CN108529923B - Modified cement grinding aid and preparation method thereof - Google Patents
Modified cement grinding aid and preparation method thereof Download PDFInfo
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- CN108529923B CN108529923B CN201810515477.1A CN201810515477A CN108529923B CN 108529923 B CN108529923 B CN 108529923B CN 201810515477 A CN201810515477 A CN 201810515477A CN 108529923 B CN108529923 B CN 108529923B
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- 239000004568 cement Substances 0.000 title claims abstract description 70
- 238000000227 grinding Methods 0.000 title claims abstract description 65
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- -1 sodium carboxylate Chemical class 0.000 claims abstract description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 35
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims abstract description 33
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000011737 fluorine Substances 0.000 claims abstract description 29
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 29
- 229910004298 SiO 2 Inorganic materials 0.000 claims abstract description 19
- 239000011734 sodium Substances 0.000 claims abstract description 16
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 16
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 14
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims abstract description 12
- 235000013379 molasses Nutrition 0.000 claims abstract description 12
- 229920005862 polyol Polymers 0.000 claims abstract description 12
- 150000003077 polyols Chemical class 0.000 claims abstract description 12
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 11
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229920000058 polyacrylate Polymers 0.000 claims abstract description 11
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 11
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000002699 waste material Substances 0.000 claims abstract description 11
- XPBBUZJBQWWFFJ-UHFFFAOYSA-N fluorosilane Chemical compound [SiH3]F XPBBUZJBQWWFFJ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 150000002148 esters Chemical class 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 229920001909 styrene-acrylic polymer Polymers 0.000 claims abstract description 8
- 239000010413 mother solution Substances 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 15
- 235000019441 ethanol Nutrition 0.000 claims description 14
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 9
- 150000007942 carboxylates Chemical class 0.000 claims description 8
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 8
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 8
- 239000012452 mother liquor Substances 0.000 claims description 6
- 230000032683 aging Effects 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 3
- MWKJTNBSKNUMFN-UHFFFAOYSA-N trifluoromethyltrimethylsilane Chemical compound C[Si](C)(C)C(F)(F)F MWKJTNBSKNUMFN-UHFFFAOYSA-N 0.000 claims description 3
- 125000005456 glyceride group Chemical group 0.000 claims description 2
- 238000009413 insulation Methods 0.000 claims description 2
- 238000010907 mechanical stirring Methods 0.000 claims description 2
- 239000002245 particle Substances 0.000 abstract description 9
- 206010016807 Fluid retention Diseases 0.000 abstract description 5
- 239000000843 powder Substances 0.000 abstract description 3
- 238000000034 method Methods 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 5
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 4
- 238000004321 preservation Methods 0.000 description 4
- NJVOHKFLBKQLIZ-UHFFFAOYSA-N (2-ethenylphenyl) prop-2-enoate Chemical compound C=CC(=O)OC1=CC=CC=C1C=C NJVOHKFLBKQLIZ-UHFFFAOYSA-N 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- QQGISFDJEJMKIL-JAIQZWGSSA-N (5z)-5-[[3-(hydroxymethyl)thiophen-2-yl]methylidene]-10-methoxy-2,2,4-trimethyl-1h-chromeno[3,4-f]quinolin-9-ol Chemical group C1=CC=2NC(C)(C)C=C(C)C=2C2=C1C=1C(OC)=C(O)C=CC=1O\C2=C/C=1SC=CC=1CO QQGISFDJEJMKIL-JAIQZWGSSA-N 0.000 description 2
- 230000006978 adaptation Effects 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 230000000740 bleeding effect Effects 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 150000005846 sugar alcohols Polymers 0.000 description 2
- 239000002023 wood Substances 0.000 description 2
- HXKKHQJGJAFBHI-UHFFFAOYSA-N 1-aminopropan-2-ol Chemical compound CC(O)CN HXKKHQJGJAFBHI-UHFFFAOYSA-N 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 239000002075 main ingredient Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/40—Compounds containing silicon, titanium or zirconium or other organo-metallic compounds; Organo-clays; Organo-inorganic complexes
- C04B24/42—Organo-silicon compounds
- C04B24/425—Organo-modified inorganic compounds, e.g. organo-clays
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/52—Grinding aids; Additives added during grinding
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention discloses a modified cement grinding aid and a preparation method thereof, wherein the cement grinding aid is prepared from the following raw materials in parts by mass: 100-140 parts of absolute ethyl alcohol, 12-16 parts of ammonia water, 18-24 parts of tetraethoxysilane, 8-12 parts of methyltriethoxysilane, 5-8 parts of fluorosilane, 20-35 parts of a polymeric polyol mother solution, 4-8 parts of triethanolamine, 2-8 parts of polyacrylate, 2-8 parts of styrene-acrylic ester, 3-10 parts of polyvinyl alcohol, 2-8 parts of sodium carboxylate, 4-8 parts of waste molasses, 3-6 parts of propylene glycol and 15-45 parts of water. The invention utilizes fluorine-containing nano SiO 2 Modified cement grinding aid and fluorine-containing nano SiO 2 The mixing amount of the cement powder is smaller, so that the grinding efficiency can be obviously improved, the ground cement particles have larger specific surface area and smaller screen residue, the early strength of the cement is obviously improved, and the water retention of the ground cement is effectively improved.
