CN108529923A - A kind of modified cement grinding aid and preparation method thereof - Google Patents
A kind of modified cement grinding aid and preparation method thereof Download PDFInfo
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- CN108529923A CN108529923A CN201810515477.1A CN201810515477A CN108529923A CN 108529923 A CN108529923 A CN 108529923A CN 201810515477 A CN201810515477 A CN 201810515477A CN 108529923 A CN108529923 A CN 108529923A
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- Prior art keywords
- parts
- grinding aid
- cement grinding
- water
- cement
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- 239000004568 cement Substances 0.000 title claims abstract description 67
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims abstract description 30
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims abstract description 29
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 29
- 239000011737 fluorine Substances 0.000 claims abstract description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 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 claims abstract description 16
- 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
- 239000000908 ammonium hydroxide Substances 0.000 claims abstract description 14
- ABTOQLMXBSRXSM-UHFFFAOYSA-N silicon tetrafluoride Chemical compound F[Si](F)(F)F ABTOQLMXBSRXSM-UHFFFAOYSA-N 0.000 claims abstract description 13
- 150000005846 sugar alcohols Polymers 0.000 claims abstract description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000012452 mother liquor Substances 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
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 9
- -1 acrylic ester Chemical class 0.000 claims description 24
- 150000001875 compounds Chemical class 0.000 claims description 15
- 150000001732 carboxylic acid derivatives Chemical class 0.000 claims description 13
- ZZVUWRFHKOJYTH-UHFFFAOYSA-N diphenhydramine Chemical class C=1C=CC=CC=1C(OCCN(C)C)C1=CC=CC=C1 ZZVUWRFHKOJYTH-UHFFFAOYSA-N 0.000 claims description 9
- 238000013019 agitation Methods 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 238000009413 insulation Methods 0.000 claims description 6
- 239000008236 heating water Substances 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 4
- 230000032683 aging Effects 0.000 claims description 2
- 235000019441 ethanol Nutrition 0.000 claims description 2
- MWKJTNBSKNUMFN-UHFFFAOYSA-N trifluoromethyltrimethylsilane Chemical compound C[Si](C)(C)C(F)(F)F MWKJTNBSKNUMFN-UHFFFAOYSA-N 0.000 claims description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims 2
- DNIAPMSPPWPWGF-GSVOUGTGSA-N (R)-(-)-Propylene glycol Chemical group C[C@@H](O)CO DNIAPMSPPWPWGF-GSVOUGTGSA-N 0.000 claims 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims 1
- 125000003784 fluoroethyl group Chemical group [H]C([H])(F)C([H])([H])* 0.000 claims 1
- 238000004321 preservation Methods 0.000 claims 1
- 239000008187 granular material Substances 0.000 abstract description 3
- NJVOHKFLBKQLIZ-UHFFFAOYSA-N (2-ethenylphenyl) prop-2-enoate Chemical compound C=CC(=O)OC1=CC=CC=C1C=C NJVOHKFLBKQLIZ-UHFFFAOYSA-N 0.000 abstract 1
- 150000001735 carboxylic acids Chemical class 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 5
- 230000004048 modification Effects 0.000 description 5
- 238000012986 modification Methods 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 150000002148 esters Chemical class 0.000 description 4
- 239000007864 aqueous solution 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
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- 230000000740 bleeding effect Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- OFTXZYLODJJDPV-UHFFFAOYSA-N ethyl-(fluoromethoxy)-dimethoxysilane Chemical compound FCO[Si](OC)(OC)CC OFTXZYLODJJDPV-UHFFFAOYSA-N 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- WZZBNLYBHUDSHF-DHLKQENFSA-N 1-[(3s,4s)-4-[8-(2-chloro-4-pyrimidin-2-yloxyphenyl)-7-fluoro-2-methylimidazo[4,5-c]quinolin-1-yl]-3-fluoropiperidin-1-yl]-2-hydroxyethanone Chemical group CC1=NC2=CN=C3C=C(F)C(C=4C(=CC(OC=5N=CC=CN=5)=CC=4)Cl)=CC3=C2N1[C@H]1CCN(C(=O)CO)C[C@@H]1F WZZBNLYBHUDSHF-DHLKQENFSA-N 0.000 description 1
- HXKKHQJGJAFBHI-UHFFFAOYSA-N 1-aminopropan-2-ol Chemical compound CC(O)CN HXKKHQJGJAFBHI-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- WUGQZFFCHPXWKQ-UHFFFAOYSA-N Propanolamine Chemical compound NCCCO WUGQZFFCHPXWKQ-UHFFFAOYSA-N 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229920005551 calcium lignosulfonate Polymers 0.000 description 1
