CN106430503A - Preparation method of cationic flocculant - Google Patents
Preparation method of cationic flocculant Download PDFInfo
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- CN106430503A CN106430503A CN201611077108.6A CN201611077108A CN106430503A CN 106430503 A CN106430503 A CN 106430503A CN 201611077108 A CN201611077108 A CN 201611077108A CN 106430503 A CN106430503 A CN 106430503A
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- Prior art keywords
- cationic
- ammonium
- allyl
- cationic flocculant
- flocculant
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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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
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- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
Abstract
The invention provides cationic flocculant and a preparation method thereof. The cationic flocculant is prepared from acrylamide, cationic monomer, hydrophobic monomer, photoinitiator 784 and adjuvant through polyreaction under the action of sunlight, wherein the cationic monomer comprises one of or a mixture of acryloyl yloxyethyl alkyl quaternary ammonium salts and/or allyl alkyl quaternary ammonium salts; the hydrophobic monomer comprises one of or a mixture of styrene, acrylonitrile, ethyl acetate, vinyl trimethoxy silane, vinyltriethoxysilane and acrylate; the adjuvant comprises one of or a mixture of azodiisobutyronitrile, azobisisoheptonitrile, 2,2'-azobis [2-methylpropionamidine] dihydrochloride, cyclohexanone peroxide, benzoperoxide and persulfate. The flocculant can adsorb anionic organic substances, has good affinity with uncharged organic substances or organic substances with a small amount of anion and has excellent flocculation and precipitation effects.
Description
Technical field
The present invention relates to a kind of cationic flocculant preparation method, and in particular to a kind of light-initiated synthesis of polyacrylamide
Method, is more particularly to polymerization under a kind of daylight of polyacrylamide.
Background technology
Cationic-type polyacrylamide（PHP）Class flocculant is widely used in dirt with its excellent performance and environmental friendliness
Water process.PHP has flocculation, thickening concurrently, drops the performances such as resistive, dispersibility, is widely used in oil recovery, ore dressing, coal washing, metallurgy, change
The performances such as work, papermaking, environmental protection.Especially in the process of pharmaceutical industry pharmaceutical wastewater, there is irreplaceable effect.
The synthetic method of polyacrylamide has：Aqueous solution homogeneous polymerization, dispersion phase-polymerization, light initiation polymerization etc., typically adopt
Caused with chemical initiator and be polymerized, its technical maturity, have the production history of more than 30 year.But these methods are also defective, mainly
Be that product quality is understable, and production cost be higher etc., have impact on PHP as flocculant widely using in terms of environmental protection.
Light polymerization method synthesizing cationic polyacrylamide has building-up process environmentally safe, synthesis mode environmental protection section
Can, the experiment condition of synthesis is simple, and process is easy to operate, the advantages of low production cost.With chemistry initiation system or composite initiation
System compares, and while certain intrinsic viscosity is ensured, can more improve the cationic degree of polymer, gathers so as to play its cation
Good characteristic of the acrylamide in sewage disposal.
Commonly use at present uv photopolymerization there are problems of poor stability, and visible ray can then solve above-mentioned asking
Topic, this patent selects the light trigger 784 for having preferable absorption in 400-760nm, in the sunlight synthesizing cationic flocculant.
Content of the invention
For solve uv-light polymerization presence technical problem, it is an object of the invention to provide a kind of visible ray sun from
The synthetic method of sub- flocculant, the method process is easy to operate, substantially reduces production cost.
For reaching above-mentioned purpose, the invention provides a kind of cationic flocculant, the cationic flocculant passes through propylene
Amide, cationic monomer, hydrophobic monomer, light trigger 784 and auxiliary agent carry out polyreaction in the presence of daylight and obtain；With
The following component of mass fraction meter：
100 weight portion of acrylamide
50～500 weight portion of cationic monomer
10～100 weight portion of hydrophobic monomer
784 1～10 weight portion of light trigger
5～20 weight portion of auxiliary agent
The cationic monomer includes acrylyl oxy-ethyl alkyl quaternary ammonium saltss and/or the one kind or several in allyl alkyl quaternary ammonium salt
The combination that plants；
The hydrophobic monomer includes styrene, acrylonitrile, Methane Carboxylic Acid ester, vinyltrimethoxy silane, three second of vinyl
TMOS, the combination of one or more of acrylate apoplexy due to endogenous wind；
The auxiliary agent include azodiisobutyronitrile, 2,2'-Azobis(2,4-dimethylvaleronitrile), azo diisobutyl amidine hydrochlorate, cyclohexanone peroxide,
One or more combination in benzoyl peroxide, persulfate.
