CN107501443B - A kind of preparation method of magnetic hydrophobic modified cation polyacrylamide oil removing flocculant - Google Patents
A kind of preparation method of magnetic hydrophobic modified cation polyacrylamide oil removing flocculant Download PDFInfo
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- CN107501443B CN107501443B CN201710872400.5A CN201710872400A CN107501443B CN 107501443 B CN107501443 B CN 107501443B CN 201710872400 A CN201710872400 A CN 201710872400A CN 107501443 B CN107501443 B CN 107501443B
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- 229920002401 polyacrylamide Polymers 0.000 title claims abstract description 35
- 150000001768 cations Chemical class 0.000 title claims abstract description 34
- 230000002209 hydrophobic effect Effects 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000000178 monomer Substances 0.000 claims abstract description 22
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000000843 powder Substances 0.000 claims abstract description 16
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 12
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 11
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910021642 ultra pure water Inorganic materials 0.000 claims abstract description 9
- 239000012498 ultrapure water Substances 0.000 claims abstract description 9
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims abstract description 8
- 235000014113 dietary fatty acids Nutrition 0.000 claims abstract description 8
- GQOKIYDTHHZSCJ-UHFFFAOYSA-M dimethyl-bis(prop-2-enyl)azanium;chloride Chemical compound [Cl-].C=CC[N+](C)(C)CC=C GQOKIYDTHHZSCJ-UHFFFAOYSA-M 0.000 claims abstract description 8
- 239000000194 fatty acid Substances 0.000 claims abstract description 8
- 229930195729 fatty acid Natural products 0.000 claims abstract description 8
- 150000004665 fatty acids Chemical class 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 235000013162 Cocos nucifera Nutrition 0.000 claims abstract description 6
- 244000060011 Cocos nucifera Species 0.000 claims abstract description 6
- 238000005286 illumination Methods 0.000 claims abstract description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 6
- 238000010521 absorption reaction Methods 0.000 claims abstract description 5
- 239000002351 wastewater Substances 0.000 claims description 15
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- 238000005189 flocculation Methods 0.000 claims description 9
- 230000016615 flocculation Effects 0.000 claims description 8
- -1 polypropylene Polymers 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 7
- 239000008187 granular material Substances 0.000 claims description 6
- KWOLFJPFCHCOCG-UHFFFAOYSA-N Acetophenone Natural products CC(=O)C1=CC=CC=C1 KWOLFJPFCHCOCG-UHFFFAOYSA-N 0.000 claims description 5
- 239000012901 Milli-Q water Substances 0.000 claims description 5
- 239000004743 Polypropylene Substances 0.000 claims description 5
- 150000001408 amides Chemical class 0.000 claims description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 5
- 239000001301 oxygen Substances 0.000 claims description 5
- 229910052760 oxygen Inorganic materials 0.000 claims description 5
- 229920001155 polypropylene Polymers 0.000 claims description 5
- 238000007789 sealing Methods 0.000 claims description 5
- 125000002091 cationic group Chemical group 0.000 claims description 4
- 239000003999 initiator Substances 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 238000012545 processing Methods 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 230000003311 flocculating effect Effects 0.000 claims 1
- 238000005303 weighing Methods 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 10
- 239000000126 substance Substances 0.000 abstract description 9
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 abstract description 8
- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 abstract description 8
- 230000000295 complement effect Effects 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 3
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 abstract description 3
- 239000002245 particle Substances 0.000 abstract description 3
- 238000009833 condensation Methods 0.000 abstract description 2
- 230000005494 condensation Effects 0.000 abstract description 2
- 238000000227 grinding Methods 0.000 abstract description 2
- 239000000084 colloidal system Substances 0.000 abstract 1
- 238000001816 cooling Methods 0.000 abstract 1
- 230000005669 field effect Effects 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- 230000010148 water-pollination Effects 0.000 abstract 1
- 239000003921 oil Substances 0.000 description 34
- 235000019198 oils Nutrition 0.000 description 34
- 239000000243 solution Substances 0.000 description 8
- 238000005345 coagulation Methods 0.000 description 7
- 230000015271 coagulation Effects 0.000 description 7