- RYAGRZNBULDMBW-UHFFFAOYSA-L calcium;3-(2-hydroxy-3-methoxyphenyl)-2-[2-methoxy-4-(3-sulfonatopropyl)phenoxy]propane-1-sulfonate Chemical compound [Ca+2].COC1=CC=CC(CC(CS([O-])(=O)=O)OC=2C(=CC(CCCS([O-])(=O)=O)=CC=2)OC)=C1O RYAGRZNBULDMBW-UHFFFAOYSA-L 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 description 1
- 229940043237 diethanolamine Drugs 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 125000005456 glyceride group Chemical group 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- JAXFJECJQZDFJS-XHEPKHHKSA-N gtpl8555 Chemical group OC(=O)C[C@H](N)C(=O)N[C@@H](CCC(O)=O)C(=O)N[C@@H](C(C)C)C(=O)N[C@@H](C(C)C)C(=O)N1CCC[C@@H]1C(=O)N[C@H](B1O[C@@]2(C)[C@H]3C[C@H](C3(C)C)C[C@H]2O1)CCC1=CC=C(F)C=C1 JAXFJECJQZDFJS-XHEPKHHKSA-N 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 235000012907 honey Nutrition 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- ZLVXBBHTMQJRSX-VMGNSXQWSA-N jdtic Chemical group C1([C@]2(C)CCN(C[C@@H]2C)C[C@H](C(C)C)NC(=O)[C@@H]2NCC3=CC(O)=CC=C3C2)=CC=CC(O)=C1 ZLVXBBHTMQJRSX-VMGNSXQWSA-N 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000013379 molasses Nutrition 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920000223 polyglycerol Polymers 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 229920005552 sodium lignosulfonate Polymers 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 125000002023 trifluoromethyl group Chemical group FC(F)(F)* 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
Abstract
The invention discloses a kind of modified cement grinding aids and preparation method thereof, which is prepared from the following raw materials of the following mass：100 140 parts of absolute ethyl alcohol, 12 16 parts of ammonium hydroxide, 18 24 parts of ethyl orthosilicate, 8 12 parts of methyltriethoxysilane, 58 parts of silicon fluoride, 20 35 parts of polymerized polyalcohol mother liquor, 48 parts of triethanolamine, 28 parts of polyacrylate, 28 parts of styrene-acrylate, 3 10 parts of polyvinyl alcohol, 28 parts of carboxylic acid sodium, 48 parts of blackstrap, 36 parts of propylene glycol, 15 45 parts of water.The present invention utilizes fluorine-containing Nano-meter SiO_22Modified cement grinding aid, fluorine-containing Nano-meter SiO_22Volume it is smaller when can significantly improve mill efficiency so that after grinding cement granules have bigger specific surface area and smaller screen over-size, significantly improve the early strength of cement, effectively improve the water-retaining property of cement after grinding.
Description
Technical field
The present invention relates to the production fields of cement, more particularly, to a kind of fluorine-containing Nano-meter SiO_22Modified cement grinding aid and
Preparation method.
Technical background
Grinding process energy consumption in manufacture of cement is high, and when carrying out further fine grinding and Ultrafine Grinding to mineral, energy
Consume higher.Therefore, the energy consumption in grinding process is reduced, powder efficient utilization is improved and is of great significance.Cement grinding aid is that one kind carries
High grinding efficiency improves material grindability energy in manufacture of cement, and a kind of production auxiliary agent that addition content is little.In cement grinding mistake
Cheng Zhong, grinding aid can significantly improve mill efficiency, substantially reduce grinding pow consumption, especially be imitated during fine grinding and Ultrafine Grinding
Fruit is more preferable.Meanwhile grinding aid can also improve the early strength of cement, on the basis of not damaging cement self performance, reduce water
Mud production cost.Cement granules are gradually refined with grinding, the particle surface generation charge due to fracture of chemical bond, between particle
Mutually absorption generates reunion, and mill efficiency is made to be greatly reduced.Grinding aid acts between the particle of cement material, reduces particle
Surface energy, principle are to prevent particle aggregation, improve its mobility, improve mill efficiency, to energy-saving and emission-reduction.
Currently, the grinding aid used in cement plant is generally alcohol-based liquid grinding aid, and there are powder for current cement grinding aid
Grind the shortcomings of efficiency is relatively low, early stage cement mechanical strength promotes inadequate and after grinding water mud poor water retention property.
