CN115745464A - Flocculating agent and preparation method thereof - Google Patents
Flocculating agent and preparation method thereof Download PDFInfo
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- CN115745464A CN115745464A CN202211465856.7A CN202211465856A CN115745464A CN 115745464 A CN115745464 A CN 115745464A CN 202211465856 A CN202211465856 A CN 202211465856A CN 115745464 A CN115745464 A CN 115745464A
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- flocculant
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- ammonium chloride
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- 239000008394 flocculating agent Substances 0.000 title abstract description 26
- 238000002360 preparation method Methods 0.000 title abstract description 16
- 239000002270 dispersing agent Substances 0.000 claims abstract description 41
- 229920002401 polyacrylamide Polymers 0.000 claims abstract description 26
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 20
- 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 claims abstract description 17
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000012744 reinforcing agent Substances 0.000 claims abstract description 16
- 229920002472 Starch Polymers 0.000 claims abstract description 15
- 235000019698 starch Nutrition 0.000 claims abstract description 15
- 239000008107 starch Substances 0.000 claims abstract description 15
- 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 13
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims description 28
- 238000002156 mixing Methods 0.000 claims description 24
- 239000000047 product Substances 0.000 claims description 24
- 238000001035 drying Methods 0.000 claims description 17
- 238000005406 washing Methods 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 10
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- 229920005552 sodium lignosulfonate Polymers 0.000 claims description 8
- 229940048053 acrylate Drugs 0.000 claims description 7
- 239000012456 homogeneous solution Substances 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
- 239000003623 enhancer Substances 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
- PZNOBXVHZYGUEX-UHFFFAOYSA-N n-prop-2-enylprop-2-en-1-amine;hydrochloride Chemical compound Cl.C=CCNCC=C PZNOBXVHZYGUEX-UHFFFAOYSA-N 0.000 claims description 5
- WFIZEGIEIOHZCP-UHFFFAOYSA-M potassium formate Chemical compound [K+].[O-]C=O WFIZEGIEIOHZCP-UHFFFAOYSA-M 0.000 claims description 5
- 235000019270 ammonium chloride Nutrition 0.000 claims description 4
- 229920002126 Acrylic acid copolymer Polymers 0.000 claims description 3
- CBOCVOKPQGJKKJ-UHFFFAOYSA-L Calcium formate Chemical compound [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 compound 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
- 229920001577 copolymer Polymers 0.000 claims description 3
- 229920006037 cross link polymer Polymers 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 Substances 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
- 239000012265 solid product Substances 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 18
- 238000005189 flocculation Methods 0.000 abstract description 16
- 230000016615 flocculation Effects 0.000 abstract description 15
- 239000004576 sand Substances 0.000 abstract description 11
- 239000004568 cement Substances 0.000 abstract description 8
- 238000007334 copolymerization reaction Methods 0.000 abstract description 6
- 239000002245 particle Substances 0.000 abstract description 5
- 239000000126 substance Substances 0.000 abstract description 4
- 239000003638 chemical reducing agent Substances 0.000 abstract description 3
- 229920000867 polyelectrolyte Polymers 0.000 abstract description 3
- 238000009826 distribution Methods 0.000 abstract description 2
- 238000005381 potential energy Methods 0.000 abstract description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 12
- 238000002835 absorbance Methods 0.000 description 8
- 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
- 229910052757 nitrogen Inorganic materials 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 5
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 4
- 230000000977 initiatory effect Effects 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000001179 sorption measurement Methods 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
- 238000011156 evaluation Methods 0.000 description 3
- 239000000203 mixture Substances 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
- 239000005995 Aluminium silicate Substances 0.000 description 2
- 235000012211 aluminium silicate Nutrition 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000011243 crosslinked material Substances 0.000 description 2
- 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 2
- 230000003311 flocculating effect Effects 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
- 239000000178 monomer Substances 0.000 description 2
- 229910052901 montmorillonite Inorganic materials 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 230000000379 polymerizing effect Effects 0.000 description 2
- 150000003254 radicals Chemical class 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000007796 conventional method Methods 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
- 230000006872 improvement Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000002689 soil Substances 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
Landscapes
- Separation Of Suspended Particles By Flocculating Agents (AREA)
Abstract
The invention relates to a flocculating agent and a preparation method thereof, wherein the flocculating agent comprises 25 to 30 parts by weight of a raw material for preparing the flocculating agent; 8-12 parts of dimethyl diallyl ammonium chloride; 40-60 parts of polymeric ferric sulfate; 1-20 parts of a dispersing agent; 1-10 parts of a reinforcing agent; 1-10 parts of early strength agent. The polyacrylamide can enable suspended substances to be electrically neutralized, the flocculation effect is good, the dimethyl diallyl ammonium chloride has a remarkable polyelectrolyte effect, the viscosity is reduced along with the increase of the concentration by adding the dimethyl diallyl ammonium chloride, the fluidity of concrete is improved, the electronic potential energy distribution among cement particles can be adjusted by starch grafted acrylate modified copolymerization cross-linked substances, the water reducing agent and the slump retaining agent can be replaced, the flocculant molecules can preferentially adsorb the water reducing agent and the slump retaining agent, the viscosity of the pipe pile concrete is effectively reduced, the fluidity of the pipe pile concrete is improved, and therefore the influence of the residual of the machine-made sand flocculant on the strength of the pipe pile concrete is reduced.
