CN108706899B - Preparation method of modified cement dispersant - Google Patents
Preparation method of modified cement dispersant Download PDFInfo
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- CN108706899B CN108706899B CN201810523340.0A CN201810523340A CN108706899B CN 108706899 B CN108706899 B CN 108706899B CN 201810523340 A CN201810523340 A CN 201810523340A CN 108706899 B CN108706899 B CN 108706899B
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- 239000004568 cement Substances 0.000 title claims abstract description 41
- 239000002270 dispersing agent Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 39
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000000203 mixture Substances 0.000 claims abstract description 30
- 238000010438 heat treatment Methods 0.000 claims abstract description 29
- -1 polyoxyethylene monomethyl ether methacrylate Polymers 0.000 claims abstract description 27
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 22
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000000926 separation method Methods 0.000 claims abstract description 16
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 239000005543 nano-size silicon particle Substances 0.000 claims abstract description 13
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims abstract description 11
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229920005551 calcium lignosulfonate Polymers 0.000 claims abstract description 11
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims abstract description 9
- 239000007864 aqueous solution Substances 0.000 claims abstract description 9
- 239000008367 deionised water Substances 0.000 claims abstract description 9
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 9
- 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 claims abstract description 8
- 238000003760 magnetic stirring Methods 0.000 claims abstract description 8
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 7
- 230000003472 neutralizing effect Effects 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- 239000000243 solution Substances 0.000 claims description 13
- 239000002245 particle Substances 0.000 claims description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 238000011049 filling Methods 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims 2
- 239000000843 powder Substances 0.000 claims 1
- 239000000377 silicon dioxide Substances 0.000 claims 1
- 239000002253 acid Substances 0.000 abstract description 3
- 239000004566 building material Substances 0.000 abstract description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 abstract description 2
- 229910000077 silane Inorganic materials 0.000 abstract description 2
- 239000011863 silicon-based powder Substances 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 239000004408 titanium dioxide Substances 0.000 abstract description 2
- 239000003513 alkali Substances 0.000 abstract 1
- 238000005119 centrifugation Methods 0.000 abstract 1
- 230000007935 neutral effect Effects 0.000 abstract 1
- 239000003638 chemical reducing agent Substances 0.000 description 16
- 239000004567 concrete Substances 0.000 description 15
- 239000000654 additive Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 229920005646 polycarboxylate Polymers 0.000 description 3
- 230000000996 additive effect Effects 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 229920000578 graft copolymer Polymers 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 150000002790 naphthalenes Chemical class 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- WPJGWJITSIEFRP-UHFFFAOYSA-N 1,3,5-triazine-2,4,6-triamine;hydrate Chemical compound O.NC1=NC(N)=NC(N)=N1 WPJGWJITSIEFRP-UHFFFAOYSA-N 0.000 description 1
- 229920001732 Lignosulfonate Polymers 0.000 description 1
- 229920000877 Melamine resin Polymers 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000740 bleeding effect Effects 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000005357 flat glass Substances 0.000 description 1
- NVVZQXQBYZPMLJ-UHFFFAOYSA-N formaldehyde;naphthalene-1-sulfonic acid Chemical compound O=C.C1=CC=C2C(S(=O)(=O)O)=CC=CC2=C1 NVVZQXQBYZPMLJ-UHFFFAOYSA-N 0.000 description 1
- 239000004574 high-performance concrete Substances 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- IIACRCGMVDHOTQ-UHFFFAOYSA-M sulfamate Chemical compound NS([O-])(=O)=O IIACRCGMVDHOTQ-UHFFFAOYSA-M 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010998 test method Methods 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
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/16—Sulfur-containing compounds
- C04B24/18—Lignin sulfonic acid or derivatives thereof, e.g. sulfite lye
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
- C08F283/065—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals on to unsaturated polyethers, polyoxymethylenes or polyacetals
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F289/00—Macromolecular compounds obtained by polymerising monomers on to macromolecular compounds not provided for in groups C08F251/00 - C08F287/00
-
- 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
- C04B2103/40—Surface-active agents, dispersants
- C04B2103/408—Dispersants
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
- Emulsifying, Dispersing, Foam-Producing Or Wetting Agents (AREA)
Abstract
A preparation method of a modified cement dispersant belongs to the technical field of building materials. The preparation process comprises the following steps: adding polyoxyethylene monomethyl ether methacrylate and acid liquor into nano titanium dioxide, and heating in a water bath under the condition of magnetic stirring; cooling the mixture to room temperature after heating, then carrying out centrifugal separation, washing the mixture after centrifugation with deionized water, and drying; taking acrylic acid, calcium lignosulphonate, nano silicon powder and ethanol, stirring, heating and reacting; adding the dried substance and an ammonium persulfate aqueous solution into the mixture after the reaction, and then heating for reaction; and neutralizing the reaction product to be neutral by using alkali liquor after the reaction is finished, and finally preparing the modified cement dispersant. According to the invention, the nanometer titanium dioxide modified polyoxyethylene monomethyl ether methacrylate, acrylic acid, calcium lignosulfonate, nanometer silane and ethanol are mixed, and especially, nanometer silicon powder is added to play a role in synergy, so that the dispersibility of the modified cement dispersant prepared by the invention on cement is greatly improved.