- 238000001514 detection method Methods 0.000 description 7
- 238000004458 analytical method Methods 0.000 description 6
- 239000000839 emulsion Substances 0.000 description 6
- 238000004062 sedimentation Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 238000011161 development Methods 0.000 description 4
- 238000004090 dissolution Methods 0.000 description 4
- 235000015110 jellies Nutrition 0.000 description 4
- 239000008274 jelly Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 239000004094 surface-active agent Substances 0.000 description 4
- 238000013019 agitation Methods 0.000 description 3
- 125000000217 alkyl group Chemical group 0.000 description 3
- 239000012153 distilled water Substances 0.000 description 3
- 238000011010 flushing procedure Methods 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000002105 nanoparticle Substances 0.000 description 3
- 229920000620 organic polymer Polymers 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000010189 synthetic method Methods 0.000 description 3
- 150000001412 amines Chemical group 0.000 description 2
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 description 2
- 235000019864 coconut oil Nutrition 0.000 description 2
- 239000003240 coconut oil Substances 0.000 description 2
- 238000007334 copolymerization reaction Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000004945 emulsification Methods 0.000 description 2
- 238000004134 energy conservation Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 230000000977 initiatory effect Effects 0.000 description 2
- 230000005389 magnetism Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 1
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 240000002853 Nelumbo nucifera Species 0.000 description 1
- 235000006508 Nelumbo nucifera Nutrition 0.000 description 1
- 235000006510 Nelumbo pentapetala Nutrition 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 125000002252 acyl group Chemical group 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000011953 bioanalysis Methods 0.000 description 1
- 238000004581 coalescence Methods 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 239000006071 cream Substances 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 239000003651 drinking water Substances 0.000 description 1
- 235000020188 drinking water Nutrition 0.000 description 1
- 230000002500 effect on skin Effects 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 239000003673 groundwater Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 235000013336 milk Nutrition 0.000 description 1
- 239000008267 milk Substances 0.000 description 1
- 210000004080 milk Anatomy 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- DCKVNWZUADLDEH-UHFFFAOYSA-N sec-butyl acetate Chemical compound CCC(C)OC(C)=O DCKVNWZUADLDEH-UHFFFAOYSA-N 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 230000032258 transport Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F8/00—Chemical modification by after-treatment
- C08F8/42—Introducing metal atoms or metal-containing groups
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/46—Polymerisation initiated by wave energy or particle radiation
- C08F2/48—Polymerisation initiated by wave energy or particle radiation by ultraviolet or visible light
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/56—Acrylamide; Methacrylamide
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Medicinal Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Polymers & Plastics (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Engineering & Computer Science (AREA)
- Hydrology & Water Resources (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
Abstract
The present invention provides a kind of preparation methods of magnetic hydrophobic modified cation polyacrylamide oil removing flocculant, belong to environmentally friendly water-treatment technology field.Dodecyl heteroside (or cocoanut fatty acid diethanolamide), dimethyl diallyl ammonium chloride, acrylamide, photoinitiator are dissolved in the water by this method, adjust pH value, it is passed through nitrogen and seals reaction flask, it is placed in illumination polymerization under low pressure ultraviolet lamp again and generates lacteous colloid, it is re-dissolved in ultrapure water, magnetic nano ferroferric oxide particle and ammonium persulfate stirring are added, washing, dry, grinding finally obtain black powder oil removing flocculant.Polymerization time of the invention is short, reaction temperature is low, is not required to condensation cooling, energy-saving；The introducing of hydrophobic monomer reduces the hydrophily of flocculant, enhances the absorption property to oily substance, enhances flocculant demulsification ability；For the magnetic nano ferroferric oxide particle of introducing under complementary field effect, settling velocity is fast, easily separated.
