CN115745464B - Flocculant and preparation method thereof - Google Patents
Flocculant and preparation method thereof Download PDFInfo
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- CN115745464B CN115745464B CN202211465856.7A CN202211465856A CN115745464B CN 115745464 B CN115745464 B CN 115745464B CN 202211465856 A CN202211465856 A CN 202211465856A CN 115745464 B CN115745464 B CN 115745464B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000002270 dispersing agent Substances 0.000 claims abstract description 36
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 18
- 239000012744 reinforcing agent Substances 0.000 claims abstract description 18
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims description 27
- 238000002156 mixing Methods 0.000 claims description 20
- 239000000047 product Substances 0.000 claims description 20
- 229920002472 Starch Polymers 0.000 claims description 16
- 235000019698 starch Nutrition 0.000 claims description 16
- 239000008107 starch Substances 0.000 claims description 16
- 238000001035 drying Methods 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 238000005406 washing Methods 0.000 claims description 13
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 9
- 229940048053 acrylate Drugs 0.000 claims description 9
- 229920006037 cross link polymer Polymers 0.000 claims description 7
- 229920005552 sodium lignosulfonate Polymers 0.000 claims description 7
- PQUXFUBNSYCQAL-UHFFFAOYSA-N 1-(2,3-difluorophenyl)ethanone Chemical compound CC(=O)C1=CC=CC(F)=C1F PQUXFUBNSYCQAL-UHFFFAOYSA-N 0.000 claims description 6
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 6
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 6
- 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 description 6
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 6
- 229940047670 sodium acrylate Drugs 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 239000003999 initiator Substances 0.000 claims description 5
- WFIZEGIEIOHZCP-UHFFFAOYSA-M potassium formate Chemical compound [K+].[O-]C=O WFIZEGIEIOHZCP-UHFFFAOYSA-M 0.000 claims description 5
- CBOCVOKPQGJKKJ-UHFFFAOYSA-L Calcium formate Chemical group [Ca+2].[O-]C=O.[O-]C=O CBOCVOKPQGJKKJ-UHFFFAOYSA-L 0.000 claims description 3
- 239000004280 Sodium formate Substances 0.000 claims description 3
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical group OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 3
- 235000019255 calcium formate Nutrition 0.000 claims description 3
- 229940044172 calcium formate Drugs 0.000 claims description 3
- 239000004281 calcium formate Substances 0.000 claims description 3
- INHCSSUBVCNVSK-UHFFFAOYSA-L lithium sulfate Inorganic materials [Li+].[Li+].[O-]S([O-])(=O)=O INHCSSUBVCNVSK-UHFFFAOYSA-L 0.000 claims description 3
- 239000002159 nanocrystal Chemical group 0.000 claims description 3
- 235000010333 potassium nitrate Nutrition 0.000 claims description 3
- 239000004323 potassium nitrate Substances 0.000 claims description 3
- HLBBKKJFGFRGMU-UHFFFAOYSA-M sodium formate Chemical compound [Na+].[O-]C=O HLBBKKJFGFRGMU-UHFFFAOYSA-M 0.000 claims description 3
- 235000019254 sodium formate Nutrition 0.000 claims description 3
- RBTVSNLYYIMMKS-UHFFFAOYSA-N tert-butyl 3-aminoazetidine-1-carboxylate;hydrochloride Chemical compound Cl.CC(C)(C)OC(=O)N1CC(N)C1 RBTVSNLYYIMMKS-UHFFFAOYSA-N 0.000 claims description 3
- 150000003385 sodium Chemical class 0.000 claims description 2
- 239000012265 solid product Substances 0.000 claims description 2
- 229920002401 polyacrylamide Polymers 0.000 abstract description 26
- 230000000694 effects Effects 0.000 abstract description 18
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 abstract description 17
- 229910000360 iron(III) sulfate Inorganic materials 0.000 abstract description 17
- 238000005189 flocculation Methods 0.000 abstract description 15
- 230000016615 flocculation Effects 0.000 abstract description 15
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 abstract description 12
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 abstract description 7
- PYGSKMBEVAICCR-UHFFFAOYSA-N hexa-1,5-diene Chemical group C=CCCC=C PYGSKMBEVAICCR-UHFFFAOYSA-N 0.000 abstract description 7
- 229920000867 polyelectrolyte Polymers 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- 238000006386 neutralization reaction Methods 0.000 abstract description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 12
- 239000004576 sand Substances 0.000 description 10