Description
Technical Field
The invention belongs to the technical field of building materials, and particularly relates to a preparation method of a modified cement dispersant.
Background
The cement dispersant, also called water reducing agent, can reduce the mixing water consumption of concrete under the condition of not influencing the fluidity of the concrete, or increase the fluidity of concrete mixture under the condition of not influencing the water consumption, or both, and is an additive with the functions of reducing water and enhancing. The cement dispersant is mainly used in engineering for reducing water consumption of concrete, lowering water cement ratio, saving cement and improving workability.
After the cement dispersant is applied, the flowability and strength of concrete can be greatly improved, and thus the engineering quality is improved. Concrete is the most used building material in the world, and cement dispersant has become an essential additive in concrete production. At present, in developed countries and regions, the amount of cement dispersant in concrete is more than 80%. The cement dispersant mainly comprises the following components: a modified lignosulfonate water reducing agent; a naphthalenesulfonic acid formaldehyde condensate water reducing agent; a melamine water reducing agent; a sulfamate water reducing agent; an aliphatic water reducing agent; a carboxylic acid graft copolymer water reducing agent.
The polycarboxylate graft copolymer water reducing agent is a novel high-performance water reducing agent at present, and has the following advantages: high water reducing rate, small slump loss and high later strength: the 28d strength increase is more than 40%. The mixing amount is small, and is generally below 1%. Although the Zeta potential value of the surface of cement particles of the cement paste mixed with the water reducing agent is smaller than that of naphthalene series or melamine, the slump constant is not lost basically within 1-2 hours. The reason for this is that the carboxylate ions react with Ca in the cement paste2+In combination, the hydration rate is slowed down without a rapid decrease in the water reducer concentration due to the relatively small amount of hydrate. In addition, the main side chain molecular structure form of the polycarboxylate is determined to be three-dimensional zigzag adsorption on the cement surface, which is different from the horizontal adsorption mode of naphthalene series, so that the polycarboxylate has a three-dimensional potential protection effect and can keep a dispersion stable state for a long time. The water reducing agent is suitable for high-performance concrete. Its disadvantages are: poor compatibility and poor predictability in concrete, such as: when the polycarboxylic acid water reducing agent is used together with other additives, the concrete slump loss is too fast, the phenomena of quick hardening and the like easily occur, and the compatibility problem of cement and chemical additives exists; in concrete using a high performance water reducing agent, when the slump increases as the unit water amount decreases, the following problems often occur: the water reducing agent consumption is too large, the concrete viscosity is too large, the segregation and bleeding phenomena occur, and the pumping is difficult. And the polycarboxylic acid water reducing agent has complex synthesis process and expensive raw materials.
Disclosure of Invention
The technical problem to be solved is as follows: aiming at the technical problems, the invention provides a preparation method of a modified cement dispersant, which has the advantages of low energy consumption, low production cost and the like, and the prepared dispersant can improve various performances of concrete, has no pollution to the environment and is harmless to human bodies.
The technical scheme is as follows: a preparation method of a modified cement dispersant, comprising the following steps:
step one, weighing 8-12 parts by mass of nano titanium dioxide, adding 30-50 parts by mass of polyoxyethylene monomethyl ether methacrylate and 60-80 parts by mass of 5 vt.% HCl solution, and heating in a water bath at 80-90 ℃ for 1-2 hours under the condition of magnetic stirring;
step two, cooling the mixture to room temperature after heating, then carrying out centrifugal separation at the rotating speed of 500-650 r/min, washing the mixture after centrifugal separation with deionized water, and drying to obtain the nano titanium dioxide modified polyoxyethylene monomethyl ether methacrylate;
taking 3-5 parts by mass of acrylic acid, 4-6 parts by mass of calcium lignosulfonate, 0.2-0.6 part by mass of nano silicon powder and 70-90 parts by mass of 75wt.% ethanol, heating to 50-60 ℃ under the conditions of stirring and nitrogen filling, and reacting for 30-45 min;
adding 20-30 parts by mass of the nano titanium dioxide modified polyoxyethylene monomethyl ether methacrylate dried in the second step and 2-6 parts by mass of 5wt.% ammonium persulfate aqueous solution into the reacted mixture, and heating to 70-80 ℃ to react for 3-5 h;
and step five, after the reaction is finished, neutralizing the reaction product by using a 30wt.% NaOH solution until the pH value is 7, and finally obtaining the modified cement dispersant.