Light trigger 784（Tetrafluoro diphenyl titanocenes）There is very wide absorption region, its effective absorption peak is 390,
460nm, absorbed to 500nm always or so, sensitive volume width, and can be used for visible ray photocuring system, and make with photobleaching
With.Light color systems are can be not only used for, can be used for dark system again, thus can be used for UV coating, UV ink, UV binding agent, photic anti-
Erosion agent, photopolymerization printing plate, composite, tooth inserts etc..Can be used alone or use cooperatively with other light triggers.It is based on
784 above feature, the light trigger in the inventive method selects 784（Tetrafluoro diphenyl titanocenes）.
In above-mentioned cationic flocculant, it is preferable that the acrylyl oxy-ethyl alkyl quaternary ammonium saltss include acryloyl-oxy second
Base trimethyl ammonium chloride, acrylyl oxy-ethyl-trimethyl ammonium bromide, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, metering system
The combination of one or more in acyloxyethyl trimethylammonium bromide.
In above-mentioned cationic flocculant, it is preferable that the allyl alkyl quaternary ammonium salt includes pi-allyl trimethyl ammonia chloride
Ammonium, pi-allyl trimethylammonium bromide, dimethyl diallyl ammonium chloride, dimethyl diallyl ammonium bromide, dimethyl
Base allyl ammonium chloride, dodecyl dimethyl allylic bromination ammonium, dodecyldimethylamine base allyl ammonium chloride, myristyl
Dimethyl-allyl ammonium bromide, hexadecyldimethyl benzyl ammonium allyl ammonium chloride, hexadecyldimethyl benzyl ammonium allylic bromination ammonium, 18
The combination of one or more in alkyl dimethyl allyl ammonium chloride, octadecyldimethyl allylic bromination ammonium.
The invention provides a kind of preparation method of above-mentioned cationic flocculant, the method is included acrylamide and reaction
Monomer is polymerized in the presence of light trigger 784 and auxiliary agent in the sunlight, and the response time is 4-12h.
In above-mentioned preparation method, it is preferable that the light initiating polymerizing reaction is comprised the following steps：
Step one, in a transparent reaction container, acrylamide, cationic monomer and hydrophobic monomer is added, add solvent to be made into
The additional proportion of the solution of desired concn, wherein acrylamide and cationic monomer is 1：0.5～1：5.
Step 2, add a certain amount of auxiliary agent and light trigger 784 in transparent reaction container in batches, and be filled with nitrogen
More than 30min, drives sealing preserve after oxygen.
Step 3, will be equipped with the transparent reaction of acrylamide, cationic monomer, hydrophobic monomer, light trigger and auxiliary agent
Container is placed and reacts 4-12h in the sunlight, obtains cationic flocculant, and the solid content of the flocculant is 20～60%.
With respect to prior art, the beneficial effects of the present invention is：
（1）The present invention simplifies the control of reaction condition by synthesizing cationic flocculant in the sunlight, and process is easy to operate, greatly
Flocculant synthesis cost is reduced greatly.While certain intrinsic viscosity is ensured, the cationic degree of polymer can be more improved, from
And play good characteristic of its PAMC in sewage disposal.
（2）The cationic flocculant that the present invention is provided not only contains substantial amounts of cation group, and dredges containing substantial amounts of
Water base group, cation group can will carry the material of a large amount of aniones by electrostatic attraction effect（Such as reactive dye and acid
Property dyestuff）Absorb, and hydrophobic group can pass through heat resistance and salt tolerance will be not charged or with the organic of a small amount of anion
Thing rapid aggregation is insoluble flco；Therefore compared with traditional cationic flocculant, the cation flocculation that the present invention is provided
Not only flocculation rate is fast for agent, and flocculating effect is more thorough.
Description of the drawings
Fig. 1 is the building-up process of cationic flocculant.
Specific embodiment
The invention will be further described below.
（One）The preparation of cationic flocculant
Embodiment 1
Present embodiments provide a kind of cationic flocculant.The raw material composition of the cationic flocculant is as shown in table 1.
The raw material composition of 1 cationic flocculant of table
The preparation method of the cationic flocculant is comprised the following steps：
80ml ethanol and all monomers is added in there-necked flask（Acrylamide, hydrophobic monomer and cationic monomer）, stirring
Mix homogeneously, and 0.9g light trigger 784 and 0.2g azodiisobutyronitrile is added, seal after being filled with nitrogen 30min, in the sunlight
Reaction 12h.Reaction obtains cationic flocculant after terminating.
Embodiment 2
Present embodiments provide a kind of cationic flocculant.The raw material composition of the cationic flocculant is as shown in table 2.
The raw material composition of 2 cationic flocculant of table
The preparation method of the cationic flocculant is comprised the following steps：
80ml ethanol and all monomers is added in there-necked flask（Acrylamide, hydrophobic monomer and cationic monomer）, stirring
Mix homogeneously, and 0.9g light trigger 784 and 0.5g benzoyl peroxide is added, seal after being filled with nitrogen 30min, in the sunlight
Reaction 12h.Reaction obtains cationic flocculant after terminating.