Description
Technical Field
The invention relates to the field of cement production, in particular to a fluorine-containing nano SiO 2 A modified cement grinding aid and a preparation method thereof.
Technical Field
The grinding process in cement production has extremely high energy consumption, and the energy consumption is higher when the minerals are further finely ground and ultra-finely ground. Therefore, the method has the important significance of reducing the energy consumption in the grinding process and improving the powder efficiency. The cement grinding aid is a production auxiliary agent which improves grinding efficiency, improves material grindability in cement production and has very small doping amount. In the cement grinding process, the grinding aid can obviously improve the grinding efficiency, greatly reduce the grinding power consumption, and has better effect especially in the fine grinding and superfine grinding processes. Meanwhile, the grinding aid can also improve the early strength of cement, and reduce the production cost of cement on the basis of not damaging the self performance of the cement. The cement particles are gradually thinned along with grinding, charges are generated on the surfaces of the particles due to the rupture of chemical bonds, and the particles are mutually adsorbed to generate agglomeration, so that the grinding efficiency is greatly reduced. The grinding aid acts between particles of cement materials, reduces the surface energy of the particles, and has the principle of preventing particle agglomeration, improving the fluidity of the particles and improving the grinding efficiency, thereby saving energy and reducing emission.
At present, the grinding aid used in cement factories is generally an alcohol liquid grinding aid, and the existing cement grinding aid has the defects of low grinding efficiency, insufficient improvement of early-stage cement mechanical strength, poor water retention of the cement after grinding and the like.
Disclosure of Invention
In order to solve the technical problems, the invention provides a fluorine-containing nano SiO 2 A modified cement grinding aid and a preparation method thereof.
The technical scheme adopted by the invention is as follows:
the modified cement grinding aid is prepared from the following raw materials in parts by mass: 100-140 parts of absolute ethyl alcohol, 12-16 parts of ammonia water, 18-24 parts of tetraethoxysilane, 8-12 parts of methyltriethoxysilane, 5-8 parts of fluorosilane, 20-35 parts of a polymeric polyol mother solution, 4-8 parts of triethanolamine, 2-8 parts of polyacrylate, 2-8 parts of styrene-acrylic ester, 3-10 parts of polyvinyl alcohol, 2-8 parts of sodium carboxylate, 4-8 parts of waste molasses, 3-6 parts of propylene glycol and 15-45 parts of water.
Further, the fluorosilane is nonafluoroethyltrimethyloxysilane, heptadecafluorosilane or trifluoromethyl trimethylsilane.
Further, the sodium carboxylate is sodium fatty alcohol polyoxyethylene ether carboxylate.
The preparation method of the modified cement grinding aid comprises the following steps:
(1) Mixing 100-140 parts of absolute ethyl alcohol, 12-16 parts of ammonia water and 5-15 parts of water in a flask, sequentially adding 18-24 parts of tetraethoxysilane and 8-12 parts of methyltriethoxysilane, reacting for 1-3 hours at 55-65 ℃, adding 5-8 parts of fluorosilane, continuing to perform thermal insulation reaction, and aging at 18-22 ℃ to obtain fluorine-containing nano SiO 2 Gel;
(2) Heating 20-35 parts of polymerized polyol mother liquor, 2-8 parts of polyacrylate and 2-8 parts of styrene-acrylic ester to 60-95 ℃, mechanically stirring, then dispersing by ultrasonic waves until uniform, and reacting in a water bath at 60-95 ℃ for 1-3 hours to obtain an alcohol amine ester compound;
(3) Adding fluorine-containing nano SiO obtained in the step (1) into the alcohol amine ester compound obtained in the step (2) 2 Gel, after ultrasonic dispersion to be uniform, reacting for 2-4 hours at 60-95 ℃ to obtain fluorine-containing nano SiO 2 Modified alcohol amine ester compounds;
(4) Fluorine-containing nano SiO obtained in the step (3) 2 Adding 10-30 parts of water into the modified alcohol amine ester compound, dispersing the mixture to be uniform by ultrasonic waves, then adding 4-8 parts of triethanolamine, 3-10 parts of polyvinyl alcohol, 2-8 parts of sodium carboxylate, 4-8 parts of waste molasses and 3-6 parts of propylene glycol, dispersing the mixture to be uniform by ultrasonic waves, and standing the mixture to obtain the modified cement grinding aid.