Preferably, the nano titanium dioxide in the first step is rutile type nano titanium dioxide, and the particle size is 20-50 nm.
Preferably, in the step one, 10 parts by mass of nano titanium dioxide is weighed, 45 parts by mass of polyoxyethylene monomethyl ether methacrylate and 70 parts by mass of 5 vt.% HCl solution are added, and then the mixture is heated in a water bath at 85 ℃ for 1.5 hours under the condition of magnetic stirring.
Preferably, in the second step, after the mixture is heated, the mixture is cooled to room temperature, then centrifugal separation is carried out at the rotating speed of 600r/min, and the mixture after centrifugal separation is washed by deionized water and then dried to obtain the nano titanium dioxide modified polyoxyethylene monomethyl ether methacrylate.
Preferably, the particle size of the nano silicon powder in the third step is 100-200 nm.
Preferably, in the third step, 4 parts by mass of acrylic acid, 5 parts by mass of calcium lignosulfonate, 0.4 part by mass of nano silicon powder and 85 parts by mass of 75wt.% ethanol are taken, stirred and filled with nitrogen, heated to 55 ℃ and reacted for 40 min.
Preferably, in the fourth step, 25 parts by mass of the dried nano titanium dioxide modified polyoxyethylene monomethyl ether methacrylate in the second step and 4 parts by mass of a 5wt.% ammonium persulfate aqueous solution are added into the mixture after the reaction, and then the temperature is raised to 75 ℃ for reaction for 4 hours.
Has the advantages that: the modified cement dispersant prepared by the method is liquid, is dripped into the clinker at a uniform speed during the conveying of the clinker, and the clinker is rapidly dispersed, so that the service life of the ball mill can be prolonged, and the energy consumption and the production cost are reduced. The dispersant can improve various performances of concrete, has no pollution to the environment and is harmless to human bodies. The nanometer titanium dioxide modified polyoxyethylene monomethyl ether methacrylate, acrylic acid, calcium lignosulfonate, nanometer silane and ethanol are mixed, and especially, nanometer silicon powder is added to play a role in synergy, so that the dispersibility of the modified cement dispersant prepared by the invention on cement is greatly improved.
Detailed Description
Example 1
A preparation method of a modified cement dispersant, comprising the following steps:
step one, weighing 8 parts by mass of nano titanium dioxide, adding 30 parts by mass of polyoxyethylene monomethyl ether methacrylate and 60 parts by mass of 5 vt.% HCl solution, and heating in a water bath at 80 ℃ for 1h under the condition of magnetic stirring, wherein the nano titanium dioxide is rutile type nano titanium dioxide, and the particle size is 20-50 nm.
And step two, cooling the mixture to room temperature after heating, then carrying out centrifugal separation at the rotating speed of 500r/min, washing the mixture after centrifugal separation by using deionized water, and drying to obtain the nano titanium dioxide modified polyoxyethylene monomethyl ether methacrylate.
And thirdly, heating 3 parts by mass of acrylic acid, 4 parts by mass of calcium lignosulfonate, 0.2 part by mass of nano silicon powder and 70 parts by mass of 75wt.% ethanol to 50 ℃ under the conditions of stirring and nitrogen filling, and reacting for 30min, wherein the particle size of the nano silicon powder is 100-200 nm.
And step four, adding 20 parts by mass of the dried nano titanium dioxide modified polyoxyethylene monomethyl ether methacrylate in the step two and 2 parts by mass of a 5wt.% ammonium persulfate aqueous solution into the reacted mixture, and then heating to 70 ℃ for reaction for 3 hours.
And step five, after the reaction is finished, neutralizing the reaction product by using a 30wt.% NaOH solution until the pH value is 7, and finally obtaining the modified cement dispersant.