Description
Technical Field
The invention relates to the technical field of building additives, in particular to a flocculating agent and a preparation method thereof.
Background
The machine-made sand generates 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, machine-made sand needs to be washed, and in order to improve the turnover efficiency of the waste water, a flocculating agent is added into the washed waste water to accelerate the sedimentation of silt particles.
When the machine-made sand added with the flocculating agent is applied to the tubular pile concrete, the strength of the tubular pile is greatly reduced.
Disclosure of Invention
Based on this, it is necessary to provide a flocculant that has little effect on the strength of the pipe pile.
In order to achieve the above purpose, the invention provides a technical scheme:
the flocculant comprises the following raw materials in parts by weight:
wherein the first dispersant comprises a starch grafted acrylate modified copolymer cross-linked polymer.
Preferably, the flocculant further comprises 1-10 parts of reinforcing agent by weight.
Preferably, the enhancer comprises at least one of calcium formate, triethanolamine, a nanocrystal core enhancer, potassium nitrate, and lithium sulfate.
Preferably, the flocculant further comprises 1-10 parts of an early strength agent by weight.
Preferably, the early strength agent comprises at least one of potassium formate and sodium formate.
Preferably, the flocculant further comprises 1-10 parts of a second dispersing agent, and the second dispersing agent comprises sodium lignosulfonate and acrylic acid copolymerization derivatives.
The invention also provides a preparation method of the flocculant, which comprises the following steps:
and mixing the polyacrylamide, the polydimethy diallyl ammonium chloride, the polyferric 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 to gelatinize;
and (3) after pasting, stirring and cooling, adding sodium acrylate and dimethyl diallyl ammonium chloride, dropwise adding an initiator, reacting for 3-8 h at constant temperature, and 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 polydimethyldiallylammonium chloride, stirring and dispersing to form a homogeneous solution, adding the 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 a reinforcing agent, an early strength agent and a second dispersing agent to obtain the flocculant.
Preferably, the temperature for drying and crushing at constant temperature is 70 ℃.
The invention has the beneficial effects that:
the flocculant is prepared from polyacrylamide, polydimethy diallyl ammonium chloride, polymeric ferric sulfate and a first dispersing agent, wherein the first dispersing agent comprises a starch grafted acrylate modified copolymerization cross-linked product. The polyacrylamide is a water-soluble linear high-molecular polymer which is formed by polymerizing acrylamide monomers through free radicals, can enable suspended substances to have a good flocculation effect through electric neutralization and bridging adsorption, and the dimethyl diallyl ammonium chloride has a remarkable polyelectrolyte effect, so that the viscosity is reduced along with the increase of the concentration by adding the dimethyl diallyl ammonium chloride, and the fluidity of the tubular pile concrete is improved. With the improvement of the fluidity of the pipe pile concrete and the assistance of the early strength agent and the reinforcing agent, the influence of the residual flocculating agent on the strength of the pipe pile concrete can be obviously reduced.
Detailed Description
The present invention will be further described with reference to specific examples for better illustrating the objects, technical solutions and advantages of the present invention.
In the examples, the test methods used were conventional methods unless otherwise specified, and the materials, reagents and the like used were commercially available without otherwise specified.
The flocculant comprises the following raw materials in parts by weight:
wherein the first dispersant comprises a starch grafted acrylate modified copolymer 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, a 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 comprises at least one of potassium formate and sodium formate.
