers
The preparation method of acrylamide.
The present invention realizes that above-mentioned purpose technical scheme is：
A kind of preparation method of PAMC, comprises the following steps：
(1) it is that Span-80 is well mixed with vegetable oil and is added in container by oleic acid sorbitan ester at 20-25 DEG C,
Its mass concentration is controlled 0.1~2.0%, 10~50% respectively；
(2) Nano-meter SiO_2 is prepared2Particle dispersion, then by the Nano-meter SiO_22Particle dispersion, dimethyl diallyl chlorination
Ammonium monomer and the acrylamide monomer aqueous solution are added sequentially in container, and the total mass concentration for controlling monomer is 10~50%, is stirred
Mixing is well mixed it, 20-25 DEG C of 20~60min of emulsification；
(3) oxidation-reduction initiator is added into container, its total mass concentration control continues breast 0.01~0.5%
Change 20~60min；
(4) the 1mol/L disodium EDTA i.e. EDTA aqueous solution is added as complexing agent, mass concentration control
System is 0.02%~0.5%；
(5) 10~50min of nitrogen is passed through, the purpose for removing oxygen in monomer mixed solution is reached；
(6) container is placed in microwave reactor, opens microwave, microwave power is controlled in 20~100W, it is warming up to 40~
120 DEG C, then keeping temperature is certain, and 3~15min of reaction polymerize it；
(7) container is taken out after completion of the reaction, then be placed under 30~70 DEG C of water bath conditions, continue to react 1~5h；
(8) a certain amount of acetone is poured slowly into container, demulsification processing is carried out to glue milky product；
(9) product after demulsification is washed with absolute ethyl alcohol, then is ground into powdery solid after being dried and produce product.
What deserves to be explained is, each mass concentration of the above is for reactant gross mass.
Further, the vegetable oil is preferably peanut oil, soya-bean oil or rapeseed oil.
Further, the Nano-meter SiO_22The preparation method of particle dispersion is：By Nano-meter SiO_22Ultrasonic disperse 2.0 hours, so
Afterwards in the basic conditions control tetraethyl orthosilicate hydrolysis, you can obtain surface have can poly- functional group Nano-meter SiO_22Particle point
Dispersion liquid.
Further, the oxidant in the oxidation-reduction initiator is hydrogen peroxide, sodium peroxide, calper calcium peroxide, oxidation
Mixture more than one or both of dibenzoyl or dilauroyl peroxide；Reducing agent is N, N- dipropyl -1- propylamine,
N, accelerine, cobalt naphthenate, manganese naphthenate, calcium naphthenate, methyl mercaptan, ethyl mercaptan, coacetylase and organo-metallic compound
One or both of more than mixture.
Further, in the step (2), Nano-meter SiO_22Nano-meter SiO_2 in dispersion liquid2, dimethyl diallyl ammonium chloride list
The mol ratio of body and acrylamide monomer is 10~80：10~80：80~10.
Second object of the present invention is the application for providing novel cation polyacrylamide prepared by the above method, i.e.,
It will be used to remove the heavy metal Cr in water environment after solid product wiring solution-forming6+Ion, Hg2+Ion, phenol, phthalic acid
Dimethyl ester.
Polymerizate cationic degree prepared by the present invention is 10~90%.
Compared to prior art, beneficial effects of the present invention are embodied in：
(1) preparation method of the invention is polymerize using three kinds of monomers, and with Nano-meter SiO_22For core, product property can be made
Viscosity profile is uniform.
(2) present invention triggers polymerization technique using microwave radiation technology, can make full use of microwave heating effect and the non-thermal effect of microwave
Should, heating polymerization is carried out to the monomer of synthesis from molecular level, the time of product preparation can be shortened, and product dissolubility is more
It is good.
(3) the PAMC heavy metal ion and organic matter prepared by the present invention have removes effect well
Really, its clearance reaches more than 40%, can expand the application of PAMC.
Embodiment
The present invention is described in further detail with reference to specific embodiment, but the present invention is not limited thereto.