Invention content
In order to solve the above technical problems, the present invention provides a kind of fluorine-containing Nano-meter SiO_2s2Modified cement grinding aid and its system
Preparation Method.
The technical solution adopted in the present invention is：
A kind of modified cement grinding aid is prepared from the following raw materials of the following mass：100-140 parts of absolute ethyl alcohol, ammonium hydroxide
12-16 parts, 18-24 parts of ethyl orthosilicate, 8-12 parts of methyltriethoxysilane, 5-8 parts of silicon fluoride, polymerized polyalcohol mother liquor
20-35 parts, 4-8 parts of triethanolamine, 2-8 parts of polyacrylate, 2-8 parts of cinnamic acrylic ester, 3-10 parts of polyvinyl alcohol, carboxylic
Sour sodium 2-8 parts, 4-8 parts of blackstrap, 3-6 parts of propylene glycol, 15-45 parts of water.
Further, the silicon fluoride is nine fluoro ethyl trimethyl oxysilane, 17 silicon fluorides or trifluoromethyl front three
Base silane.
Further, the carboxylic acid sodium is AEO carboxylic acid sodium.
The preparation method of above-mentioned modified cement grinding aid, includes the following steps：
(1) 5-15 parts of 100-140 parts of absolute ethyl alcohol, 12-16 parts of ammonium hydroxide and water are sufficiently mixed in flask, then successively
18-24 parts of ethyl orthosilicate, 8-12 parts of methyltriethoxysilane is added, 1h-3h is reacted at 55-65 DEG C, adds silicon fluoride
5-8 parts, continues insulation reaction, be aged under the conditions of being placed on 18-22 DEG C, obtain fluorine-containing Nano-meter SiO_22Gel；
(2) by 2-8 parts of 20-35 parts of polymerized polyalcohol mother liquor, 2-8 parts of polyacrylate and cinnamic acrylic ester heating
To 60-95 DEG C, mechanical agitation reacts 1-3h in 60-95 DEG C of water-bath, obtains hydramine after then ultrasonic wave is dispersed to uniformly
Ester type compound；
(3) the fluorine-containing Nano-meter SiO_2 that step (1) obtains is added in the hydramine ester type compound that step (2) obtains2Gel,
After ultrasonic wave is dispersed to uniformly, 2-4h is reacted under the conditions of 60-95 DEG C, obtains fluorine-containing Nano-meter SiO_22Modified hydramine esters chemical combination
Object；
(4) the fluorine-containing Nano-meter SiO_2 obtained in step (3)210-30 parts of water is added in modified hydramine ester type compound, surpasses
After sound wave is dispersed to uniformly, 4-8 parts of triethanolamine, 3-10 parts of polyvinyl alcohol, 2-8 parts of carboxylic acid sodium, blackstrap 4-8 is then added
Part, 3-6 parts of propylene glycol, ultrasonic wave are dispersed to uniformly, and modified cement grinding aid is obtained after standing.
Wherein, in step (1), the time of insulation reaction is 2-4h, and the time of ageing is 12h-48h.
It is described to be heated to be heating water bath in step (2), mechanical agitation 20-30min, then ultrasonic wave disperse 10-20min
To uniform.
In step (3), ultrasonic wave disperses 5-20min to uniform.
In step (4), after water is added, ultrasonic wave disperses 30-50min, and other raw materials are then added, and continues ultrasonic wave dispersion
10-30min。
Beneficial effects of the present invention are：The present invention utilizes fluorine-containing Nano-meter SiO_22Modified cement grinding aid, fluorine-containing Nano-meter SiO_22's
Volume can significantly improve mill efficiency when smaller so that cement granules have the specific surface area of bigger and smaller after grinding
Screen over-size significantly improves the early strength of cement, effectively improves the water-retaining property of cement after grinding.
Specific implementation mode
The present invention is carried out with reference to embodiment explanation is explained in detail.
From yangtze river in nanjing Jiang Yu greases Co., Ltd, (it is main for the polymerized polyalcohol mother liquor purchase used in the following example
Ingredient is polyglycerol, glyceride, glycerine；Solid content ＞ 85%), remaining raw material is commercially available.