In one embodiment, the flocculant further comprises 1-10 parts by weight of a second dispersing agent, and the second dispersing agent comprises sodium lignosulfonate and acrylic acid copolymer derivatives.
The flocculant is prepared from polyacrylamide, polydimethy diallyl ammonium chloride, polymeric ferric sulfate and a first dispersing agent, wherein the first dispersing agent comprises a starch grafted acrylate modified copolymerization cross-linked product.
When the flocculant prepared by the invention is used for concrete, the polyacrylamide is a water-soluble linear high molecular polymer formed by polymerizing acrylamide monomers through free radical initiation, suspended substances in the concrete can be electrically neutralized, and a flocculating body is formed through bridging adsorption, so that the flocculant has a good flocculation effect.
After the polyacrylamide is added, the polyacrylamide can load the surface of cement particles to form an adsorption film, so that the fluidity, air entraining effect and compressive strength of the concrete are reduced.
Further, in order to reduce the reduction of the compressive strength caused by adding polyacrylamide into the flocculant, the invention adds an early strength agent and a reinforcing agent into 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 concrete, so that the hydration degree of cement can be effectively improved, and the strength of the concrete is improved. But the cement material is easy to agglomerate when being added, is extremely difficult to disperse in the cement material, and seriously influences the reinforcing effect on the cement material.
On one hand, the dimethyl diallyl ammonium chloride has a remarkable polyelectrolyte effect, and the viscosity of a concrete system is reduced along with the increase of the concentration by adding the dimethyl diallyl ammonium chloride, so that the fluidity of the concrete is improved.
On the other hand, the starch grafted acrylate modified copolymerization cross-linked material can adjust the electronic potential energy distribution among cement particles and reduce the surface activity of flocculant molecules, and meanwhile, the starch grafted acrylate modified copolymerization cross-linked material has higher activity and can replace a water reducing agent and a slump retaining agent to be preferentially adsorbed by the flocculant molecules, so that the plasticizing 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 acrylic acid copolymer derivative have hydrophobic and hydrophilic groups, have high dispersibility and anti-flocculation effect, and electrostatic force acting among cement particles is in a three-dimensional form, so that the adsorption effect of a flocculating agent on other components in a liquid material can be resisted, and meanwhile, a large amount of tiny continuous closed beneficial bubbles are introduced under the condition of not influencing the later strength of the 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 the polyacrylamide, the polydimethy diallyl ammonium chloride, the polyferric sulfate and the first dispersing agent uniformly to obtain the flocculant.
The first dispersant is prepared by the method comprising:
adding starch and water into a four-neck flask for mixing, introducing a large amount of nitrogen to enable the four-neck flask to be in a nitrogen protection state, starting a stirrer for uniformly mixing, heating to above 85 ℃, and gelatinizing for 30min; the mass concentration of the starch is 10-15%.
And (3) after pasting, stirring and cooling to 50 ℃, adding sodium acrylate and dimethyl diallyl ammonium 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 dimethyl diallyl ammonium chloride to the starch to the initiator is 100: (30-100): (20 to 100): (1:20).
Specifically, the initiator includes ammonium persulfate and sodium bisulfite.
The preparation method of the second dispersing agent comprises the following steps:
in N 2 Under protection, mixing sodium lignosulphonate solution with acrylic acid in FeSO 4 .7H 2 O and H 2 O 2 And (3) reacting under initiation, washing, drying and crushing the product to obtain a second dispersing agent. The reaction temperature is 70 ℃, and the reaction time is 3h. Wherein the sodium lignosulfonate, acrylic acid and 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 polyferric sulfate in water (the mass ratio of the polyferric sulfate to the water is 1:3) to obtain a polyacrylamide solution;
heating and stirring the polymeric ferric sulfate solution on a constant-temperature stirrer to 60 ℃, adding polydimethyldiallyl ammonium chloride, stirring and dispersing to obtain a homogeneous solution, adding a first dispersing agent, uniformly mixing, drying and crushing at the constant temperature of 70 ℃ to obtain a dried product;
and (3) uniformly mixing the dried product with polyacrylamide, and adding a reinforcing agent, an early strength agent and a second dispersing agent to obtain the flocculant.
Example 1
Preparing the first dispersant
Adding 30g of starch and 200g of water into a four-neck flask for mixing, introducing a large amount of nitrogen to ensure that the four-neck flask is in a nitrogen protection state, starting a stirrer for uniformly mixing, heating to above 85 ℃, and gelatinizing for 30min.