Description
Technical field
The invention belongs to environmentally friendly water-treatment technology fields, and in particular to a kind of water-soluble magnetic organic polymer water process is removed
The preparation method of oil flocculant, in particular to a kind of preparation side of magnetic hydrophobic modified cation polyacrylamide oil removing flocculant
Method.
Background technique
With the development of industry, the usage amount of oil product is increasing, in the oil recovery of petroleum industry, oil refining, store oil, transports
A large amount of oily waste waters can be all generated in journey and the production process of petro chemical industry, lagging in development and management due to various technologies
Reasons perfect etc. not to the utmost make a large amount of oil products enter water body, form pollution, influence drinking water sources and groundwater resources, endanger water
Produce resource；Human health；Pollute atmosphere；Influence production estimation；Destroy natural landscape, or even it is also possible to the because oil of coalescence
Product burn and generate safety problem.Therefore oily waste water improvement is current environment protection field urgent problem.Wherein oil emulsion
Removal be key points and difficulties that oily waste water is administered, oil emulsion is that granularity is 0.1~3 μm of superfine oil droplet, due to grease circle
There is the presence of surfactant in face, is usually dispersed in water with oil-in-water form stable, is difficult to be removed.
Currently, the processing method of oily waste water specifically includes that floatation, flocculence, electromagnetic method, membrane separation process, bioanalysis
Deng.Wherein, flocculence is since its is adaptable, can remove oil emulsion and dissolved oil and part is difficult to biodegrade complicated height
The characteristics of molecular organic and the processing for being widely used in oily waste water, and good growth momentum is presented.As the method exists
The research of application in oil removing process, novel de-oiling flocculant is increasing, in flocculant introduce hydrophobic monomer method by
Step development, if patent publication No. is a kind of " the preparation side of dewatered modified cation polyacrylamide flocculant CN103319652A
Method " is with acrylamide, acrylyl oxy-ethyl-trimethyl salmiac, butyl acrylate, perfluorooctylethyl group acrylate and table
Face activating agent hydrophobic synthetic flocculant of modified polyacrylamide；For another example patent publication No. is that " one kind is hydrophobic to be changed CN103319653A
Property cationic polyacrylamide flocculant agent preparation method " then use acrylamide, dimethyl diallyl ammonium chloride, acrylic acid
The hydrophobic synthetics modified polyacrylamide such as butyl ester and surfactant；For another example patent publication No. is CN106497599A " surface electricity
The preparation method and application of lotus and the controllable pH responsive type magnetism demulsifier of hydrophilic and hydrophobic " is by silicon dioxide carried to four oxidations three
On Fe nanometer particles, and surface active monomer and pH responsive type monomer acquisition demulsifier are introduced by graft copolymerization.It is above-mentioned
Method achieves certain effect, but still further improvement in need and development: 1) butyl acrylate as synthetic material not
Preferably a large amount of storages, are easy to produce secondary pollution, and be easy to happen autohemagglutination when the temperature rises；2) use of surfactant improves
The cost of preparation；3) the polymerization preparation reaction temperature of traditional polyacrylamide flocculant can increase, and it is anti-that polymerization generates crosslinking
It answers, causes product solubility property poor；4) silicon dioxide carried and graft reaction, because of complicated component, reaction is difficult to control, and temperature
It need to adjust to 20~80 DEG C, energy consumption is high；5) organic polymer coargulator sedimentation effect in coagulation oil removing is bad, it is not easy to point
From, and selective oil removing ability is poor.
Summary of the invention
In view of the above shortcomings of the prior art, the present invention solves the easy autohemagglutination of hydrophobic monomer, traditional polymerization heat release
Greatly, temperature height, problem difficult to settle, and improvement conventional polypropylene amide adsorptivity is insufficient, dissolution time is long, can not recycle benefit
With the problems such as, provide that a kind of preparation process is simple, reaction condition is mild, energy conservation and environmental protection, the high adsorption for being easy to industrialization, quickly
The synthetic method of precipitability magnetic hydrophobic oleophylic modified cation polyacrylamide flocculant.