Example 2
A preparation method of a modified cement dispersant, comprising the following steps:
step one, weighing 12 parts by mass of nano titanium dioxide, adding 50 parts by mass of polyoxyethylene monomethyl ether methacrylate and 80 parts by mass of 5 vt.% HCl solution, and heating in a water bath at 90 ℃ for 2 hours under the condition of magnetic stirring, wherein the nano titanium dioxide is rutile type nano titanium dioxide, and the particle size is 20-50 nm.
And step two, cooling the mixture to room temperature after heating, then performing centrifugal separation at the rotating speed of 650r/min, washing the mixture after centrifugal separation by using deionized water, and drying to obtain the nano titanium dioxide modified polyoxyethylene monomethyl ether methacrylate.
And step three, taking 5 parts by mass of acrylic acid, 6 parts by mass of calcium lignosulphonate, 0.6 part by mass of nano silicon powder and 90 parts by mass of 75wt.% ethanol, heating to 60 ℃ under the conditions of stirring and nitrogen filling, and reacting for 45min, wherein the particle size of the nano silicon powder is 100-200 nm.
And step four, adding 30 parts by mass of the dried nano titanium dioxide modified polyoxyethylene monomethyl ether methacrylate in the step two and 6 parts by mass of a 5wt.% ammonium persulfate aqueous solution into the reacted mixture, and then heating to 80 ℃ for reaction for 5 hours.
And step five, after the reaction is finished, neutralizing the reaction product by using a 30wt.% NaOH solution until the pH value is 7, and finally obtaining the modified cement dispersant.
Example 3
A preparation method of a modified cement dispersant, comprising the following steps:
step one, weighing 10 parts by mass of nano titanium dioxide, adding 45 parts by mass of polyoxyethylene monomethyl ether methacrylate and 70 parts by mass of 5 vt.% HCl solution, and heating in a water bath at 85 ℃ for 1.5h under the condition of magnetic stirring, wherein the nano titanium dioxide is rutile type nano titanium dioxide, and the particle size is 20-50 nm.
And step two, cooling the mixture to room temperature after heating, then carrying out centrifugal separation at the rotating speed of 600r/min, washing the mixture after centrifugal separation by using deionized water, and drying to obtain the nano titanium dioxide modified polyoxyethylene monomethyl ether methacrylate.
And thirdly, heating 4 parts by mass of acrylic acid, 5 parts by mass of calcium lignosulfonate, 0.4 part by mass of nano silicon powder and 85 parts by mass of 75wt.% ethanol to 55 ℃ under the conditions of stirring and nitrogen filling, and reacting for 40min, wherein the particle size of the nano silicon powder is 100-200 nm.
And step four, adding 25 parts by mass of the dried nano titanium dioxide modified polyoxyethylene monomethyl ether methacrylate in the step two and 4 parts by mass of a 5wt.% ammonium persulfate aqueous solution into the reacted mixture, and then heating to 75 ℃ to react for 4 hours.
And step five, after the reaction is finished, neutralizing the reaction product by using a 30wt.% NaOH solution until the pH value is 7, and finally obtaining the modified cement dispersant. Comparative example 1
The difference from example 3 is that no nano silicon powder is added, and the specific preparation process is as follows:
step one, weighing 10 parts by mass of nano titanium dioxide, adding 45 parts by mass of polyoxyethylene monomethyl ether methacrylate and 70 parts by mass of 5 vt.% HCl solution, and heating in a water bath at 85 ℃ for 1.5h under the condition of magnetic stirring, wherein the nano titanium dioxide is rutile type nano titanium dioxide, and the particle size is 20-50 nm.
And step two, cooling the mixture to room temperature after heating, then carrying out centrifugal separation at the rotating speed of 600r/min, washing the mixture after centrifugal separation by using deionized water, and drying to obtain the nano titanium dioxide modified polyoxyethylene monomethyl ether methacrylate.
And thirdly, taking 4 parts by mass of acrylic acid, 5 parts by mass of calcium lignosulphonate and 85 parts by mass of 75wt.% ethanol, heating to 55 ℃ under the conditions of stirring and nitrogen filling, and reacting for 40 min.
And step four, adding 25 parts by mass of the dried nano titanium dioxide modified polyoxyethylene monomethyl ether methacrylate in the step two and 4 parts by mass of a 5wt.% ammonium persulfate aqueous solution into the reacted mixture, and then heating to 75 ℃ to react for 4 hours.
And step five, after the reaction is finished, neutralizing the reaction product by using a 30wt.% NaOH solution until the pH value is 7, and finally obtaining the modified cement dispersant.
