CN108675665B - Preparation method of slow-release water reducer for concrete - Google Patents
Preparation method of slow-release water reducer for concrete Download PDFInfo
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- CN108675665B CN108675665B CN201810618861.4A CN201810618861A CN108675665B CN 108675665 B CN108675665 B CN 108675665B CN 201810618861 A CN201810618861 A CN 201810618861A CN 108675665 B CN108675665 B CN 108675665B
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- 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
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- 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
- C04B24/161—Macromolecular compounds comprising sulfonate or sulfate groups
- C04B24/163—Macromolecular compounds comprising sulfonate or sulfate groups obtained by reactions only involving carbon-to-carbon unsaturated bonds
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- 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
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- 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
- C04B2103/30—Water reducers, plasticisers, air-entrainers, flow improvers
- C04B2103/302—Water reducers
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention belongs to the technical field of building materials, and particularly relates to a preparation method of a slow-release water reducer for concrete. The preparation method of the slow-release water reducing agent for concrete comprises the steps of controlling the temperature of a reaction kettle at 80 ℃, adding 100 parts of water into the reaction kettle, weighing poplar powder, maleic anhydride, sodium sulfanilate and BPO in a certain mass ratio, adding into the reaction kettle, reacting for 3 hours, adding concentrated sulfuric acid, reacting for 2 hours while keeping the temperature, adding a foaming agent and a foaming regulator, reacting for 1 hour, adjusting the pH of the solution, taking a proper amount of a spin-drying solvent, adding a certain proportion of nano-silica, modified calcium carbonate, a silane coupling agent and an antioxidant, and grinding for 30 minutes at room temperature to obtain the slow-release water reducing agent for concrete; according to the invention, through modification sulfonation of poplar wood powder and addition of nano silicon dioxide, modified calcium carbonate and a silane coupling agent in a certain ratio, the water reducing agent has a certain slow release effect, and is simple in production process and low in cost.
Description
Technical Field
The invention belongs to the technical field of building materials, and particularly relates to a preparation method of a slow-release water reducer for concrete.
Background
The Chinese patent application CN 104119027B discloses a retarding and water reducing agent, which is prepared by mixing the following raw materials in parts by weight: 35-45 parts of beta-naphthalenesulfonate formaldehyde condensate, 20-30 parts of sulfonated acetone-formaldehyde condensate, 10-15 parts of hydroxypropyl methyl cellulose, 6-12 parts of casein, 3-6 parts of mirabilite, 4-8 parts of sulfonated coal tar, 2-4 parts of borax, 5-10 parts of slaked lime, 8-14 parts of activated sludge, 5-10 parts of sodium fluosilicate, 2.5-4.5 parts of oil residue, 2-3 parts of tartaric acid, 3-5 parts of zinc molybdate, 4-6 parts of triethyl phosphate, 2-4 parts of maltodextrin, 4-8 parts of sodium methallyl sulfonate and 3-6 parts of auxiliary agent. The water reducing agent has good retardation effect, can prolong the setting time by 2-4 hours, has the water reducing rate of 15-20 percent, can greatly improve the workability of concrete and various mechanical properties of the concrete, has good adaptability to various cements, has no corrosion effect on reinforcing steel bars, can be used for various reinforced concrete projects, but has complex process and increased cost undoubtedly due to more raw materials.
Chinese patent application CN 104119021A discloses a high-efficiency water reducing agent which is prepared from the following components
The raw materials in parts by weight are mixed: 50-60 parts of beta-naphthalenesulfonate formaldehyde condensate, 20-30 parts of polyethylene glycol monomethyl ether methacrylate, 15-25 parts of calcium lignosulfonate, 10-15 parts of ethylene oxide-propylene oxide copolymer, 2-4 parts of trehalose, 1.5-2.5 parts of silicone powder, 4-8 parts of shale ash, 2.5-4.5 parts of sodium bisulfite, 5-10 parts of polyoxyethylene, 8-14 parts of aluminum tripolyphosphate, 2-3 parts of cocoyl diethanolamine, 1-2 parts of barium dinonyl naphthalene sulfonate, 2-3 parts of urotropine and 3-5 parts of an auxiliary agent. The water reducing agent has high water reducing rate and good fluidity, can obviously improve the fluidity and the working degree of concrete, has obvious early strength effect after final setting, can greatly improve the strength of the concrete at each age, and is suitable for various types of concrete.