- 238000010438 heat treatment Methods 0.000 description 9
- 238000002835 absorbance Methods 0.000 description 8
- 239000004568 cement Substances 0.000 description 8
- 229920001577 copolymer Polymers 0.000 description 7
- 239000002351 wastewater Substances 0.000 description 7
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 description 6
- 239000012456 homogeneous solution Substances 0.000 description 6
- 229910052757 nitrogen Inorganic materials 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- PZNOBXVHZYGUEX-UHFFFAOYSA-N n-prop-2-enylprop-2-en-1-amine;hydrochloride Chemical compound Cl.C=CCNCC=C PZNOBXVHZYGUEX-UHFFFAOYSA-N 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 238000001179 sorption measurement Methods 0.000 description 5
- 239000007788 liquid Substances 0.000 description 4
- 239000006228 supernatant Substances 0.000 description 4
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 description 3
- 229910001870 ammonium persulfate Inorganic materials 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000000428 dust Substances 0.000 description 3
- 239000003623 enhancer Substances 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 230000000977 initiatory effect Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 230000035484 reaction time Effects 0.000 description 3
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 description 3
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 2
- 229920002126 Acrylic acid copolymer Polymers 0.000 description 2
- 239000005995 Aluminium silicate Substances 0.000 description 2
- 235000012211 aluminium silicate Nutrition 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000003638 chemical reducing agent Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000008394 flocculating agent Substances 0.000 description 2
- 230000003311 flocculating effect Effects 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 2
- 239000011344 liquid material Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 238000005381 potential energy Methods 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 239000000440 bentonite Substances 0.000 description 1
- 229910000278 bentonite Inorganic materials 0.000 description 1
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 description 1
- YDEXUEFDPVHGHE-GGMCWBHBSA-L disodium;(2r)-3-(2-hydroxy-3-methoxyphenyl)-2-[2-methoxy-4-(3-sulfonatopropyl)phenoxy]propane-1-sulfonate Chemical compound [Na+].[Na+].COC1=CC=CC(C[C@H](CS([O-])(=O)=O)OC=2C(=CC(CCCS([O-])(=O)=O)=CC=2)OC)=C1O YDEXUEFDPVHGHE-GGMCWBHBSA-L 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 229910052901 montmorillonite Inorganic materials 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 230000007306 turnover Effects 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- 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
- Y02W10/10—Biological treatment of water, waste water, or sewage
-
- 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
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
Abstract
The invention relates to a flocculant and a preparation method thereof, wherein the flocculant preparation raw material comprises 25-30 parts of polyacrylamide by weight; 8-12 parts of dimethyl diallyl ammonia chloride; 40-60 parts of polymeric ferric sulfate; 1-20 parts of dispersing agent; 1-10 parts of reinforcing agent; 1-10 parts of early strength agent. The polyacrylamide can make suspended substances have good flocculation effect through electric neutralization, the dimethyl diallyl ammonia chloride has obvious polyelectrolyte effect, the dimethyl diallyl ammonia chloride is added to reduce the viscosity along with the increase of the concentration, and the fluidity of the concrete is improved.
Description
Technical Field
The invention relates to the technical field of building additives, in particular to a flocculant and a preparation method thereof.
Background
The machine-made sand can generate a large amount of dust in the production process, and the dust is mixed in the machine-made sand to seriously damage the quality of the machine-made sand. In order to remove the dust, the machine-made sand needs to be washed, and in order to improve the turnover efficiency of the wastewater, a flocculating agent is added into the washed wastewater to accelerate the precipitation of silt particles.
When the machine-made sand added with the flocculant is applied to the pipe pile concrete, the strength of the pipe pile can be greatly reduced.