Embodiment 1
A kind of modified cement grinding aid is prepared from the following raw materials of the following mass：120 parts of absolute ethyl alcohol, 15 parts of ammonium hydroxide,
20 parts of ethyl orthosilicate, 10 parts of methyltriethoxysilane, 6 parts of silicon fluoride, 30 parts of polymerized polyalcohol mother liquor, 8 parts of triethanolamine,
4 parts of polyacrylate, 6 parts of cinnamic acrylic ester, 5 parts of polyvinyl alcohol, 4 parts of AEO carboxylic acid sodium, blackstrap
6 parts, 3 parts of propylene glycol, 30 parts of water.
The preparation method of the modification cement grinding aid includes the following steps：
(1) 10 parts of 120 parts of absolute ethyl alcohol, 15 parts of ammonium hydroxide and water are sufficiently mixed 15min in three-necked flask (ammonium hydroxide is most
Final concentration of 1mol/L), 10 parts of 20 parts of ethyl orthosilicate and methyltriethoxysilane are sequentially added later, are reacted at 60 DEG C
2h adds nine 6 parts of fluoro ethyl trimethyl oxysilane, continues insulation reaction 2h, is aged 12h under the conditions of being placed on 20 DEG C, obtains
To fluorine-containing Nano-meter SiO_22Gel；
(2) by 30 parts of polymerized polyalcohol mother liquor, 6 parts of heating water baths of 4 parts of polyacrylate and cinnamic acrylic ester to 65
DEG C, mechanical agitation 25min, then ultrasonic wave disperse 20min to uniformly after, react 2h in 65 DEG C of water-bath, obtain alkanolamine ester
Class compound；
(3) the fluorine-containing Nano-meter SiO_2 that step (1) obtains is added in the hydramine ester type compound that step (2) obtains2Gel,
Ultrasonic wave disperse 10min to uniformly after, react 2h in 65 DEG C of water-bath, obtain fluorine-containing Nano-meter SiO_22Modified hydramine esters
Close object；
(4) 65 DEG C of bath temperature is maintained, in the fluorine-containing Nano-meter SiO_2 that step (3) obtains2In modified hydramine ester type compound
20 parts of water is added, ultrasonic wave disperses 30min, obtains the aqueous solution of hydramine ester type compound；In the solution configured, three second are added
8 parts of hydramine, 5 parts of polyvinyl alcohol, 4 parts of AEO carboxylic acid sodium, 6 parts of blackstrap, 3 parts of propylene glycol, then ultrasonic wave
Disperse 30min, last solution left standstill is for 24 hours.After standing, discharging after the assay was approved is packed up to cement grinding aid.
The cement grinding aid that the present embodiment 1 obtains after testing has no irritating odor, solid content is qualified, pH value is qualified, chlorine from
Sub- content is qualified, complies fully with the requirement of GB/T26748-2011.
Embodiment 2
A kind of modified cement grinding aid is prepared from the following raw materials of the following mass：100 parts of absolute ethyl alcohol, 12 parts of ammonium hydroxide,
18 parts of ethyl orthosilicate, 8 parts of methyltriethoxysilane, 5 parts of silicon fluoride, 20 parts of polymerized polyalcohol mother liquor, 5 parts of triethanolamine,
2 parts of polyacrylate, 8 parts of cinnamic acrylic ester, 10 parts of polyvinyl alcohol, 8 parts of AEO carboxylic acid sodium, useless sugar
4 parts of honey, 6 parts of propylene glycol, 15 parts of water.
The preparation method of the modification cement grinding aid includes the following steps：
(1) 5 parts of 100 parts of absolute ethyl alcohol, 12 parts of ammonium hydroxide and distilled water are sufficiently mixed 20min (ammonium hydroxide in three-necked flask
Ultimate density be 0.8mol/L), 8 parts of 18 parts of ethyl orthosilicate and methyltriethoxysilane are sequentially added later, at 55 DEG C
3h is reacted, 5 parts of 17 silicon fluoride is added, continues insulation reaction 3h, 48h is aged under the conditions of being placed on 18 DEG C and is received to get fluorine-containing
Rice SiO2Gel；
(2) by 20 parts of polymerized polyalcohol mother liquor, 8 parts of heating water baths of 2 parts of polyacrylate and cinnamic acrylic ester to 60
DEG C, mechanical agitation 20min, then ultrasonic wave disperse 15min to uniformly after, react 3h in 55 DEG C of water-bath, obtain alkanolamine ester
Class compound；
(3) the fluorine-containing Nano-meter SiO_2 that step (1) obtains is added in the hydramine ester type compound that step (2) obtains2Gel,
Ultrasonic wave disperse 20min to uniformly after, react 4h in 60 DEG C of water-bath, obtain fluorine-containing Nano-meter SiO_22Modified hydramine esters
Close object；
(4) 60 DEG C of bath temperature is maintained, in the fluorine-containing Nano-meter SiO_2 that step (3) obtains2In modified hydramine ester type compound
10 parts of water is added, ultrasonic wave disperses 50min, obtains the aqueous solution of hydramine ester type compound；In the solution configured, three second are added
5 parts of hydramine, 10 parts of polyvinyl alcohol, 8 parts of AEO carboxylic acid sodium, 4 parts of blackstrap, 6 parts of propylene glycol, then ultrasonic wave
Disperse 10min, last solution left standstill for 24 hours, obtains fluorine-containing Nano-meter SiO_22Modified cement grinding aid.