Wherein in the step (1), the reaction time of heat preservation is 2-4h, and the ageing time is 12-48 h.
In the step (2), the heating is water bath heating, mechanical stirring is carried out for 20-30min, and then ultrasonic dispersion is carried out for 10-20min until uniformity is achieved.
In the step (3), the ultrasonic dispersion is carried out for 5-20min until the ultrasonic dispersion is uniform.
In the step (4), after adding water, dispersing for 30-50min by ultrasonic wave, then adding other raw materials, and continuing dispersing for 10-30min by ultrasonic wave.
The beneficial effects of the invention are as follows: the invention utilizes fluorine-containing nano SiO 2 Modified cement grinding aid and fluorine-containing nano SiO 2 The mixing amount of the cement powder is smaller, so that the grinding efficiency can be obviously improved, the ground cement particles have larger specific surface area and smaller screen residue, the early strength of the cement is obviously improved, and the water retention of the ground cement is effectively improved.
Detailed Description
The present invention will be explained in detail with reference to examples.
The mother liquor of the polymeric polyol used in the examples below was purchased from the company Jiang Yu oil, inc., yangtze river, nanj (its main ingredients are polymeric glycerol, glycerides, glycerol; solids content > 85%) and the remaining materials were commercially available.
Example 1
The modified cement grinding aid is prepared from the following raw materials in parts by mass: 120 parts of absolute ethyl alcohol, 15 parts of ammonia water, 20 parts of tetraethoxysilane, 10 parts of methyltriethoxysilane, 6 parts of fluorosilane, 30 parts of a polymer polyol mother solution, 8 parts of triethanolamine, 4 parts of polyacrylate, 6 parts of styrene-acrylic ester, 5 parts of polyvinyl alcohol, 4 parts of sodium fatty alcohol polyoxyethylene ether carboxylate, 6 parts of waste molasses, 3 parts of propylene glycol and 30 parts of water.
The preparation method of the modified cement grinding aid comprises the following steps:
(1) 120 parts of absolute ethyl alcohol, 15 parts of ammonia water and 10 parts of water are fully mixed in a three-neck flask for 15min (the final concentration of the ammonia water is 1 mol/L), then 20 parts of tetraethoxysilane and 10 parts of methyltriethoxysilane are sequentially added, the mixture is reacted for 2h at 60 ℃,6 parts of nonafluoroethyl trimethyloxysilane are added, the heat preservation reaction is continued for 2h, and the mixture is arranged at the rear end of the reaction kettleAging for 12 hours at 20 ℃ to obtain fluorine-containing nano SiO 2 Gel;
(2) Heating 30 parts of polymerized polyol mother liquor, 4 parts of polyacrylate and 6 parts of styrene-acrylate to 65 ℃ in a water bath, mechanically stirring for 25min, then dispersing for 20min to be uniform in an ultrasonic manner, and reacting for 2h in the water bath at 65 ℃ to obtain an alcohol amine ester compound;
(3) Adding fluorine-containing nano SiO obtained in the step (1) into the alcohol amine ester compound obtained in the step (2) 2 Gel, after ultrasonic dispersion for 10min to uniformity, reacting for 2h in a water bath at 65 ℃ to obtain fluorine-containing nano SiO 2 Modified alcohol amine ester compounds;
(4) Maintaining the water bath temperature at 65 ℃, and obtaining the fluorine-containing nano SiO in the step (3) 2 Adding 20 parts of water into the modified alcohol amine ester compound, and performing ultrasonic dispersion for 30min to obtain an aqueous solution of the alcohol amine ester compound; adding 8 parts of triethanolamine, 5 parts of polyvinyl alcohol, 4 parts of sodium fatty alcohol-polyoxyethylene ether carboxylate, 6 parts of waste molasses and 3 parts of propylene glycol into the prepared solution, then dispersing for 30min by ultrasonic waves, and finally standing the solution for 24h. And (5) standing, discharging and packaging after the inspection is qualified to obtain the cement grinding aid.