Embodiment 1
(1) at 20-25 DEG C, 1.0g Span80,30.0g rapeseed oil are well mixed are added in container first；
(2) Nano-meter SiO_2 prepared is sequentially added2Dispersion liquid (its nano si-containing O2Quality be 5g), dimethyl diene
Propyl ammonium chloride monomer 15.5g (mass fraction is 60%) and acrylamide monomer 20.0g (being dissolved in 20mL distilled water),
High-speed stirred makes its well mixed emulsification 30min；
(3) initiator oxidation hydrogen peroxidase 10 .15g and methyl mercaptan 0.05g is added, 30min is emulsified；
(4) complexing agent 1.0mol/L EDTA aqueous solution 0.8mL is added after emulsifying；
(5) it is passed through nitrogen 30min and reaches the purpose for removing the oxygen in monomer mixed solution；
(6) container is placed in microwave reactor, opens microwave, it is 20W to control microwave power, be warming up to 60 DEG C, holding
Temperature is certain, and reaction 3min polymerize it；
(7) container is taken out after completion of the reaction in microwave reactor, then be placed under 60 DEG C of water bath conditions, continue to react
2h；
(8) 50mL acetone is poured slowly into glue milky product, carries out demulsification processing；
(9) finally the product after demulsification is washed with 35mL absolute ethyl alcohols；
(10) with determination of ubbelohde viscometer, its inherent viscosity is 5.3dL/g；
(11) PAMC is placed in into crushed after being dried powdering solid in 70 DEG C of baking ovens to use.
Embodiment 2
(1) at 20-25 DEG C, 0.6g Span80,20.0g soya-bean oil are well mixed are added in container first；
(2) Nano-meter SiO_2 prepared is sequentially added2Dispersion liquid (its nano si-containing O2Quality be 6g), dimethyl diene
Propyl ammonium chloride monomer 25.5g (mass fraction is 60%) and acrylamide monomer 8.5g (being dissolved in 12mL distilled water),
High-speed stirred makes its well mixed emulsification 30min；
(3) initiator hydrogen peroxidase 10 .1g and ethyl mercaptan 0.05g are added, 30min is emulsified；
(4) complexing agent 1.0mol/L EDTA aqueous solution 0.8mL is added after emulsifying；
(5) it is passed through nitrogen 40min and reaches the purpose for removing oxygen in monomer mixed solution；
(6) container is placed in microwave reactor and triggered, open microwave, it is 40W to control microwave power, is warming up to 60
DEG C, then keeping temperature is certain, and reaction 2min polymerize it；
(7) container is taken out after completion of the reaction in microwave reactor, then be placed under 60 DEG C of water bath conditions, continue to react
3h；
(8) 50mL acetone is poured slowly into white size milky product, carries out demulsification processing；
(9) finally the product after demulsification is washed with 30mL absolute ethyl alcohols；
(10) with determination of ubbelohde viscometer, its inherent viscosity is 6.2dL/g；
(11) dimethyl diallyl ammonium chloride acrylamide copolymer is placed in 75 DEG C of baking ovens crushed after being dried into powder
Shape solid is used.
Embodiment 3
The products therefrom of embodiment 2 is applied to Cr in water6+Ion, Hg2+Ion, phenol, repefral
Remove：
(1) Cr in analysis accessing pending water6+Ion, Hg2+Ion, phenol, the concentration of repefral；
(2) according to Cr in water6+Ion, Hg2+Ion, phenol, the concentration of repefral calculate cation and gathered
The amount of the contained flocculant PAMC (products therefrom of embodiment 2) added is in the reacting dose of acrylamide, water
0.01~20mg/L.
(3) removal process is：
(1) Cr will be contained6+Ion, Hg2+Ion, phenol, the water of repefral are delivered in reactor, are pressed
Above-mentioned reaction ratio, flocculant PAMC is added by chemical feed pipe into reactor；Meanwhile, starting agitator will
Above-mentioned water body and the flocculant are sufficiently stirred for, and (are stirred 2 minutes with 350r/min speed, then again with 60r/min speed
Stirring 6 minutes), by the flocculation of flocculant so that Cr among water environment6+Ion, Hg2+Ion, phenol, adjacent benzene two
Formic acid diformazan ester concentration declines more than 40%.
(2) by the water body of step (1) processing, 1~10h is stood；Flocculant cation in water is made by flocculating setting effect
Polyacrylamide and its adsorbate are deposited to bottom.