Embodiment 3
A kind of modified cement grinding aid is prepared from the following raw materials of the following mass：140 parts of absolute ethyl alcohol, 16 parts of ammonium hydroxide,
24 parts of ethyl orthosilicate, 12 parts of methyltriethoxysilane, 8 parts of silicon fluoride, 35 parts of polymerized polyalcohol mother liquor, 4 parts of triethanolamine,
8 parts of polyacrylate, 2 parts of cinnamic acrylic ester, 3 parts of polyvinyl alcohol, 2 parts of AEO carboxylic acid sodium, blackstrap
8 parts, 3 parts of propylene glycol, 45 parts of water.
The preparation method of the modification cement grinding aid includes the following steps：
(1) 15 parts of 140 parts of absolute ethyl alcohol, 16 parts of ammonium hydroxide and water are sufficiently mixed 20min in three-necked flask (ammonium hydroxide is most
Final concentration of 1.2mol/L), 12 parts of 24 parts of ethyl orthosilicate and methyltriethoxysilane are sequentially added later, are reacted at 65 DEG C
1h, adds 8 parts of trifluoromethyl trimethylsilane, continues insulation reaction 4h, be aged under the conditions of being placed on 22 DEG C 36h to get containing
Fluorine Nano-meter SiO_22Gel；
(2) by 35 parts of polymerized polyalcohol mother liquor, 2 parts of heating water baths of 8 parts of polyacrylate and cinnamic acrylic ester to 95
DEG C, mechanical agitation 30min, then ultrasonic wave disperse 10min to uniformly after, react 1h in 95 DEG C of water-bath, obtain alkanolamine ester
Class compound；
(3) the fluorine-containing Nano-meter SiO_2 that step (1) obtains is added in the hydramine ester type compound that step (2) obtains2Gel,
Ultrasonic wave disperse 5min to uniformly after, react 3h in 95 DEG C of water-bath, obtain fluorine-containing Nano-meter SiO_22Modified hydramine esters
Close object；
(4) 95 DEG C of bath temperature is maintained, in the fluorine-containing Nano-meter SiO_2 that step (2) obtains2In modified hydramine ester type compound
30 parts of water is added, ultrasonic wave disperses 30min, obtains the aqueous solution of hydramine ester type compound；In the solution configured, three second are added
4 parts of hydramine, 3 parts of polyvinyl alcohol, 2 parts of AEO carboxylic acid sodium, 8 parts of blackstrap, 3 parts of propylene glycol, then ultrasonic wave
Disperse 20min, last solution left standstill for 24 hours, obtains fluorine-containing Nano-meter SiO_22Modified cement grinding aid product.
By cement grinding aid made from the embodiment of the present invention 1 and commercially available cement grinding aid, (commercially available cement grinding aid is
Polyhydric alcohol amine class I liquid I grinding aid, key component are triethanolamine, diethanol amine, three b propanol amine, diethanol monoisopropanolamine,
Molasses, the wooden sodium and calcium lignosulfonate etc.) it is respectively added in PC42.5 cement, cement sample A, B is obtained, not add any grinding aid
Cement sample is C.The water retention property of cement, the mechanical property of grinding aid grinding aid performance and cement are tested respectively, and test result is such as
Shown in table 1- tables 3.
The cement bleeding rate of 1 different time of table is tested
2 cement grinding aid grinding aid performance test of table
3 cement performance of table is tested and analysis
As shown in table 1, cement grinding aid of the invention can significantly improve the water-retaining property of after grinding water mud, reduce bleeding rate；
As shown in table 2, cement grinding aid of the invention significantly improves the specific surface area of cement, reduces screen over-size；As shown in table 3,
Simultaneously on the basis of not influencing cement base fluidity and setting time, cement grinding aid of the invention significantly improves cement
Early mechanics characteristics.Therefore, the present invention utilizes fluorine-containing Nano-meter SiO_22Modified cement grinding aid has preferable grinding-aid effect.