The present invention adopts the following technical scheme that realize: a kind of magnetic hydrophobic oleophylic modified cation polyacrylamide flocculation
The synthetic method of agent, comprising the following steps:
(1) the hydrophobic oleophilic oil monomer dodecyl that mass fraction (ratio for accounting for monomer gross mass) is 20%~30% is weighed
Heteroside (or cocoanut fatty acid diethanolamide), 20%~40% cationic monomer diallyldimethylammonChloride Chloride and
40%~60% acrylamide is added in wide-mouth bottle, stirs after adding a certain amount of deionized water to being completely dissolved, adds light
Initiator adjusts pH to 5~9 to being completely dissolved to obtain mixed liquor.
(2) Xiang Shangshu mixed liquor leads to oxygen in nitrogen certain time to wide-mouth bottle and is emptied completely, at room temperature by bottle sealing
It is placed under low pressure UV fluorescent tube illumination 1h and opalescent colloidal is obtained by polymerization reaction, jelly is used in cable type extractor according
Acetone purifies 48h, obtains white solid sample, as dewatered modified cation polyacrylamide.
(3) white pigmented samples after will be purified are dissolved in ultrapure water, are added at 30 DEG C~40 DEG C in thermostat water bath
With dewatered modified cation polyacrylamide mass ratio be 1:(1~3) nano ferriferrous oxide granule and suitable initiation
Agent ammonium persulfate, high-speed stirred 12h, obtains dark solution, dries grinding after using milli-Q water 3~5 times under magnet absorption
Black powder, as magnetic hydrophobic modified cation polyacrylamide flocculant are obtained at powder.
In the second step and second step, the ultraviolet light that polymerization reaction uses is produced by power for the low pressure mercury lamp of 10W-100W
It is raw, and the ultraviolet light dominant wavelength generated is 253.7nm or 185nm.The ultraviolet light of the wavelength has enough penetration powers, release
Energy can accelerate the fracture of chemical bond in monomer, shorten and cause the time, and calorific value is small, and temperature of reaction system increases unknown
It is aobvious, and energy conservation and environmental protection, practical safety.In the second step, photoinitiator used in polymerization reaction is 2- hydroxyl -4'- (2- hydroxyl
Ethyoxyl) -2- methyl phenyl ketone, above-mentioned initiator amount is low, efficiency of initiation is high, nontoxic.In the second step, polymerization is anti-
It should be at 2~20 DEG C at room temperature by ultraviolet light-initiated.In the third step, use ammonium persulfate as initiator, it will be magnetic
On nano-particles reinforcement to macromolecule organic, process is simple, easy to operate, easily separated.
Magnetic hydrophobic modified cation polyacrylamide oil removing flocculant obtained above can be at oily waste water flocculation
It is applied in reason.Especially when oily waste water concentration is 100~300mg/L, elaioleucite is having a size of 0.5~3 μm, deoiling effect is more
It is significant.
Compared with prior art, the present invention has following beneficial effect:
1, dodecyl heteroside has been widely used in cosmetic industry, and price is cheap, easily obtains, on strand
The chain alkyl structure contained has good adsorptivity to oily substance, it equally has good associativity in aqueous solution
Can, and the C-O-C structure on its molecule can effectively destroy the emulsifying film of oil-water interfaces, discharge the oils object in emulsified oil droplet
Matter；Cocoanut fatty acid diethanolamide also belongs to chain alkyl structure, and oleophylic is functional.Therefore, in cation polypropylene
Dodecyl heteroside (or cocoanut fatty acid diethanolamide) is introduced on amide long-chain improves polyacrylamide flocculant
Absorption emulsive oily energy so that modified flocculant have both breaking milk and removing oil ability and association ability of aggregation；And copolymerization sun
Ion monomer dimethyl diallyl ammonium chloride positive charge density is big, has strong charge neutrality absorption property.