It can be seen that the slow-release water reducing agent develops slowly, so that the research and development of the slow-release water reducing agent are particularly important.
Disclosure of Invention
In order to overcome the problems in the prior art, the invention provides a preparation method of a slow-release water reducer for concrete, and the prepared water reducer has a certain slow-release effect, simple production process and lower cost.
The technical scheme adopted by the invention for solving the technical problems is as follows: the invention discloses a preparation method of a slow-release water reducing agent for concrete, which is characterized by comprising the following steps:
(1) controlling the temperature of the reaction kettle at 80 ℃, adding 100 parts of water into the reaction kettle, and weighing the mixture with the mass ratio of 100-: 1-1.5 of poplar powder, maleic anhydride, sodium sulfanilate and BPO are added into a reaction kettle, after reaction for 3 hours, the reaction temperature is reduced by 10 ℃ under high-speed stirring, concentrated sulfuric acid is added dropwise within 1 hour, after reaction for 2 hours under heat preservation, 0.5-0.8 part of foaming agent and 0.2-0.3 part of foaming regulator are added, after reaction for 1 hour, the pH of the solution is adjusted by sodium carbonate/sodium bicarbonate buffer solution, and the solution is kept stand after the solvent is dried by spinning;
(2) and (2) taking 60-80 parts of the particles obtained in the step (1), adding 5-8 parts of nano silicon dioxide, 8-10 parts of modified calcium carbonate, 0.2-0.5 part of silane coupling agent and 1-2 parts of antioxidant, and grinding at room temperature for 30 minutes to obtain the slow-release water reducer for concrete.
Further, the preparation method of the modified calcium carbonate comprises the steps of placing butanone and hydroxyl-containing PVC resin in a reaction kettle according to the mass ratio of 80-100:10-15 at room temperature, stirring for 1 hour, adding 600 parts of common calcium carbonate, controlling the stirring speed at 300rpm, stirring for 10 minutes, adding 8-12 parts of IPDI, stirring for 15 minutes to obtain the modified calcium carbonate, wherein the modified calcium carbonate has obviously increased fluidity after modification, and is convenient for subsequent processing.
Further, the preparation method of the foaming regulator comprises the following steps of controlling the temperature of the reaction kettle to be 70 ℃, rotating at 200rpm, and weighing the components in a mass ratio of 80-100: 10-15: 2-4 of acrylate monomer with higher glass transition temperature, butyl acrylate and acrylic acid, adding 1/8 into a reaction kettle, adding 100 parts of ethyl acetate and 0.3-0.8 part of initiator, reacting for half an hour, gradually dripping the residual monomer, heating to 5 ℃, keeping the temperature, reacting for 6 hours, and taking out to obtain the foaming regulator.
Furthermore, the particle size of the poplar wood powder is 80-100 meshes.
Furthermore, the acceleration of the concentrated sulfuric acid drops must be slow enough, and the concentrated sulfuric acid drops must be stirred at a high speed while being dropped, so that heat accumulation is avoided.
Further, the pH regulator is used for controlling the pH of the system to be 7 +/-0.3.
Further, the antioxidant is obtained by mixing 1-2 parts by mass of glycerol and 2-3 parts by mass of vitamin C.
Advantageous effects
1. According to the water reducer for the slow-release concrete, the nano silicon dioxide, the modified calcium carbonate and the silane coupling agent are added, and after grinding, a certain polymerization reaction is carried out on the surface, so that the water reducer has a slow-release effect, when the water reducer is used, the water reducer is balanced and moves in the direction of releasing water reducer particles along with the increase of the use, the slow-release effect is achieved, the water consumption of the water reducer is reduced, the quality guarantee period of concrete is prolonged, and the concrete is not easy to agglomerate;
2. according to the invention, the modified calcium carbonate is added, and the ratio of butanone to hydroxyl-containing PVC resin is adjusted to modify the calcium carbonate, so that the flowability of the modified calcium carbonate is obviously increased, and the subsequent processing is facilitated.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, preferred embodiments of the present invention will be described in detail below with reference to experimental data to facilitate understanding of the skilled person.