Disclosure of Invention
Based on this, it is necessary to provide a flocculant which has little influence on the strength of the pipe pile.
In order to achieve the above object, the present invention provides a technical solution:
the flocculant is prepared from the following raw materials in parts by weight:
wherein the first dispersant comprises a starch grafted acrylate modified co-cross-linked polymer.
Preferably, the flocculant further comprises 1-10 parts by weight of a reinforcing agent.
Preferably, the reinforcing agent includes at least one of calcium formate, triethanolamine, a nanocrystal core reinforcing agent, potassium nitrate, and lithium sulfate.
Preferably, the flocculant also comprises 1-10 parts of early strength agent in parts by weight.
Preferably, the early strength agent includes at least one of potassium formate and sodium formate.
Preferably, the flocculant further comprises 1-10 parts of a second dispersant, wherein the second dispersant comprises sodium lignosulfonate and acrylic acid copolymer derivatives.
The invention also provides a preparation method of the flocculant, which comprises the following steps:
and mixing the polyacrylamide, the polydimethyl diallyl ammonium chloride, the polymeric ferric sulfate and the first dispersing agent uniformly to obtain the flocculant.
Preferably, the preparation method of the first dispersing agent comprises the following steps:
mixing starch and water, and stirring and gelatinizing;
and after gelatinization, stirring and cooling, adding sodium acrylate and dimethyl diallyl ammonia chloride, dripping an initiator, reacting at constant temperature for 3-8 h, washing, drying and crushing the product to obtain a solid product.
Preferably, the specific steps of the preparation method of the flocculant comprise:
dissolving the polymeric ferric sulfate in water to obtain a polyacrylamide solution;
heating and stirring the polyacrylamide solution on a constant-temperature stirrer, adding the polydimethyldiallyl ammonia chloride, stirring and dispersing to a homogeneous solution, adding a first dispersing agent, uniformly mixing, drying at constant temperature, and crushing to obtain a dried product;
and uniformly mixing the dried product with the polyacrylamide, and adding an enhancer, an early strength agent and a second dispersant to obtain the flocculant.
Preferably, the temperature of the constant temperature drying and crushing is 70 ℃.
The invention has the beneficial effects that:
the flocculant is prepared from polyacrylamide, polydimethyl diallyl ammonium chloride, polymeric ferric sulfate and a first dispersing agent, wherein the first dispersing agent comprises a starch grafted acrylate modified copolymer cross-linked polymer. The polyacrylamide is a water-soluble linear high polymer formed by polymerization of acrylamide monomers initiated by free radicals, suspended substances can be subjected to electric neutralization and bridging adsorption, the water-soluble linear high polymer has good flocculation, the dimethyldiallylammonium chloride has a remarkable polyelectrolyte effect, the dimethyldiallylammonium chloride is added to enable the viscosity to be reduced along with the increase of the concentration, the fluidity of the tubular pile concrete is improved, on the other hand, the starch grafted acrylate modified copolymer cross-link can adjust the electronic potential energy distribution among cement particles, the surface activity of flocculant molecules is reduced, and meanwhile, the water reducer and slump retaining agent can be replaced by the preferential adsorption of the polyacrylamide due to the higher activity of the starch grafted acrylate modified copolymer, the plasticizing effect of the liquid is effectively improved, the viscosity of the concrete is reduced, and the fluidity of the concrete is improved. Along with the improvement of the fluidity of the tubular pile concrete, and the addition of the early strength agent and the reinforcing agent, the influence of flocculant residues on the strength of the tubular pile concrete can be obviously reduced.
Detailed Description
For a better description of the objects, technical solutions and advantages of the present invention, the present invention will be further described with reference to the following specific examples.
In the examples, the test methods used are conventional methods unless otherwise specified, and the materials, reagents, etc. used are commercially available.
The flocculant is prepared from the following raw materials in parts by weight:
wherein the first dispersant comprises a starch grafted acrylate modified co-cross-linked polymer.
Specifically, the molecular weight of polyacrylamide is 800 ten thousand.
In one embodiment, the flocculant further comprises 1 to 10 parts by weight of a reinforcing agent.