The cement grinding aid obtained in the example 1 is detected to be free of pungent smell, qualified in solid content, qualified in pH value and qualified in chloride ion content, and completely meets the requirements of GB/T26748-2011.
Example 2
The modified cement grinding aid is prepared from the following raw materials in parts by mass: 100 parts of absolute ethyl alcohol, 12 parts of ammonia water, 18 parts of tetraethoxysilane, 8 parts of methyltriethoxysilane, 5 parts of fluorosilane, 20 parts of a polyalcohol mother solution, 5 parts of triethanolamine, 2 parts of polyacrylate, 8 parts of styrene-acrylic ester, 10 parts of polyvinyl alcohol, 8 parts of sodium fatty alcohol polyoxyethylene ether carboxylate, 4 parts of waste molasses, 6 parts of propylene glycol and 15 parts of water.
The preparation method of the modified cement grinding aid comprises the following steps:
(1) 100 parts of absolute ethyl alcohol, 12 parts of ammonia water and 5 parts of distilled water are fully mixed in a three-neck flask for 20min (the final concentration of the ammonia water is 0.8 mol/L), and 18 parts of ethyl orthosilicate and 5 parts of distilled water are sequentially added8 parts of methyltriethoxysilane is reacted for 3 hours at 55 ℃, 5 parts of heptadecafluoro silane is added, the heat preservation reaction is continued for 3 hours, and then the mixture is aged for 48 hours at 18 ℃ to obtain the fluorine-containing nano SiO 2 Gel;
(2) Heating 20 parts of a polymerized polyol mother solution, 2 parts of polyacrylate and 8 parts of styrene-acrylate to 60 ℃ in a water bath, mechanically stirring for 20min, then dispersing for 15min to be uniform in an ultrasonic manner, and reacting for 3h in the water bath at 55 ℃ to obtain an alcohol amine ester compound;
(3) Adding fluorine-containing nano SiO obtained in the step (1) into the alcohol amine ester compound obtained in the step (2) 2 Gel, after ultrasonic dispersion for 20min to uniformity, reacting for 4h in a water bath at 60 ℃ to obtain fluorine-containing nano SiO 2 Modified alcohol amine ester compounds;
(4) Maintaining the water bath temperature at 60 ℃, and obtaining the fluorine-containing nano SiO in the step (3) 2 Adding 10 parts of water into the modified alcohol amine ester compound, and performing ultrasonic dispersion for 50min to obtain an aqueous solution of the alcohol amine ester compound; adding 5 parts of triethanolamine, 10 parts of polyvinyl alcohol, 8 parts of sodium fatty alcohol-polyoxyethylene ether carboxylate, 4 parts of waste molasses and 6 parts of propylene glycol into the prepared solution, then dispersing for 10min by ultrasonic waves, and finally standing the solution for 24h to obtain fluorine-containing nano SiO 2 Modified cement grinding aid.
Example 3
The modified cement grinding aid is prepared from the following raw materials in parts by mass: 140 parts of absolute ethyl alcohol, 16 parts of ammonia water, 24 parts of tetraethoxysilane, 12 parts of methyltriethoxysilane, 8 parts of fluorosilane, 35 parts of a polymer polyol mother solution, 4 parts of triethanolamine, 8 parts of polyacrylate, 2 parts of styrene-acrylic ester, 3 parts of polyvinyl alcohol, 2 parts of sodium fatty alcohol polyoxyethylene ether carboxylate, 8 parts of waste molasses, 3 parts of propylene glycol and 45 parts of water.