Table 1 is to remove Cr in water removal using the products therefrom of the embodiment of the present invention 26+Ion, Hg2+Ion, phenol, O-phthalic
The experimental data table of dimethyl phthalate：
Table 1
Cr in water environment6+Ion, Hg2+Ion, phenol, repefral are flocculated agent cation polypropylene
Acid amides falls to make its sedimentation so as to remove by flocculation absorption, and cationic polyacrylamide flocculant agent prepared by the present invention can make
Cr6+Ion, Hg2+Ion, phenol, the adsorption rate of repefral reach more than 40%.
Claims (5)
1. a kind of preparation method of PAMC, it is characterised in that comprise the following steps：
(1) it is that Span-80 is well mixed with vegetable oil and is added in container by oleic acid sorbitan ester at 20-25 DEG C, its matter
Amount concentration is controlled 0.1~2.0%, 10~50% respectively；
(2) Nano-meter SiO_2 is prepared2Particle dispersion, then by the Nano-meter SiO_22Particle dispersion, dimethyl diallyl ammonium chloride list
Body and the acrylamide monomer aqueous solution are added sequentially in container, and the total mass concentration for controlling monomer is 10~50%, and stirring makes
It is well mixed, 20-25 DEG C of 20~60min of emulsification；
(3) oxidation-reduction initiator is added into container, its total mass concentration control continues to emulsify 20 0.01~0.5%
~60min；
(4) the 1mol/L disodium EDTA i.e. EDTA aqueous solution is added as complexing agent, and mass concentration control exists
0.02%~0.5%；
(5) it is passed through 10~50min of nitrogen；
(6) container is placed in microwave reactor, opens microwave, microwave power is controlled in 20-100W, is warming up to 40-120 DEG C,
Then keeping temperature is certain, reacts 3-15min；
(7) container is taken out after completion of the reaction, then be placed under 30-70 DEG C of water bath condition, continue to react 1-5h；
(8) a certain amount of acetone is poured into container, demulsification processing is carried out to glue milky product；
(9) product after demulsification is washed with absolute ethyl alcohol, then is ground into powdery solid after being dried and produce product；
Wherein, the oxidant in the oxidation-reduction initiator is hydrogen peroxide, sodium peroxide, calper calcium peroxide, diphenyl peroxide
Mixture more than one or both of formyl or dilauroyl peroxide；Reducing agent is N, N- dipropyl -1- propylamine, N, N-
More than one or both of dimethylaniline, cobalt naphthenate, manganese naphthenate, calcium naphthenate, methyl mercaptan, ethyl mercaptan, coacetylase
Mixture.
2. the preparation method of PAMC according to claim 1, it is characterised in that：The vegetable oil is flower
Oil generation, soya-bean oil or rapeseed oil.
3. the preparation method of PAMC according to claim 1, it is characterised in that the Nano-meter SiO_22Particle
The preparation method of dispersion liquid is：By Nano-meter SiO_22Ultrasonic disperse 2.0 hours, then controls tetraethyl orthosilicate in the basic conditions
Hydrolysis, you can obtain surface have can poly- functional group Nano-meter SiO_22Particle dispersion.
4. the preparation method of PAMC according to claim 1, it is characterised in that：In the step (2),
Nano-meter SiO_22Nano-meter SiO_2 in dispersion liquid2, the mol ratio of dimethyldiallylammonchloride chloride monomer and acrylamide monomer is 10
~80：10~80：80~10.