2, magnetic ferroferric oxide nanoparticle is combined in organic polymer coargulator, it can be in the item of externally-applied magnetic field
Under part, it is separated by solid-liquid separation performance when improving flocculation treatment, can selectively assemble wadding body, to reduce hydraulic detention time.And
Nanoscale particle has quantum size effect, skin effect and macro quanta tunnel effect, using it to cation polypropylene
Amide surface is modified, and can effectively improve flocculant flocculation efficiency；In flocculation process under hydraulic mixing state, nanometer four
Fe 3 O is different from the tangential revolving speed of oil emulsion, and physical shear is caused to play demulsification, further increases oil removal efficiency.It uses
Magnetic hydrophobic modified cation polyacrylamide flocculant measures 3~5min of sedimentation separation time by experiment, and use is free of
Magnetic dewatered modified cation polyacrylamide flocculant, sedimentation separation time then need 20~30min.
3, there is good removal effect to oily substance.Dodecyl heteroside (or coco-nut oil fatty acid diethanol acyl
Amine) ehter bond in molecule or amido bond can abolish the oil-water interfaces of oil emulsion, and itself can displace oil-water interfaces
Natural surfactant, release is emulsified the oils of film package, the in addition positive charge of the quaternary amines institute band of cationic monomer
The negative electricity sublayer that oil emulsion outer layer covers can be destroyed, to reach demulsification；Hydrophobic chain alkyl can be effective close attached
The oily substance being released, is applied in oily waste water, has selectivity well and specificity.By experiment pair
Than using magnetic hydrophobic modified cation polyacrylamide flocculant, the turbidity removal rate for measuring oily waste water reaches 93.85%
~98.08%, emulsification oil content removal rate reaches 78.83%~85.22%；And use the cation polypropylene acyl of same monomer
Amine flocculant (non-hydrophobically modified is free of magnetism), the turbidity removal rate for measuring oily waste water reach 81.37%~87.42%, cream
Carburetion content removal rate reaches 56.47%~69.24%.
4, low pressure UV causes polymerization and can cause at room temperature, and temperature will not be significantly raised in reaction process.Such as
At 20 DEG C of room temperature, increase slowly through temperature in detection reaction process, up to 30 DEG C~36 DEG C, far below tradition heat
Cause or ultraviolet light-initiated 50 DEG C~80 DEG C of high pressure；If room temperature is lower, temperature reaches in reaction process maximum temperature
It can reduce.Therefore it does not need to carry out control condensation to temperature, simplifies operating procedure, and mild condition, easily controllable, energy-saving ring
It protects, is more suitable for industrialized production.
5, (or the coco-nut oil fatty acid of acrylamide, dodecyl heteroside selected by synthetic method provided by the present invention
Diglycollic amide), dimethyl diallyl ammonium chloride, nano ferriferrous oxide, ammonium persulfate be the commercially available material being easily obtained
Material, it is cheap, and small-power low pressure ultraviolet lamp saves energy consumption, whole production cost is low；Product is environmentally friendly, can be recycled, no
Secondary pollution can be generated.
Specific embodiment
It elaborates below by specific embodiment to the present invention, but the present invention is not limited to following embodiments.
Embodiment 1
(1) taking mass fraction (ratio for accounting for monomer gross mass) is 20% dodecyl heteroside, 20% dimethyl
Diallyl ammonium chloride and 60% acrylamide are dissolved in ultrapure water under magnetic agitation, it is backward to reach the state being completely dissolved
Photoinitiator 2- hydroxyl -4'- (2- hydroxy ethoxy) -2- methyl phenyl ketone that mass fraction is 1 ‰ is added in solution, stirring makes it
Be completely dissolved, adjustment pH be 9, after be passed through purity be 99.999% 15 minutes expeling oxygen of nitrogen, in 15 DEG C of room temperature condition
Lower bottle sealing is placed under the low pressure ultraviolet lamp that power is 20W, wavelength is 253.7nm after illumination 1h obtains milky glue
Object.