Example 1
The preparation method of the slow-release water reducer for concrete comprises the following steps:
(1) placing butanone and hydroxyl-containing PVC resin in a reaction kettle at room temperature according to the mass ratio of 100:12, stirring for 1h, adding 550 parts of common calcium carbonate, controlling the stirring speed at 300rpm, stirring for 10 minutes, adding 10 parts of IPDI, and stirring for 15 minutes to obtain modified calcium carbonate;
(2) controlling the temperature of the reaction kettle at 70 ℃, rotating at 200rpm, and weighing the components in a mass ratio of 90: 11: 3, adding 1/8 into a reaction kettle, adding 100 parts of ethyl acetate and 0.4 part of initiator, reacting for half an hour, gradually dropwise adding the rest monomers, heating to 5 ℃, keeping the temperature, reacting for 6 hours, and taking out to obtain a foaming regulator;
(3) controlling the temperature of the reaction kettle at 80 ℃, adding 100 parts of water into the reaction kettle, and weighing the components in a mass ratio of 110:22: 28: 1.2 adding poplar powder, maleic anhydride, sodium sulfanilate and BPO into a reaction kettle, reacting for 3 hours, reducing the reaction temperature by 10 ℃ under high-speed stirring, dropwise adding concentrated sulfuric acid into the reaction kettle within 1 hour, keeping the temperature for reacting for 2 hours, then adding 0.6 part of foaming agent and 0.25 part of foaming regulator, reacting for 1 hour, adjusting the pH of the solution by using a sodium carbonate/sodium bicarbonate buffer solution, spin-drying the solvent, taking 75 parts of obtained particles, adding 6 parts of nano-silica, 9 parts of modified calcium carbonate, 0.3 part of silane coupling agent and 1.5 parts of antioxidant, and grinding for 30 minutes at room temperature to obtain the slow-release concrete water reducer.
Example 2
The preparation method of the slow-release water reducer for concrete comprises the following steps:
(1) placing butanone and hydroxyl-containing PVC resin in a reaction kettle according to a mass ratio of 90:11 at room temperature, stirring for 1h, adding 550 parts of common calcium carbonate, controlling the stirring speed at 300rpm, stirring for 10 minutes, adding 8 parts of IPDI, and stirring for 15 minutes to obtain modified calcium carbonate;
(2) controlling the temperature of the reaction kettle at 70 ℃, rotating at 200rpm, and weighing the components in a mass ratio of 100: 13: 3, adding 1/8 into a reaction kettle, adding 100 parts of ethyl acetate and 0.5 part of initiator, reacting for half an hour, gradually dropwise adding the rest monomers, heating to 5 ℃, keeping the temperature, reacting for 6 hours, and taking out to obtain a foaming regulator;
(3) controlling the temperature of the reaction kettle at 80 ℃, adding 100 parts of water into the reaction kettle, and weighing the components in a mass ratio of 100:23: 28: 1.2 adding poplar powder, maleic anhydride, sodium sulfanilate and BPO into a reaction kettle, reacting for 3 hours, reducing the reaction temperature by 10 ℃ under high-speed stirring, dropwise adding concentrated sulfuric acid into the reaction kettle within 1 hour, keeping the temperature for reacting for 2 hours, then adding 0.5 part of foaming agent and 0.25 part of foaming regulator, reacting for 1 hour, adjusting the pH of the solution by using a sodium carbonate/sodium bicarbonate buffer solution, spin-drying the solvent, taking 70 parts of obtained particles, adding 8 parts of nano-silica, 8 parts of modified calcium carbonate, 0.4 part of silane coupling agent and 1 part of antioxidant, and grinding for 30 minutes at room temperature to obtain the slow-release concrete water reducer.