In one embodiment, the enhancer comprises at least one of calcium formate, triethanolamine, nanocrystal core enhancer, potassium nitrate, and lithium sulfate.
In one embodiment, the flocculant further comprises 1-10 parts by weight of an early strength agent.
In one embodiment, the early strength agent includes at least one of potassium formate and sodium formate.
In one embodiment, the flocculant further comprises 1-10 parts by weight of a second dispersant comprising a co-polymer derivative of sodium lignosulfonate and acrylic acid.
The flocculant is prepared from polyacrylamide, polydimethyl diallyl ammonium chloride, polymeric ferric sulfate and a first dispersing agent, wherein the first dispersing agent comprises a starch grafted acrylate modified copolymer cross-linked polymer.
When the flocculant prepared by the invention is used for concrete, polyacrylamide is a water-soluble linear high polymer prepared by polymerization of acrylamide monomers initiated by free radicals, so that suspended substances in the concrete can be neutralized electrically, and flocculating bodies are formed by bridging adsorption, so that the flocculant has good flocculation effect.
And after the polyacrylamide is added, the polyacrylamide can be loaded on the surfaces of the cement particles to form an adsorption film, so that the fluidity, the air entraining effect and the compressive strength of the concrete are reduced.
Further, in order to reduce the decrease in compressive strength caused by the addition of polyacrylamide to the flocculant, the present invention adds an early strength agent and a reinforcing agent to the flocculant.
The early strength agent comprises potassium formate, and the potassium formate improves the early strength of the concrete and has no influence on the later strength increase of the concrete.
The reinforcing agent comprises a nanocrystalline reinforcing agent, and the nanocrystalline reinforcing agent is added into the concrete, so that the hydration degree of the cement can be effectively improved, and the strength of the concrete is improved. However, the cement is easy to agglomerate when added, is difficult to disperse in the cement material, and seriously influences the reinforcing effect on the cement material.
On one hand, as the dimethyldiallylammonium chloride has a remarkable polyelectrolyte effect, the dimethyldiallylammonium chloride is added, so that the viscosity of a concrete system is reduced along with the increase of the concentration, and the fluidity of the concrete is improved.
On the other hand, the starch grafted acrylate modified copolymer cross-linked polymer can adjust the electronic potential energy distribution among cement particles, reduce the surface activity of flocculant molecules, and simultaneously can replace the water reducer and slump retaining agent to be preferentially adsorbed by flocculant molecules due to higher activity of the starch grafted acrylate modified copolymer cross-linked polymer, so that the plasticization effect of liquid materials is effectively improved, the viscosity of concrete is reduced, and the fluidity of the concrete is improved.
In addition, the sodium lignosulfonate and the acrylic acid copolymer derivative have both hydrophobic and hydrophilic groups, have high dispersibility and deflocculating effects, have a three-dimensional electrostatic force acting between cement particles, can resist the adsorption effect of flocculant on other components in liquid materials, and simultaneously introduce a large number of tiny continuous closed beneficial bubbles under the condition of not affecting the later strength of tubular pile concrete, so that the workability and the working performance of the concrete are improved.
The invention also provides a preparation method of the flocculant, which comprises the following steps:
and mixing polyacrylamide, polydimethyl diallyl ammonium chloride, polymeric ferric sulfate and the first dispersing agent uniformly to obtain the flocculant.
The preparation method of the first dispersing agent comprises the following steps:
adding starch and water into a four-neck flask, mixing, introducing a large amount of nitrogen to ensure that the four-neck flask is in a nitrogen protection state, starting a stirrer, uniformly mixing, heating to above 85 ℃, and gelatinizing for 30min; the mass concentration of the starch is 10-15%.
And after gelatinization, stirring and cooling to 50 ℃, adding sodium acrylate and dimethyl diallyl ammonia chloride, dropwise adding an initiator, keeping the temperature for 5 hours, washing, drying and crushing the product to obtain the first dispersing agent. The mass ratio of the sodium acrylate to the dimethyldiallylammonium chloride to the starch to the initiator is 100: (30-100): (20-100): (1:20).