(2) jelly is wrapped in after acetone soln purifies for 24 hours in cable type extractor according with filter paper, with distilled water flushing,
Drying for 24 hours, is ground up, sieved to obtain white powder sample at 105 DEG C.By analysis with detection, finally obtained dredge is measured
The inherent viscosity of water modified cation polyacrylamide is 747mLg-1, positive charge density 20.1mmolg-1, when dissolution
Between be 60min.
(3) above-mentioned powder is taken and is dissolved in ultrapure water in right amount, is added and dewatered modified cation polyacrylamide quality
Than for 1:1 nano ferriferrous oxide granule and mass fraction (ratio for accounting for monomer gross mass) be 0.1% ammonium persulfate, it is high
Dark solution is obtained after speed stirring 12h, is used milli-Q water 3 times in complementary field, it is hydrophobic that drying obtains black magnetic
Modified cation Polyacrylamide Powder.
(4) taking 1L concentration is that the emulsification oil solution of 100mg/L is placed in coagulation stirrer, and above-mentioned black powder is added
0.12g can remove the oily substance in water after coagulation is stirred.By analysis with detection, magnetic flocculation sedimentation time 3min, place
Supernatant fluid turbidity after reason reduces 93.85%, and oil content reduces 88.22%.
Embodiment 2
(1) taking mass fraction (ratio for accounting for monomer gross mass) is 20% dodecyl heteroside, 40% dimethyl
Diallyl ammonium chloride and 40% acrylamide are dissolved in ultrapure water under magnetic agitation, it is backward to reach the state being completely dissolved
Photoinitiator 2- hydroxyl -4'- (2- hydroxy ethoxy) -2- methyl phenyl ketone that mass fraction is 1 ‰ is added in solution, stirring makes it
Be completely dissolved, adjustment pH be 7, after be passed through purity be 99.999% 15 minutes expeling oxygen of nitrogen, in 20 DEG C of room temperature condition
Lower bottle sealing is placed under the low pressure ultraviolet lamp that power is 40W, wavelength is 253.7nm after illumination 2h obtains milky glue
Object.
(2) jelly is wrapped in after acetone soln purifies for 24 hours in cable type extractor according with filter paper, with distilled water flushing,
Drying for 24 hours, is ground up, sieved to obtain white powder sample at 105 DEG C.By analysis with detection, finally obtained dredge is measured
The inherent viscosity of water modified cation polyacrylamide is 572mLg-1, positive charge density 42.6mmolg-1, when dissolution
Between be 55min.
(3) above-mentioned powder is taken and is dissolved in ultrapure water in right amount, is added and dewatered modified cation polyacrylamide quality
Than for 1:1.5 nano ferriferrous oxide granule and mass fraction (ratio for accounting for monomer gross mass) be 0.3% ammonium persulfate,
Dark solution is obtained after high-speed stirred 12h, is used milli-Q water 4 times in complementary field, drying obtains black magnetic and dredges
Water modified cation Polyacrylamide Powder.
(4) taking 1L concentration is that the emulsifiable oil waste water of 200mg/L is placed in coagulation stirrer, and above-mentioned black powder is added
0.15g can remove the oily substance in water after coagulation is stirred.By analysis with detection, magnetic flocculation sedimentation time 4min, place
Liquid turbidity after reason reduces 98.08%, and oil content reduces 86.52%,.
Embodiment 3
(1) cocoanut fatty acid diethanolamide, 20% that mass fraction (ratio for accounting for monomer gross mass) is 30% are taken
Dimethyl diallyl ammonium chloride and 50% acrylamide, be dissolved in ultrapure water under magnetic agitation, reach and be completely dissolved
Photoinitiator 2- hydroxyl -4'- (2- hydroxy ethoxy) -2- methyl phenyl ketone that mass fraction is 1 ‰ is added after state into solution,
Stirring makes it completely dissolved, adjustment pH be 5, after be passed through purity be 99.999% 15 minutes expeling oxygen of nitrogen, 2 DEG C of room
Bottle sealing is placed under the low pressure ultraviolet lamp that power is 80W, wavelength is 185nm under the conditions of temperature and obtains milky white coloring agent after illumination 3h
Shape object.