Example 3
The preparation method of the slow-release water reducer for concrete comprises the following steps:
(1) placing butanone and hydroxyl-containing PVC resin in a reaction kettle according to a mass ratio of 85:10 at room temperature, stirring for 1h, adding 500 parts of common calcium carbonate, controlling the stirring speed at 300rpm, stirring for 10 minutes, adding 8 parts of IPDI, and stirring for 15 minutes to obtain modified calcium carbonate;
(2) controlling the temperature of the reaction kettle at 70 ℃, rotating at 200rpm, and weighing the components in a mass ratio of 100: 11: 2, adding 1/8 into a reaction kettle, adding 100 parts of ethyl acetate and 0.4 part of initiator, reacting for half an hour, gradually dropwise adding the rest monomers, heating to 5 ℃, keeping the temperature, reacting for 6 hours, and taking out to obtain a foaming regulator;
(3) controlling the temperature of the reaction kettle at 80 ℃, adding 100 parts of water into the reaction kettle, and weighing the mixture in a mass ratio of 110:20: 30: adding 1 part of poplar powder, maleic anhydride, sodium sulfanilate and BPO into a reaction kettle, reacting for 3 hours, reducing the reaction temperature by 10 ℃ under high-speed stirring, dropwise adding concentrated sulfuric acid into the reaction kettle within 1 hour, keeping the temperature for reacting for 2 hours, then adding 0.5 part of foaming agent and 0.2 part of foaming regulator, reacting for 1 hour, adjusting the pH of the solution by using a sodium carbonate/sodium bicarbonate buffer solution, spin-drying the solvent, taking 80 parts of obtained particles, adding 5 parts of nano-silica, 10 parts of modified calcium carbonate, 0.25 part of silane coupling agent and 1 part of antioxidant, and grinding for 30 minutes at room temperature to obtain the slow-release concrete water reducer.
Example 4
The preparation method of the slow-release water reducer for concrete comprises the following steps:
(1) placing butanone and hydroxyl-containing PVC resin in a reaction kettle at room temperature according to the mass ratio of 100:15, stirring for 1h, adding 600 parts of common calcium carbonate, controlling the stirring speed at 300rpm, stirring for 10 minutes, adding 12 parts of IPDI, and stirring for 15 minutes to obtain modified calcium carbonate;
(2) controlling the temperature of the reaction kettle at 70 ℃, rotating at 200rpm, and weighing the components in a mass ratio of 100: 15: 2, adding 1/8 into a reaction kettle, adding 100 parts of ethyl acetate and 0.3 part of initiator, reacting for half an hour, gradually dropwise adding the rest monomers, heating to 5 ℃, keeping the temperature, reacting for 6 hours, and taking out to obtain a foaming regulator;
(3) controlling the temperature of the reaction kettle at 80 ℃, adding 100 parts of water into the reaction kettle, and weighing the mixture in a mass ratio of 120:25: 30: 1.5 adding poplar powder, maleic anhydride, sodium sulfanilate and BPO into a reaction kettle, reacting for 3 hours, reducing the reaction temperature by 10 ℃ under high-speed stirring, dropwise adding concentrated sulfuric acid into the reaction kettle within 1 hour, preserving the temperature, reacting for 2 hours, then adding 0.5 part of foaming agent and 0.3 part of foaming regulator, reacting for 1 hour, adjusting the pH of the solution by using a sodium carbonate/sodium bicarbonate buffer solution, spin-drying the solvent, taking 75 parts of obtained particles, adding 5 parts of nano-silica, 10 parts of modified calcium carbonate, 0.25 part of silane coupling agent and 2 parts of antioxidant, and grinding for 30 minutes at room temperature to obtain the slow-release concrete water reducer.
Experimental analysis:
1. water reducing agent performance test
| Item | Example 1 | Example 2 | Example 3 | Example 4 | Water reducing agent on the market |
| The water reduction rate% | 30 | 29 | 32 | 27 | 14 |
| Compressive Strength ratio% (3 d) | 166 | 164 | 170 | 159 | 142 |
| Compressive strength ratio% (30 d) | 155 | 154 | 149 | 148 | 112 |
As can be seen from the table, the water reducing agent prepared by the invention obviously reduces the using amount of water, and the prepared product has better mechanical property and can be put into daily use.
Finally, it is noted that the above-mentioned preferred embodiments illustrate rather than limit the invention, and that, although the invention has been described in detail with reference to the above-mentioned preferred embodiments, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the scope of the invention as defined by the appended claims.