Specifically, the initiator includes ammonium persulfate and sodium bisulfite.
The preparation method of the second dispersing agent comprises the following steps:
at N 2 Under the protection, the sodium lignosulfonate solution and the acrylic acid are mixed in FeSO 4 .7H 2 O and H 2 O 2 And (3) reacting under the initiation, washing, drying and crushing the product to obtain the second dispersing agent. The reaction temperature was 70℃and the reaction time was 3 hours. Wherein sodium lignin sulfonate, acrylic acid, feSO4.7H 2 O 2 、H 2 O 2 The mass ratio of (1-3) to (2-6) is 100 (3-8).
The preparation method of the flocculant comprises the following specific steps:
dissolving polymeric ferric sulfate in water (the mass ratio of the polymeric ferric sulfate to the water is 1:3) to obtain a polyacrylamide solution;
heating and stirring a polymeric ferric sulfate solution to 60 ℃ on a constant-temperature stirrer, adding polydimethyl diallyl ammonium chloride, stirring and dispersing to a homogeneous solution, adding a first dispersing agent, uniformly mixing, and drying and crushing at a constant temperature of 70 ℃ to obtain a dried product;
and uniformly mixing the dried product with polyacrylamide, and adding the reinforcing agent, the early strength agent and the second dispersing agent to obtain the flocculant.
Example 1
Preparation of the first dispersant
Adding 30g of starch and 200g of water into a four-neck flask, mixing, introducing a large amount of nitrogen, enabling the four-neck flask to be in a nitrogen protection state, starting a stirrer, uniformly mixing, heating to above 85 ℃, and gelatinizing for 30min.
And after gelatinization, stirring and cooling to 50 ℃, adding 100g of sodium acrylate and 3g of dimethyl diallyl ammonia chloride, dropwise adding 2g of ammonium persulfate and 2g of sodium bisulfite, keeping the temperature for 5 hours, and washing, drying and crushing the product to obtain the first dispersing agent.
Preparation of the second dispersant
At N 2 Under protection, 100g of sodium lignosulfonate solution and 8g of acrylic acid are mixed in 3g of FeSO 4 .7H 2 O and 6g H 2 O 2 And (3) reacting under the initiation, washing, drying and crushing the product to obtain the second dispersing agent. The reaction temperature was 70℃and the reaction time was 3 hours.
Preparation of flocculant
45g of polymeric ferric sulfate is dissolved in 135g of water to obtain a polyacrylamide solution;
heating and stirring a polymeric ferric sulfate solution to 60 ℃ on a constant-temperature stirrer, adding 10g of polydimethyldiallyl ammonia chloride, stirring and dispersing to a homogeneous solution, adding 5g of a first dispersing agent, uniformly mixing, and drying and crushing at a constant temperature of 70 ℃ to obtain a dried product;
and uniformly mixing the dried product with 27g of polyacrylamide, and adding 5g of reinforcing agent, 7g of early strength agent and 1.2g of second dispersing agent to obtain the flocculant 1.
Example 2
Preparation of the second dispersant
At N 2 Under protection, 100g of sodium lignosulfonate solution and 8g of acrylic acid are mixed in 3g of FeSO 4 .7H 2 O and 6g H 2 O 2 And (3) reacting under the initiation, washing, drying and crushing the product to obtain the second dispersing agent. The reaction temperature was 70℃and the reaction time was 3 hours.
Preparation of flocculant
45g of polymeric ferric sulfate is dissolved in 135g of water to obtain a polyacrylamide solution;
heating and stirring the polymeric ferric sulfate solution to 60 ℃ on a constant temperature stirrer, adding 10g of polydimethyldiallyl ammonia chloride, stirring and dispersing to a homogeneous solution, and drying and crushing at a constant temperature of 70 ℃ to obtain a dried product;
and uniformly mixing the dried product with 27g of polyacrylamide, and adding 5g of reinforcing agent, 7g of early strength agent and 1.2g of second dispersing agent to obtain the flocculant 2.