And (3) cooling to 50 ℃ while stirring after gelatinization, adding 100g of sodium acrylate and 3g of dimethyl diallyl ammonium chloride, dropwise adding 2g of ammonium persulfate and 2g of sodium bisulfite, keeping the temperature for 5 hours, washing, drying and crushing the product to obtain the first dispersing agent.
Preparation of the second dispersant
In 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 initiation, washing, drying and crushing the product to obtain a second dispersing agent. The reaction temperature is 70 ℃, and the reaction time is 3h.
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 on a constant-temperature stirrer to 60 ℃, adding 10g of polydimethyldiallylchloride, stirring and dispersing to obtain a homogeneous solution, adding 5g of a first dispersing agent, uniformly mixing, drying and crushing at the constant temperature of 70 ℃ to obtain a dried product;
and (3) 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
In N 2 Under the protection of the air conditioner, the air conditioner is protected,100g of sodium lignosulfonate solution and 8g of acrylic acid in 3g of FeSO 4 .7H 2 O and 6g H 2 O 2 And (3) reacting under initiation, washing, drying and crushing the product to obtain a second dispersing agent. The reaction temperature is 70 ℃, and the reaction time is 3h.
Preparation of flocculating agent
45g of polymeric ferric sulfate is dissolved in 135g of water to obtain a polyacrylamide solution;
heating and stirring the polymeric ferric sulfate solution on a constant-temperature stirrer to 60 ℃, adding 10g of polydimethyldiallyl ammonium chloride, stirring and dispersing to obtain a homogeneous solution, and drying and crushing at a constant temperature of 70 ℃ to obtain a dried product;
and (3) 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
Preparing the first dispersant
Adding 30g of starch and 200g of 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 to uniformly mix, heating to above 85 ℃, and gelatinizing for 30min.
And (3) cooling to 50 ℃ while stirring after gelatinization, adding 100g of sodium acrylate and 3g of dimethyl diallyl ammonium chloride, dropwise adding 2g of ammonium persulfate and 2g of sodium bisulfite, keeping the temperature for 5 hours, washing, drying and crushing the product to obtain the first dispersing agent.
Preparation of flocculating agent
Dissolving 45g of polymeric ferric sulfate in 135g of water to obtain a polyacrylamide solution;
heating and stirring the polymeric ferric sulfate solution on a constant-temperature stirrer to 60 ℃, adding 10g of polydimethyldiallylchloride, stirring and dispersing to obtain a homogeneous solution, adding 5g of a first dispersing agent, uniformly mixing, drying and crushing at the constant temperature of 70 ℃ to obtain a dried product;
and (3) 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 flocculating agent
45g of polymeric ferric sulfate is dissolved in 135g of water to obtain a polyacrylamide solution;
heating and stirring the polymeric ferric sulfate solution on a constant-temperature stirrer to 60 ℃, adding 10g of polydimethyldiallyl ammonium chloride, stirring and dispersing to obtain a homogeneous solution, and drying and crushing at a constant temperature of 70 ℃ to obtain a dried product;
and (3) 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.
A flocculation effect test and evaluation method capable of accurately measuring a flocculant is obtained by carrying out a series of researches on the flocculation performance of the flocculant, 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, standing the turbid solution of the montmorillonite for 10min, and determining the initial absorbance A 0 Standing kaolin turbid liquid for 5min, and determining initial absorbance A 0 ；
S300, opening stirring, adjusting the rotating speed to 150r/min, adding 4mL of pre-prepared flocculant solution to be detected with the concentration of 0.05g/L into the turbid liquid after the turbid liquid is stirred uniformly again; the flocculating agents to be detected are flocculating agent 1, flocculating agent 2, flocculating agent 3 and commercially available flocculating agent.
S400, keeping rapid stirring for 5min until the flocculating agent and the sand washing wastewater are uniformly mixed, standing for 2min, and determining the absorbance of the supernatant as A 1 ；
S500, repeating the step (4) to obtain the absorbance A of the supernatant liquid after the sand washing wastewater is treated by the flocculating agent and the stirring times are different 1 ～A i (i＝2，3，4……)；
S600, respectively calculating the flocculation efficiency a and the turbidity removal rate eta of the flocculating agent according to the formulas (3-2) and (3-3) i And eta to be calculated i The turbidity removal rate at which the median value is the greatest is defined as the maximum turbidity removal rate η max ：
In the formula:
A 0 measuring the absorbance of the supernatant of the sand washing wastewater before adding the flocculating agent;
A i measuring the absorbance of the supernatant of the sand washing wastewater when the stirring frequency is i after the flocculating agent is added;
i-when eta i ≥95％×η max The minimum number of stirring is required.