The modified cement dispersants prepared in examples 1 to 3 and comparative example 1 were tested. Referring to the relevant regulations of the national standard GB.T8077-2000 'test method for homogeneity of concrete admixture', the mixing amount of the samples prepared in the embodiments 1-3 and the comparative example 1 is 0.3 wt% of the cement dosage, the fluidity of the net paste on the plate glass is tested after stirring for three minutes, and the fluidity of the net paste after 30 minutes is tested. The results of the experimental tests are referred to in the table below.
Claims (5)
1. A preparation method of the modified cement dispersant is characterized by comprising the following steps:
step one, weighing 10 parts by mass of nano titanium dioxide, adding 45 parts by mass of polyoxyethylene monomethyl ether methacrylate and 70 parts by mass of 5 vt.% HCl solution, and heating in a water bath at 85 ℃ for 1.5h under the condition of magnetic stirring, wherein the nano titanium dioxide is rutile type nano titanium dioxide, and the particle size is 20-50 nm;
step two, cooling the mixture to room temperature after heating, then carrying out centrifugal separation at the rotating speed of 500-650 r/min, washing the mixture after centrifugal separation with deionized water, and drying to obtain the nano titanium dioxide modified polyoxyethylene monomethyl ether methacrylate;
taking 3-5 parts by mass of acrylic acid, 4-6 parts by mass of calcium lignosulfonate, 0.2-0.6 part by mass of nano silicon powder and 70-90 parts by mass of 75wt.% ethanol, heating to 50-60 ℃ under the conditions of stirring and nitrogen filling, and reacting for 30-45 min;
adding 20-30 parts by mass of the nano titanium dioxide modified polyoxyethylene monomethyl ether methacrylate dried in the second step and 2-6 parts by mass of 5wt.% ammonium persulfate aqueous solution into the reacted mixture, and heating to 70-80 ℃ to react for 3-5 h;
and step five, neutralizing the reaction product by using a 30wt.% NaOH solution until the pH value is 7, and finally obtaining the modified cement dispersant.
2. The preparation method of the modified cement dispersant of claim 1, wherein in the second step, after heating, the mixture is cooled to room temperature, then is centrifugally separated at a rotation speed of 600r/min, and after the centrifugal separation, the mixture is washed by deionized water and then is dried to obtain the nano titanium dioxide modified polyoxyethylene monomethyl ether methacrylate.
3. The preparation method of the modified cement dispersant of claim 1, wherein the particle size of the nano silicon powder in the third step is 100-200 nm.
4. The preparation method of the modified cement dispersant of claim 1, wherein 4 parts by mass of acrylic acid, 5 parts by mass of calcium lignosulfonate, 0.4 part by mass of nano silica powder and 85 parts by mass of 75wt.% ethanol are taken in the third step, and the reaction is carried out for 40min at a temperature of 55 ℃ under the conditions of stirring and nitrogen charging.
5. The preparation method of the modified cement dispersant of claim 1, wherein 25 parts by mass of the dried nano titanium dioxide modified polyoxyethylene monomethyl ether methacrylate of the second step and 4 parts by mass of a 5wt.% ammonium persulfate aqueous solution are added to the reacted mixture in the fourth step, and then the temperature is raised to 75 ℃ for reaction for 4 hours.
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| CN113955967A (en) * | 2021-12-03 | 2022-01-21 | 山西科腾环保新材料股份有限公司 | Nano tackifying additive and preparation method thereof |
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| CN103626424A (en) * | 2012-08-20 | 2014-03-12 | 上海杰事杰新材料(集团)股份有限公司 | Method for preparing polycarboxylic acid water reducer |
| CN104725573A (en) * | 2014-10-11 | 2015-06-24 | 江苏苏博特新材料股份有限公司 | Superplasticizer for facilitating cement hydration, preparation method thereof and application |
| KR20160150463A (en) * | 2015-06-22 | 2016-12-30 | 세명대학교 산학협력단 | Admixture composition having high performance fiber cement |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103626424A (en) * | 2012-08-20 | 2014-03-12 | 上海杰事杰新材料(集团)股份有限公司 | Method for preparing polycarboxylic acid water reducer |
| CN104725573A (en) * | 2014-10-11 | 2015-06-24 | 江苏苏博特新材料股份有限公司 | Superplasticizer for facilitating cement hydration, preparation method thereof and application |
| KR20160150463A (en) * | 2015-06-22 | 2016-12-30 | 세명대학교 산학협력단 | Admixture composition having high performance fiber cement |
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