5. the Cr of PAMC prepared by any one of Claims 1-4 methods described in water environment is removed6+From
Son, Hg2+Ion, phenol, the application of repefral.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410767113.4A CN104448133B (en) | 2014-12-11 | 2014-12-11 | A kind of preparation method and application of PAMC |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410767113.4A CN104448133B (en) | 2014-12-11 | 2014-12-11 | A kind of preparation method and application of PAMC |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104448133A CN104448133A (en) | 2015-03-25 |
| CN104448133B true CN104448133B (en) | 2017-07-28 |
Family
ID=52894932
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410767113.4A Active CN104448133B (en) | 2014-12-11 | 2014-12-11 | A kind of preparation method and application of PAMC |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104448133B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105199044A (en) * | 2015-11-11 | 2015-12-30 | 重庆城市管理职业学院 | Method for preparing cationic polyacrylamide employing microwave-induced template polymerization |
| CN108191027A (en) * | 2017-12-27 | 2018-06-22 | 南昌水业集团有限责任公司 | The preparation method of cation-modified polyacrylamide, sewage water treatment method |
| CN108484828B (en) * | 2018-04-18 | 2020-02-28 | 西南石油大学 | Water-in-water type cationic emulsion containing nano silicon dioxide core-shell microspheres and preparation method thereof |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06322010A (en) * | 1993-05-10 | 1994-11-22 | Dia Furotsuku Kk | Production of amphoteric water-soluble high-molecular compound |
| CN100402563C (en) * | 2005-01-31 | 2008-07-16 | 大连广汇化学有限公司 | Method for preparing temperature-resistant and anti-salt type polyacrylamide |
| CN102633937A (en) * | 2012-05-14 | 2012-08-15 | 湖南科技大学 | Preparation and application of diallyl dimethyl ammonium chloride and acrylamide copolymer |
-
2014
- 2014-12-11 CN CN201410767113.4A patent/CN104448133B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN104448133A (en) | 2015-03-25 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105621809B (en) | A kind of processing method of shale gas fracturing outlet liquid | |
| CN104085969B (en) | Spent acid is utilized to produce the method for compound polynary flocculant poly silicic acid chloro sulphuric acid ferro-aluminum | |
| CN104448133B (en) | A kind of preparation method and application of PAMC | |
| CN102718295B (en) | Compound medicament for treating coking wastewater and preparation method thereof | |
| CN105688764A (en) | Coated nano iron ball as well as preparation and application thereof | |
| CN108083609A (en) | A kind of method that municipal sludge is nursed one's health by composite reagent | |
| CN102250291A (en) | Ampholytic modified grafted starch flocculant | |
| CN108892347A (en) | A method of improving aerobic digested sludge dewatering | |
| CN103203212A (en) | Preparation method and application of polymeric phosphorus ferric aluminum sulfate flocculating agent | |
| CN103880211B (en) | A kind of recycling treatment process containing magnesium high-salt wastewater | |
| CN104403064B (en) | Ultraviolet initiation prepares method and the application of PAMC | |
| CN114212921B (en) | Treatment method of landfill leachate | |
| CN103274578B (en) | Surplus sludge dewatering method for aerobic granular sludge reactor | |
| CN106554140B (en) | A kind of residual active sludge cracks decrement method | |
| CN110342624A (en) | A kind of preparation method of oxidisability organic polymer coargulator | |
| CN103449535A (en) | Production method for solid polyferric sulphate | |
| CN108083400A (en) | A kind of preparation method of phosphorous polyiron sulfate and its application for handling coking wastewater | |
| CN103964554B (en) | Polyaluminum sulfate titanium-polydimethyldiallylachloride chloride composite coagulant and preparation and application method thereof | |
| CN103848933B (en) | A kind of preparation method of flocculation agent and application thereof | |
| CN109956648B (en) | Method for dewatering waste drilling mud based on Fenton oxidation instability and scale adsorption weighting coupling | |
| CN116675318A (en) | Preparation method of flocculant for oily wastewater treatment | |
| CN105254067A (en) | Resource utilization method for advanced wastewater treatment Fenton method sludge | |
| CN102633937A (en) | Preparation and application of diallyl dimethyl ammonium chloride and acrylamide copolymer | |
| CN103833118A (en) | Preparation method of polyaluminium chloride coagulant | |
| CN114436500A (en) | Functional composite flocculant for sludge and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| CB03 | Change of inventor or designer information | ||
| CB03 | Change of inventor or designer information |
Inventor after: Zhang Peng Inventor after: Liao Weixiong Inventor after: Ren Bozhi Inventor after: Zhu Guocheng Inventor after: Zhang Yanjun Inventor after: Zhang Wei Inventor after: Ding Wenjie Inventor before: Zhang Peng Inventor before: Ren Bozhi Inventor before: Zhu Guocheng Inventor before: Zhang Yanjuan Inventor before: Zhang Wei Inventor before: Ding Wenjie |
|
| GR01 | Patent grant | ||
| GR01 | Patent grant |