Claims (6)
1. The preparation method of the slow-release water reducer for concrete is characterized by comprising the following steps of:
(1) controlling the temperature of the reaction kettle at 80 ℃, adding 100 parts of water into the reaction kettle, and weighing the mixture with the mass ratio of 100-: 1-1.5 of poplar powder, maleic anhydride, sodium sulfanilate and BPO are added into a reaction kettle, after reaction for 3 hours, the reaction temperature is reduced by 10 ℃ under high-speed stirring, concentrated sulfuric acid is added dropwise within 1 hour, after reaction for 2 hours under heat preservation, 0.5-0.8 part of foaming agent and 0.2-0.3 part of foaming regulator are added, after reaction for 1 hour, the pH value of the solution is adjusted by sodium carbonate/sodium bicarbonate buffer solution, and the solution is stood after the solvent is dried by spinning;
(2) taking 60-80 parts of the particles obtained in the step (1), adding 5-8 parts of nano silicon dioxide, 8-10 parts of modified calcium carbonate, 0.2-0.5 part of silane coupling agent and 1-2 parts of antioxidant, and grinding at room temperature for 30 minutes to obtain the slow-release water reducer for concrete;
the preparation method of the modified calcium carbonate comprises the steps of placing butanone and hydroxyl-containing PVC resin in a reaction kettle according to a mass ratio of 80-100:10-15 at room temperature, stirring for 1h, adding 600 parts of common calcium carbonate, controlling the stirring speed at 300rpm, stirring for 10 minutes, adding 8-12 parts of IPDI, stirring for 15 minutes to obtain the modified calcium carbonate, wherein the modified calcium carbonate has obviously increased fluidity and is convenient for subsequent processing.
2. The preparation method of the slow-release water reducer for concrete according to claim 1, wherein the preparation method of the foaming regulator comprises the steps of controlling the temperature of the reaction kettle to be 70 ℃, controlling the rotation speed to be 200rpm, and weighing the components in a mass ratio of 80-100: 10-15: 2-4 of acrylate monomer with higher glass transition temperature, butyl acrylate and acrylic acid, adding 1/8 into a reaction kettle, adding 100 parts of ethyl acetate and 0.3-0.8 part of initiator, reacting for half an hour, gradually dripping the residual monomer, heating to 5 ℃, keeping the temperature, reacting for 6 hours, and taking out to obtain the foaming regulator.
3. The preparation method of the slow-release water reducer for concrete according to claim 1, wherein the particle size of the poplar wood flour is 80-100 meshes.
4. The preparation method of the slow-release water reducer for concrete according to claim 1, wherein the acceleration of the concentrated sulfuric acid drops must be sufficiently slow, and the concentrated sulfuric acid drops must be stirred at a high speed while being dropped, so that heat accumulation is avoided.
5. The preparation method of the slow-release water reducer for concrete according to claim 1, wherein the sodium carbonate/sodium bicarbonate buffer solution is used for controlling the pH of the system to be 7 +/-0.3.
6. The preparation method of the slow-release water reducer for concrete according to claim 1, wherein the antioxidant is prepared by mixing 1-2 parts by mass of glycerin and 2-3 parts by mass of vitamin C.
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| CN110563373B (en) * | 2019-08-29 | 2023-05-23 | 中国电力科学研究院有限公司 | Dispersing agent for nano silicon dioxide and preparation method thereof |
| CN112723901B (en) * | 2021-01-28 | 2022-12-06 | 中电建南方建筑科技有限公司 | Cement foamed concrete and preparation process thereof |
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| FR2944023B1 (en) * | 2009-04-01 | 2013-01-11 | Chryso | PROCESS FOR THE PREPARATION OF SUPERPLASTIFIERS |
| CN104177562B (en) * | 2014-07-30 | 2017-05-10 | 广西红墙新材料有限公司 | Slow-release high-adaptability polyester polycarboxylic acid water-reducing agent and preparation method and application thereof |
| CN106365494A (en) * | 2016-08-30 | 2017-02-01 | 卓达新材料科技集团威海股份有限公司 | Sodium sulfanilate-containing high-efficiency water reducing agent for 3D printing house slurry |
| CN107383289A (en) * | 2017-07-31 | 2017-11-24 | 贵州凯襄新材料有限公司 | A kind of polycarboxylate water-reducer and preparation method thereof |
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