Embodiment 3
Present embodiments provide a kind of cationic flocculant.The raw material composition of the cationic flocculant is as shown in table 3.
The raw material composition of 3 cationic flocculant of table
The preparation method of the cationic flocculant is comprised the following steps：
80ml ethanol, 20g acrylamide, 10g dodecyldimethylamine base allyl ammonium chloride, 40g first is added in there-necked flask
Base acrylyl oxy-ethyl-trimethyl salmiac, 12g vinylacetate, 8g n-octyl, are uniformly mixed, and add
0.7g light trigger 784 and 0.2g azo diisobutyl amidine hydrochlorate and 0.2g potassium peroxydisulfate, seal after being filled with nitrogen 30min,
12h is reacted in the sunlight.Reaction obtains cationic flocculant after terminating.
Embodiment 4
Present embodiments provide a kind of cationic flocculant.The raw material composition of the cationic flocculant is as shown in table 4.
The raw material composition of 4 cationic flocculant of table
The preparation method of the cationic flocculant is comprised the following steps：
80ml ethanol, 20g acrylamide, 25g dimethyl diallyl ammonium chloride, 20g dodecyl is added in there-necked flask
Dimethylallylammonium chloride, 7g n-butyl acrylate, 10g acrylic acid methyl ester., 4g n-propyl, are uniformly mixed,
And 1.2g light trigger 784,0.3g azo diisobutyl amidine hydrochlorate and 0.2g, sodium sulfite is added, after being filled with nitrogen 30min
Sealing, reacts 12h in the sunlight.Reaction obtains cationic flocculant after terminating.
（Two）The flocculating effect test of cationic flocculant：
Method of testing：Take the fermentation waste water of Pharmaceutical limited company of old name for the Arabian countries in the Middle East：Outer light is faint yellow, with the presence of canescence float,
There is pungent stench, whole water body has certain viscosity.The cationic flocculant that embodiment 1-4 is provided puts into fermentation respectively
Flocculation decoloration process is carried out in waste water.And with the turbidity of waste water solution and COD before and after national standard method test flocculant flocculation sediment
Content.Configure a certain amount of polyacrylamide solution（PAM）Equally put in fermentation waste water, as a comparison.Its result such as table 5
Shown.
From table 5 test result indicate that, as long as the cationic flocculant of the present invention and common flocculant PAM are to turbidity of wastewater
There is very high clearance, but PAM, to the COD in waste water substantially without clearance, the cationic flocculant of the present invention is to COD
There is good removal effect.
Claims (5)
1. a kind of cationic flocculant, the cationic flocculant passes through acrylamide, cationic monomer, hydrophobic monomer, light
Initiator 784 and auxiliary agent carry out polyreaction in the presence of daylight and obtain；Following component in terms of mass fraction：
100 weight portion of acrylamide
50～500 weight portion of cationic monomer
10～100 weight portion of hydrophobic monomer
784 1～10 weight portion of light trigger
5～20 weight portion of auxiliary agent
The cationic monomer includes acrylyl oxy-ethyl alkyl quaternary ammonium saltss and/or the one kind or several in allyl alkyl quaternary ammonium salt
The combination that plants；
The hydrophobic monomer includes styrene, acrylonitrile, Methane Carboxylic Acid ester, vinyltrimethoxy silane, three second of vinyl
TMOS, the combination of one or more of acrylate apoplexy due to endogenous wind；
The auxiliary agent include azodiisobutyronitrile, 2,2'-Azobis(2,4-dimethylvaleronitrile), azo diisobutyl amidine hydrochlorate, cyclohexanone peroxide,
One or more combination in benzoyl peroxide, persulfate.
2. cationic flocculant according to claim 1, wherein：The acrylyl oxy-ethyl alkyl quaternary ammonium saltss include propylene
Acyloxyethyl trimethyl ammonium chloride, acrylyl oxy-ethyl-trimethyl ammonium bromide, furniture acrylyl oxy-ethyl-trimethyl salmiac, first
The combination of one or more in base acrylyl oxy-ethyl-trimethyl ammonium bromide.
3. cationic flocculant according to claim 1 and 2, wherein：The allyl alkyl quaternary ammonium salt includes pi-allyl
Trimethyl ammonium chloride, pi-allyl trimethylammonium bromide, dimethyl diallyl ammonium chloride, dimethyl diallyl ammonium bromide, ten
Dialkyl dimethyl allyl ammonium chloride, dodecyl dimethyl allylic bromination ammonium, dodecyldimethylamine base pi-allyl chlorination
Ammonium, dodecyldimethylamine base allylic bromination ammonium, hexadecyldimethyl benzyl ammonium allyl ammonium chloride, hexadecyldimethyl benzyl ammonium pi-allyl
One or more in ammonium bromide, solution property, octadecyldimethyl allylic bromination ammonium
Combination.