Example 3
Preparation of the first dispersant
Adding 30g of starch and 200g of water into a four-neck flask, mixing, introducing a large amount of nitrogen, enabling the four-neck flask to be in a nitrogen protection state, starting a stirrer, uniformly mixing, heating to above 85 ℃, and gelatinizing for 30min.
And after gelatinization, stirring and cooling to 50 ℃, adding 100g of sodium acrylate and 3g of dimethyl diallyl ammonia chloride, dropwise adding 2g of ammonium persulfate and 2g of sodium bisulfite, keeping the temperature for 5 hours, and washing, drying and crushing the product to obtain the first dispersing agent.
Preparation of flocculant
45g of polymeric ferric sulfate is dissolved in 135g of water to obtain a polyacrylamide solution;
heating and stirring a polymeric ferric sulfate solution to 60 ℃ on a constant-temperature stirrer, adding 10g of polydimethyldiallyl ammonia chloride, stirring and dispersing to a homogeneous solution, adding 5g of a first dispersing agent, uniformly mixing, and drying and crushing at a constant temperature of 70 ℃ to obtain a dried product;
and uniformly mixing the dried product with 27g of polyacrylamide, and adding 5g of reinforcing agent and 7g of early strength agent to obtain the flocculant 3.
Example 4
Preparation of flocculant
45g of polymeric ferric sulfate is dissolved in 135g of water to obtain a polyacrylamide solution;
heating and stirring the polymeric ferric sulfate solution to 60 ℃ on a constant temperature stirrer, adding 10g of polydimethyldiallyl ammonia chloride, stirring and dispersing to a homogeneous solution, and drying and crushing at a constant temperature of 70 ℃ to obtain a dried product;
and uniformly mixing the dried product with 27g of polyacrylamide, and adding 5g of reinforcing agent and 7g of early strength agent to obtain the flocculant 4.
Through a series of researches on flocculation performance of the flocculant, a flocculation effect test evaluation method capable of accurately measuring the flocculant is obtained, and the specific experimental steps are as follows:
s100, preparing sand washing wastewater: weighing 3g of montmorillonite or 10g of kaolin in a 500mL beaker, adding 500mL of water, adjusting the rotating speed to 150r/min, and stirring for 5min until the soil is uniformly stirred;
s200, stopping stirring, and measuring the initial absorbance to be A after the turbidimetric bentonite solution is kept stand for 10min 0 After the kaolin turbid liquid is kept stand for 5min, the initial absorbance is measured to be A 0 ；
S300, stirring is started, the rotating speed is regulated to 150r/min, after the turbid liquid is stirred uniformly again, 4mL of a pre-prepared flocculant solution to be measured with the concentration of 0.05g/L is added, and the turbid liquid is added; the flocculant to be tested is flocculant 1, flocculant 2, flocculant 3 and a commercially available flocculant.
S400, maintaining rapid stirring for 5min until the flocculant and the sand washing wastewater are uniformly mixed, and after standing for 2min, measuring the absorbance of the supernatant fluid to be A 1 ；
S500, repeating the step (4) to obtain the absorbance A of the supernatant fluid at different stirring times after the flocculant is used for treating the sand washing wastewater 1 ～A i (i＝2，3，4……)；
S600, respectively calculating flocculation efficiency a and turbidity removal rate eta of the flocculant according to formulas (3-2) and (3-3) i And will calculate eta i The haze removal rate with the greatest median value is defined as the maximum haze removal rate eta max ：
Wherein:
A 0 -measuring the absorbance of the supernatant of the sand washing wastewater before adding the flocculant;
A i measuring the absorbance of the supernatant of the sand washing wastewater when the stirring times are i after adding the flocculant;
i-when eta i ≥95％×η max When the stirring is carried out, the minimum stirring times are required.
The maximum turbidity removal rate eta max The average of 0 to 100 percent is divided into 20 grades, and when eta max The higher the grade, the better the flocculating effect of the flocculant; when eta max When the grade is the same, the flocculation effect of the flocculant is evaluated according to the value of the flocculation efficiency a, and the larger the value of the flocculation efficiency a is, the better the flocculation effect is. The absorbance test results are shown in table 1, and the flocculation property test evaluation results are shown in table 2.