(2) jelly is wrapped in after acetone soln purifies for 24 hours in cable type extractor according with filter paper, with distilled water flushing,
Drying for 24 hours, is ground up, sieved to obtain white powder sample at 105 DEG C.By analysis with detection, finally obtained dredge is measured
The inherent viscosity of water modified cation polyacrylamide is 600mLg-1, positive charge density 21.2mmolg-1, when dissolution
Between be 65min.
(3) above-mentioned powder is taken and is dissolved in ultrapure water in right amount, is added and dewatered modified cation polyacrylamide quality
Than for 1:3 nano ferriferrous oxide granule and mass fraction (ratio for accounting for monomer gross mass) be 0.5% ammonium persulfate, it is high
Dark solution is obtained after speed stirring 12h, is used milli-Q water 3 times in complementary field, it is hydrophobic that drying obtains black magnetic
Modified cation Polyacrylamide Powder.
(4) taking 1L concentration is that the emulsifiable oil waste water of 200mg/L is placed in coagulation stirrer, and above-mentioned black powder is added
0.13g can remove the oily substance in water after coagulation is stirred.By analysis with detection, magnetic flocculation sedimentation time 5min, place
Liquid turbidity after reason reduces 95.79%, and oil content reduces 78.03%.
Claims (4)
1. a kind of preparation method of magnetic hydrophobic modified cation polyacrylamide oil removing flocculant, which is characterized in that the side
Method the following steps are included:
(1) weighing and accounting for monomer gross mass ratio is 20%~30% hydrophobic oleophilic oil monomer, 20%~40% cationic monomer
Dimethyl diallyl ammonium chloride and 40%~60% acrylamide are added in wide-mouth bottle, and stirring is to complete after deionized water is added
Fully dissolved adds photoinitiator to being completely dissolved to obtain mixed liquor, and adjusts pH to 5~9；
(2) Xiang Shangshu mixed liquor leads to oxygen in nitrogen to wide-mouth bottle and is emptied completely, and it is ultraviolet that bottle sealing is placed in low pressure at room temperature
1~3h of illumination obtains opalescent colloidal by polymerization reaction under light lamp tube, and opalescent colloidal is used acetone in cable type extractor according
24~48h is purified, white solid, i.e. dewatered modified cation polyacrylamide are obtained；
(3) dewatered modified cation polyacrylamide of the step (2) after purified is dissolved in ultrapure water, in thermostat water bath
In be added nano ferriferrous oxide granule and initiator ammonium persulfate at 30 DEG C~40 DEG C, high-speed stirred time 12~for 24 hours, obtain
Dark solution, under magnet absorption with milli-Q water 3~5 times after drying pulverize to obtain black powder, it is as magnetic to dredge
Water modified cation polyacrylamide oil removing flocculant；The nano ferriferrous oxide granule and dewatered modified cation polypropylene
Amide mass ratio is 1:1~3；
Hydrophobic oleophilic oil monomer in the step (1) is lauryl glucosyl or cocoanut fatty acid diethanolamide；Institute
The low pressure UV lamp power for stating in step (2) is 10~100W, wavelength is 253.7nm or 185nm；In the step (2)
Room temperature is 2~20 DEG C.
2. the preparation method of magnetic hydrophobic modified cation polyacrylamide oil removing flocculant as described in claim 1, feature
It is, the photoinitiator in the step (1) is 2- hydroxyl -4'- (2- hydroxy ethoxy) -2- methyl phenyl ketone.
3. the magnetic hydrophobic modified cation polyacrylamide oil removing flocculant that preparation method as described in claim 1 obtains is containing
Application in oily waste water flocculating processing.
4. magnetic hydrophobic modified cation polyacrylamide oil removing flocculant as claimed in claim 3 is in oily waste water flocculation treatment
In application, which is characterized in that the oily waste water concentration is 100~300mg/L, elaioleucite is having a size of 0.5~3 μm.
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