Removing the maximum turbidity max Is divided into 20 grades from 0 to 100 percent on average when eta max The higher the grade, the better the flocculating effect of the flocculating agent; when eta max The grades are the same, the flocculation effect of the flocculating agent is evaluated through 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 results of the absorbance test are shown in table 1, and the results of the flocculation property test evaluation are shown in table 2.
TABLE 1 Absorbance test results for flocculants
Table 2 flocculation property test evaluation results
As can be seen from Table 2, the turbidity removal rates eta of the flocculant 1, the flocculant 2 and the flocculant 3 prepared by the present invention max The flocculant can reach more than 90 percent and is larger than the flocculation efficiency a value of a commercial flocculant, which shows that the flocculation effect of the flocculant prepared by the invention has no obvious difference with the flocculation effect of the commercial flocculant.
Flocculant performance test experiment
According to GB/T50080-2016 standard of common concrete mixture performance test methods, the flocculant 1, the flocculant 2, the flocculant 3 and a commercially available flocculant are added into the tubular pile concrete, and the initial slump, the 1h slump, the steam curing strength, the 1d compressive strength, the 3d compressive strength, the 7d compressive strength and the 28d compressive strength of the concrete are measured. The concrete mix ratio of the pipe pile is shown in table 3, and the test results are shown in table 4.
TABLE 3 C80 tubular pile concrete mixing ratio
TABLE 4 C80 tubular pile concrete test results
As can be seen from Table 4, the initial fluidity and the time loss of the flocculant prepared by the invention in the production of the pipe pile are obviously better than those of the flocculant sold in the market, and the steam curing strength and the compressive strength data show that the influence of the flocculant prepared by the invention on the concrete strength is smaller than that of the flocculant sold in the market.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention, and all modifications, equivalents and applications made by the present invention in the technical field of the present invention are included in the scope of the present invention.
Claims (10)
1. The flocculant 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 copolymer cross-linked polymer.
2. The flocculant of claim 1, further comprising 1 to 10 parts by weight of a reinforcing agent.
3. The flocculant of claim 2, wherein the enhancer comprises at least one of calcium formate, triethanolamine, a nanocrystal core enhancer, potassium nitrate, and lithium sulfate.
4. The flocculant of claim 1, further comprising 1 to 10 parts by weight of an early strength agent.
5. The flocculant of claim 4, wherein the early strength agent comprises at least one of potassium formate and sodium formate.
6. The flocculant of claim 1, further comprising 1-10 parts by weight of a second dispersant, wherein the second dispersant comprises sodium lignosulfonate and acrylic acid copolymer derivatives.
7. A method of preparing a flocculant according to claim 1, comprising the steps of:
and mixing the polyacrylamide, the polydimethyl diallyl ammonium chloride, the polymeric ferric sulfate and the first dispersing agent uniformly to obtain the flocculant.
8. The method for preparing a flocculant according to claim 7, wherein the method for preparing the first dispersant comprises:
mixing starch and water, and stirring to gelatinize;
and (3) after gelatinization, stirring and cooling, adding sodium acrylate and dimethyl diallyl ammonium chloride, dropwise adding an initiator, reacting at constant temperature for 3-8 h, and washing, drying and crushing the product to obtain a solid product.
9. The method for preparing the flocculant according to claim 7, wherein the specific steps of the method for preparing the flocculant comprise:
dissolving the polymeric ferric sulfate in water to obtain a polymeric ferric sulfate solution;
heating and stirring the polymeric ferric sulfate solution on a constant-temperature stirrer, adding the polydimethyldiallyl ammonium chloride, stirring and dispersing to obtain a homogeneous solution, adding the 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 a reinforcing agent, an early strength agent and a second dispersing agent to obtain the flocculant.
10. The method for preparing the flocculant according to claim 9, wherein the temperature for drying and crushing at constant temperature is 70 ℃.
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| CN117534380A (en) * | 2023-11-15 | 2024-02-09 | 万特福建筑构件有限公司 | Wet-mixed mortar and preparation method thereof |
| CN117534380B (en) * | 2023-11-15 | 2024-05-28 | 万特福建筑构件有限公司 | Wet-mixed mortar and preparation method thereof |
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