Table 1 absorbance test results for flocculants
TABLE 2 evaluation results of flocculation Performance test
As can be seen from Table 2, flocculant 1, flocculant 2 and flocculant 3 produced by the present invention have turbidity removal rates eta max The flocculation efficiency a value of the flocculant prepared by the method is higher than 90%, and the flocculation efficiency a value is higher than that of the flocculant sold in the market, so that the flocculation effect of the flocculant prepared by the method is not obviously different from that of the flocculant sold in the market.
Performance test experiments of flocculant
According to GB/T50080-2016 Standard for test methods for Performance of common concrete mixtures, the above-mentioned flocculant 1, flocculant 2, flocculant 3 and commercially available flocculant are added to tubular pile concrete, and the initial slump, 1h slump, steam curing Strength, 1d compressive Strength, 3d compressive Strength, 7d compressive Strength and 28d compressive Strength of the concrete are measured. The concrete mix ratios of the pipe piles are shown in Table 3, and the test results are shown in Table 4.
Table 3 c80 pipe pile concrete mix ratio
Table 4 c80 pipe pile concrete test results
As can be seen from Table 4, the flocculant prepared by the invention has significantly better initial fluidity and time loss in the production of pipe piles than the commercial flocculant, and the data of the steaming strength and the compressive strength show that the flocculant prepared by the invention has less influence on the concrete strength than the commercial flocculant.
The foregoing description of the preferred embodiments of the present invention is not intended to limit the scope of the invention, but rather to utilize the equivalent structure disclosed in the present specification or to directly/indirectly apply the present invention to other related technical fields, which are included in the scope of the present invention.
Claims (6)
1. The application of the flocculant in concrete is characterized in that the flocculant is prepared from the following raw materials in parts by weight:
wherein the first dispersant comprises a starch grafted acrylate modified co-cross-linked polymer,
the preparation method of the first dispersing agent comprises the following steps:
mixing starch and water, and stirring and gelatinizing;
and after gelatinization, stirring and cooling, adding sodium acrylate and dimethyl diallyl ammonium chloride, dripping an initiator, reacting at constant temperature for 3-8 h, washing, drying and crushing the product to obtain a solid product.
2. The use according to claim 1, characterized in that the flocculant further comprises 1-10 parts by weight of a reinforcing agent.
3. The use according to claim 2, wherein the reinforcing agent comprises at least one of calcium formate, triethanolamine, nanocrystal core reinforcing agent, potassium nitrate and lithium sulfate.
4. The use according to claim 1, characterized in that the flocculant further comprises, in parts by weight, 1-10 parts of an early strength agent.
5. The use of claim 4, wherein the early strength agent comprises at least one of potassium formate and sodium formate.
6. The use according to claim 1, characterized in that the flocculant further comprises, in parts by weight, 1-10 parts of a second dispersant comprising a co-derivative of sodium lignosulfonate and acrylic acid.
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| CN102585097A (en) * | 2012-02-26 | 2012-07-18 | 河南工业大学 | Method for preparing amphoteric starch |
| CN104973817A (en) * | 2015-07-06 | 2015-10-14 | 水利部交通运输部国家能源局南京水利科学研究院 | Concrete viscosity regulator suitable for compatible use with polycarboxylic acid water reducer and preparation method thereof |
| CN114349387A (en) * | 2022-01-20 | 2022-04-15 | 南京永能新材料有限公司 | Machine-made sand flocculating agent without influencing concrete performance and preparation method thereof |
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| CN102585097A (en) * | 2012-02-26 | 2012-07-18 | 河南工业大学 | Method for preparing amphoteric starch |
| CN104973817A (en) * | 2015-07-06 | 2015-10-14 | 水利部交通运输部国家能源局南京水利科学研究院 | Concrete viscosity regulator suitable for compatible use with polycarboxylic acid water reducer and preparation method thereof |
| CN114349387A (en) * | 2022-01-20 | 2022-04-15 | 南京永能新材料有限公司 | Machine-made sand flocculating agent without influencing concrete performance and preparation method thereof |
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