4. the preparation method of the cationic flocculant described in a kind of any one of claim 1-3, the method is included acrylamide
With reaction monomers in the presence of light trigger 784 and auxiliary agent, it is polymerized in the sunlight, the response time is 4-12h.
5. preparation method according to claim 4, wherein：The light initiation polymerization is comprised the following steps：
Step one, in a transparent reaction container, acrylamide, cationic monomer and hydrophobic monomer is added, add solvent to be made into
The solution of desired concn；
Step 2, add a certain amount of auxiliary agent and light trigger 784 in transparent reaction container in batches, and be filled with nitrogen flooding oxygen
Sealing preserve afterwards；
Step 3, the transparent reaction container that will be equipped with acryloyl, cationic monomer, hydrophobic monomer, light trigger and auxiliary agent are put
Put and react in the sunlight.
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| CN201611077108.6A CN106430503A (en) | 2016-11-30 | 2016-11-30 | Preparation method of cationic flocculant |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108060609A (en) * | 2017-12-07 | 2018-05-22 | 常州帝君金属构件厂 | A kind of preparation method of the compound drying strengthening agent of high bond strength |
| CN108178266A (en) * | 2018-03-09 | 2018-06-19 | 王欣欣 | A kind of efficient sewage treatment flocculant and preparation method thereof |
| CN108559020A (en) * | 2018-05-09 | 2018-09-21 | 江南大学 | A kind of multiple copolymer, preparation method and its application in the treatment of waste water |
| CN109679036A (en) * | 2018-12-28 | 2019-04-26 | 厦门大学 | The preparation method and cationic high-molecular flocculant of a kind of cationic high-molecular polymer and its application |
| WO2019213868A1 (en) * | 2018-05-09 | 2019-11-14 | 江南大学 | Multi-copolymer, preparation method therefor and application thereof in wastewater treatment |
| CN110449138A (en) * | 2019-08-05 | 2019-11-15 | 江西师范大学 | A kind of preparation method of porous type polyquaternium gel adsorber |
| CN111363073A (en) * | 2019-11-14 | 2020-07-03 | 中国科学院化学研究所 | Amphiphilic polymer with anti-swelling and flocculation effects and preparation method and application thereof |
| CN112029033A (en) * | 2020-09-02 | 2020-12-04 | 中国石油天然气集团有限公司 | Nano-micron inferior solid-phase polymer flocculant for oil-based drilling fluid and preparation method of flocculant |
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2016
- 2016-11-30 CN CN201611077108.6A patent/CN106430503A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108060609A (en) * | 2017-12-07 | 2018-05-22 | 常州帝君金属构件厂 | A kind of preparation method of the compound drying strengthening agent of high bond strength |
| CN108178266A (en) * | 2018-03-09 | 2018-06-19 | 王欣欣 | A kind of efficient sewage treatment flocculant and preparation method thereof |
| CN108178266B (en) * | 2018-03-09 | 2020-08-11 | 湖南中测玉成环境科技有限公司 | Efficient sewage treatment flocculant and preparation method thereof |
| CN108559020A (en) * | 2018-05-09 | 2018-09-21 | 江南大学 | A kind of multiple copolymer, preparation method and its application in the treatment of waste water |
| CN108559020B (en) * | 2018-05-09 | 2019-05-03 | 江南大学 | A kind of multiple copolymer, preparation method and its application in the treatment of waste water |
| WO2019213868A1 (en) * | 2018-05-09 | 2019-11-14 | 江南大学 | Multi-copolymer, preparation method therefor and application thereof in wastewater treatment |
| US11365272B2 (en) * | 2018-05-09 | 2022-06-21 | Jiangnan University | Multi-copolymer, methods for producing the same and using thereof in wastewater treatment |
| CN109679036A (en) * | 2018-12-28 | 2019-04-26 | 厦门大学 | The preparation method and cationic high-molecular flocculant of a kind of cationic high-molecular polymer and its application |
| CN110449138A (en) * | 2019-08-05 | 2019-11-15 | 江西师范大学 | A kind of preparation method of porous type polyquaternium gel adsorber |
| CN111363073A (en) * | 2019-11-14 | 2020-07-03 | 中国科学院化学研究所 | Amphiphilic polymer with anti-swelling and flocculation effects and preparation method and application thereof |
| CN112029033A (en) * | 2020-09-02 | 2020-12-04 | 中国石油天然气集团有限公司 | Nano-micron inferior solid-phase polymer flocculant for oil-based drilling fluid and preparation method of flocculant |
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