The preparation method of the modified cement grinding aid comprises the following steps:
(1) 140 parts of absolute ethyl alcohol, 16 parts of ammonia water and 15 parts of water are fully mixed in a three-neck flask for 20min (the final concentration of the ammonia water is 1.2 mol/L), then 24 parts of tetraethoxysilane and 12 parts of methyltriethoxysilane are sequentially added, the mixture is reacted for 1h at 65 ℃, and then 8 parts of trifluoromethyl trimethylsilane are added,continuing the heat preservation reaction for 4 hours, and aging for 36 hours at 22 ℃ to obtain the fluorine-containing nano SiO 2 Gel;
(2) Heating 35 parts of polymerized polyol mother liquor, 8 parts of polyacrylate and 2 parts of styrene-acrylate to 95 ℃ in a water bath, mechanically stirring for 30min, then dispersing for 10min to be uniform in an ultrasonic manner, and reacting for 1h in the water bath at the temperature of 95 ℃ to obtain an alcohol amine ester compound;
(3) Adding fluorine-containing nano SiO obtained in the step (1) into the alcohol amine ester compound obtained in the step (2) 2 Gel, after ultrasonic dispersion for 5min to uniformity, reacting for 3h in a water bath at 95 ℃ to obtain fluorine-containing nano SiO 2 Modified alcohol amine ester compounds;
(4) Maintaining the water bath temperature at 95 ℃, and obtaining the fluorine-containing nano SiO in the step (2) 2 Adding 30 parts of water into the modified alcohol amine ester compound, and performing ultrasonic dispersion for 30min to obtain an aqueous solution of the alcohol amine ester compound; adding 4 parts of triethanolamine, 3 parts of polyvinyl alcohol, 2 parts of sodium fatty alcohol-polyoxyethylene ether carboxylate, 8 parts of waste molasses and 3 parts of propylene glycol into the prepared solution, then dispersing for 20min by ultrasonic wave, and finally standing the solution for 24h to obtain fluorine-containing nano SiO 2 Modified cement grinding aid products.
The cement grinding aid prepared in example 1 of the present invention and a commercially available cement grinding aid (the commercially available cement grinding aid is a polyhydric alcohol amine liquid grinding aid, and the main components are triethanolamine, diethanolamine, triethylpropanolamine, diethanol monoisopropanolamine, molasses, sodium wood, calcium wood, etc.) were added to PC42.5 cement, respectively, to obtain cement sample A, B, and the cement sample without any grinding aid added was C. The cement was tested for water retention, grinding aid and mechanical properties, and the test results are shown in tables 1 to 3.
Table 1 cement bleeding Rate test at different times
Table 2 test of grinding aid performance of cement grinding aid
TABLE 3 Cement Performance test and analysis
As shown in table 1, the cement grinding aid of the invention can remarkably improve the water retention of the ground cement and reduce the bleeding rate; as shown in Table 2, the cement grinding aid of the invention obviously improves the specific surface area of cement and reduces the screen allowance; as shown in Table 3, the cement grinding aid of the invention obviously improves the early mechanical properties of cement on the basis of not affecting the fluidity and setting time of cement base. Thus, the invention utilizes fluorine-containing nano SiO 2 The modified cement grinding aid has a good grinding aid effect.
The cement grinding aid and the preparation method thereof provided by the invention are described in detail. The principles and embodiments of the present invention have been described herein with reference to specific examples, the description of which is intended only to facilitate an understanding of the method of the present invention and its core ideas. It should be noted that it will be apparent to those skilled in the art that various modifications and adaptations of the invention can be made without departing from the principles of the invention and these modifications and adaptations are intended to be within the scope of the invention as defined in the following claims.