Cement grinding aid provided by the present invention and preparation method thereof is described in detail above.It is used herein
Principle and implementation of the present invention are described for specific case, and the explanation of above example is only intended to help to understand this
The method and its core concept of invention.It should be pointed out that for those skilled in the art, not departing from this hair
, can be with several improvements and modifications are made to the present invention under the premise of bright principle, these improvement and modification also fall into power of the present invention
In the protection domain that profit requires.
Claims (8)
1. a kind of modified cement grinding aid, which is characterized in that the cement grinding aid is prepared from the following raw materials of the following mass：Nothing
100-140 parts of water-ethanol, 12-16 parts of ammonium hydroxide, 18-24 parts of ethyl orthosilicate, 8-12 parts of methyltriethoxysilane, silicon fluoride 5-
8 parts, 20-35 parts of polymerized polyalcohol mother liquor, 4-8 parts of triethanolamine, 2-8 parts of polyacrylate, 2-8 parts of cinnamic acrylic ester,
3-10 parts of polyvinyl alcohol, 2-8 parts of carboxylic acid sodium, 4-8 parts of blackstrap, 3-6 parts of propylene glycol, 15-45 parts of water.
2. modified cement grinding aid according to claim 1, which is characterized in that the silicon fluoride is nine fluoro ethyl trimethyls
Oxysilane, 17 silicon fluorides or trifluoromethyl trimethylsilane.
3. modified cement grinding aid according to claim 1, which is characterized in that the carboxylic acid sodium is aliphatic alcohol polyethenoxy
Ether carboxylic acid sodium.
4. a kind of method preparing modified cement grinding aid described in claim 1, which is characterized in that this method includes following step
Suddenly：
(1) 5-15 parts of 100-140 parts of absolute ethyl alcohol, 12-16 parts of ammonium hydroxide and water are sufficiently mixed in flask, are then sequentially added
18-24 parts of ethyl orthosilicate, 8-12 parts of methyltriethoxysilane react 1h-3h at 55-65 DEG C, add silicon fluoride 5-8
Part, continue insulation reaction, is aged under the conditions of being placed on 18-22 DEG C, obtains fluorine-containing Nano-meter SiO_22Gel；
(2) 2-8 parts of 20-35 parts of polymerized polyalcohol mother liquor, 2-8 parts of polyacrylate and cinnamic acrylic ester are heated to 60-
95 DEG C, mechanical agitation reacts 1-3h in 60-95 DEG C of water-bath, obtains hydramine esters after then ultrasonic wave is dispersed to uniformly
Close object；
(3) the fluorine-containing Nano-meter SiO_2 that step (1) obtains is added in the hydramine ester type compound that step (2) obtains2Gel, ultrasonic wave
After being dispersed to uniformly, 2-4h is reacted under the conditions of 60-95 DEG C, obtains fluorine-containing Nano-meter SiO_22Modified hydramine ester type compound；
(4) the fluorine-containing Nano-meter SiO_2 obtained in step (3)210-30 parts of water, ultrasonic wavelength-division are added in modified hydramine ester type compound
After being dissipated to uniformly, 4-8 parts of triethanolamine, 3-10 parts of polyvinyl alcohol, 2-8 parts of carboxylic acid sodium, 4-8 parts of blackstrap, the third two are then added
3-6 parts of alcohol, ultrasonic wave are dispersed to uniformly, and modified cement grinding aid is obtained after standing.
5. the preparation method of modified cement grinding aid according to claim 4, which is characterized in that in step (1), heat preservation is anti-
The time answered is 2-4h, and the time of ageing is 12h-48h.
6. the preparation method of modified cement grinding aid according to claim 4, which is characterized in that described to add in step (2)
Heat is heating water bath, mechanical agitation 20-30min, and then ultrasonic wave disperses 10-20min to uniform.
7. the preparation method of modified cement grinding aid according to claim 4, which is characterized in that in step (3), ultrasonic wave
Disperse 5-20min to uniform.
8. the preparation method of modified cement grinding aid according to claim 4, which is characterized in that in step (4), water is added
Afterwards, ultrasonic wave disperses 30-50min, and other raw materials are then added, and continues ultrasonic wave and disperses 10-30min.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| CN113698130A (en) * | 2021-09-16 | 2021-11-26 | 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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| 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 |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN113698130A (en) * | 2021-09-16 | 2021-11-26 | 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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| CN108529923B (en) | 2024-02-13 |
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