Claims (6)
1. The modified cement grinding aid is characterized by being prepared from the following raw materials in parts by mass: 100-140 parts of absolute ethyl alcohol, 12-16 parts of ammonia water, 18-24 parts of tetraethoxysilane, 8-12 parts of methyltriethoxysilane, 5-8 parts of fluorosilane, 20-35 parts of a polymeric polyol mother solution, 4-8 parts of triethanolamine, 2-8 parts of polyacrylate, 2-8 parts of styrene-acrylic ester, 3-10 parts of polyvinyl alcohol, 2-8 parts of sodium carboxylate, 4-8 parts of waste molasses, 3-6 parts of propylene glycol and 15-45 parts of water;
the main components of the polymerized polyol mother liquor are polymerized glycerol, glyceride and glycerol, and the solid content is more than 85%;
the fluorosilane is heptadecafluorosilane or trifluoromethyl trimethylsilane;
the preparation method of the cement grinding aid comprises the following steps:
(1) Mixing 100-140 parts of absolute ethyl alcohol, 12-16 parts of ammonia water and 5-15 parts of water in a flask, sequentially adding 18-24 parts of tetraethoxysilane and 8-12 parts of methyltriethoxysilane, reacting for 1-3 hours at 55-65 ℃, adding 5-8 parts of fluorosilane, continuing to perform thermal insulation reaction, and aging at 18-22 ℃ to obtain fluorine-containing nano SiO 2 Gel;
(2) Heating 20-35 parts of polymerized polyol mother liquor, 2-8 parts of polyacrylate and 2-8 parts of styrene-acrylic ester to 60-95 ℃, mechanically stirring, then dispersing by ultrasonic waves until uniform, and reacting in a water bath at 60-95 ℃ for 1-3 hours to obtain an alcohol amine ester compound;
(3) Adding fluorine-containing nano SiO obtained in the step (1) into the alcohol amine ester compound obtained in the step (2) 2 Gel, after ultrasonic dispersion to be uniform, reacting for 2-4 hours at 60-95 ℃ to obtain fluorine-containing nano SiO 2 Modified alcohol amine ester compounds;
(4) Fluorine-containing nano SiO obtained in the step (3) 2 Adding 10-30 parts of water into the modified alcohol amine ester compound, dispersing the mixture to be uniform by ultrasonic waves, then adding 4-8 parts of triethanolamine, 3-10 parts of polyvinyl alcohol, 2-8 parts of sodium carboxylate, 4-8 parts of waste molasses and 3-6 parts of propylene glycol, dispersing the mixture to be uniform by ultrasonic waves, and standing the mixture to obtain the modified cement grinding aid.
2. The modified cement grinding aid of claim 1, wherein the sodium carboxylate is sodium fatty alcohol polyoxyethylene ether carboxylate.
3. The modified cement grinding aid according to claim 1, wherein in the step (1), the time of the heat-retaining reaction is 2-4 hours, and the time of aging is 12-48 hours.
4. The modified cement grinding aid of claim 1, wherein in step (2), the heating is water bath heating, mechanical stirring for 20-30min, and then ultrasonic dispersion for 10-20min to uniformity.
5. The modified cement grinding aid of claim 1, wherein in step (3), ultrasonic dispersion is performed for 5 to 20 minutes to uniformity.
6. The modified cement grinding aid according to claim 1, wherein in the step (4), after adding water, ultrasonic dispersion is performed for 30 to 50 minutes, and then other raw materials are added, and ultrasonic dispersion is continued for 10 to 30 minutes.
Priority Applications (1)
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| CN109126215A (en) * | 2018-09-27 | 2019-01-04 | 廖秋芒 | A kind of defoaming agent and preparation method thereof suitable for polymer cement waterproof paint |
| CN111689715A (en) * | 2020-05-26 | 2020-09-22 | 贵州石博士科技有限公司 | Yield-increasing reinforced cement grinding aid and preparation method thereof |
| CN113698130B (en) * | 2021-09-16 | 2022-10-14 | 中建西部建设建材科学研究院有限公司 | Concrete waste slurry residue grinding aid and preparation method thereof |
| CN114369209A (en) * | 2022-01-25 | 2022-04-19 | 中建材中研益科技有限公司 | Silane polymer modified cement grinding aid and preparation method thereof |
| CN114918024A (en) * | 2022-04-16 | 2022-08-19 | 吉安豫顺新材料有限公司 | Process method for grinding silicon micropowder by airflow |
| CN116535122A (en) * | 2023-05-12 | 2023-08-04 | 辽宁天宝华瑞建材有限公司 | Grinding and activating method for steel slag and steel slag grinding-assisting activating agent |
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| CN102951864A (en) * | 2011-08-25 | 2013-03-06 | 济南润杰建材科技有限公司 | Cement grinding aid and cement containing same |
| CN104785349A (en) * | 2015-04-29 | 2015-07-22 | 浙江冠旗纳米科技有限公司 | Efficient preparation method for nano-scale solid powder |
| CN105599077A (en) * | 2015-12-18 | 2016-05-25 | 中国林业科学研究院木材工业研究所 | Method for preparation of superhydrophobic timber on the basis of sol-gel method |
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| CN102951864A (en) * | 2011-08-25 | 2013-03-06 | 济南润杰建材科技有限公司 | Cement grinding aid and cement containing same |
| CN104785349A (en) * | 2015-04-29 | 2015-07-22 | 浙江冠旗纳米科技有限公司 | Efficient preparation method for nano-scale solid powder |
| CN105599077A (en) * | 2015-12-18 | 2016-05-25 | 中国林业科学研究院木材工业研究所 | Method for preparation of superhydrophobic timber on the basis of sol-gel method |
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