CN108675665A - A kind of preparation method of slow-release concrete water-reducing agent - Google Patents
A kind of preparation method of slow-release concrete water-reducing agent Download PDFInfo
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- CN108675665A CN108675665A CN201810618861.4A CN201810618861A CN108675665A CN 108675665 A CN108675665 A CN 108675665A CN 201810618861 A CN201810618861 A CN 201810618861A CN 108675665 A CN108675665 A CN 108675665A
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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 building material technical fields, and in particular to a kind of preparation method of slow-release concrete water-reducing agent.The preparation method of the slow-release concrete water-reducing agent is:Temperature of reaction kettle is controlled at 80 DEG C, 100 parts of water are added into reaction kettle, weigh certain mass than Poplar Powder, maleic anhydride, sodium sulfanilate and BPO be added in reaction kettle, after reacting 3h, the concentrated sulfuric acid is added, after insulation reaction 2h, add some foaming agents and foaming control agent, after reacting 1h, solution PH is adjusted, solvent is spin-dried for and takes in right amount, a certain proportion of nano silicon dioxide, modified calcium carbonate, silane coupling agent is added, antioxidant grinds 30 minutes, obtains a kind of slow-release concrete water-reducing agent at room temperature；The present invention adds the nano silicon dioxide, modified calcium carbonate, silane coupling agent centainly matched by the modification sulphonation to Poplar Powder so that water-reducing agent has certain slow release effect, and simple production process, cost is relatively low.
Description
Technical field
The invention belongs to building material technical fields, and in particular to a kind of preparation side of slow-release concrete water-reducing agent
Method.
Background technology
104119027 B of Chinese patent application CN disclose a kind of retardation water reducing agent, are mixed by the raw material of following parts by weight
It closes：β-naphthalenesulfonate formaldehyde condensation compound 35-45, sulfonated acetone-formaldehyde condensation products 20-30, hydroxypropyl methyl fiber
Plain 10-15, casein 6-12, saltcake 3-6, sulfonated coal tar 4-8, borax 2-4, calcium hydroxide 5-10, activated sludge 8-
14, prodan 5-10, oil foot 2.5-4.5, tartaric acid 2-3, zinc molybdate 3-5, triethyl phosphate 4-6, maltodextrin 2-
4, methylpropene sodium sulfonate 4-8, auxiliary agent 3-6.The retarding effect of the invention water-reducing agent is good, and setting time can extend 2-4
Hour, water-reducing rate 15%-20% can substantially improve the workability of concrete, improve every mechanical property of concrete,
It is good to various cement adaptabilities, reinforcing bar non-corroding is acted on, can be used for various reinforced concrete works, but the technique is more multiple
Miscellaneous, raw material mostly undoubtedly increases cost.
104119021 A of Chinese patent application CN have disclosed a kind of high efficiency water reducing agent, by following heavy
The raw material of amount part mixes：β-naphthalenesulfonate formaldehyde condensation compound 50-60, polyethylene glycol monomethyl ethermethacrylic acid esters
20-30, calcium lignosulfonate 15-25, ethylene oxide-propylene oxide copolymer 10-15, trehalose 2-4, silicone powder 1.5-
2.5, shale ashes 4-8, sodium hydrogensulfite 2.5-4.5, polyethylene glycol oxide 5-10, aluminium triphosphate 8-14, cocounut oil acyl diethyl
Hydramine 2-3, dinonyl naphthalene sulfonate barium 1-2, methenamine 2-3, auxiliary agent 3-5.Water-reducing agent water-reducing rate of the present invention is high, mobility
It is good, concrete flowability and workability are can obviously improve, early strong effect is notable after final set, can increase substantially concrete each age
Intensity, be suitable for all kinds of concrete.
It can be seen that sustained-release water reducing agent development is slower, therefore a kind of research and development of sustained-release water reducing agent seem particularly heavy
It wants.
Invention content
Of the existing technology to overcome the problems, such as, the present invention provides a kind of preparation side of slow-release concrete water-reducing agent
Method, water-reducing agent, which is made, has certain slow release effect, and simple production process, cost is relatively low.
The present invention solve its technical problem the technical solution adopted is that：Invent a kind of system of slow-release concrete water-reducing agent
Preparation Method, which is characterized in that the preparation method of the slow-release concrete water-reducing agent is：
（1）Temperature of reaction kettle is controlled at 80 DEG C, 100 parts of water are added into reaction kettle, it is 100-120 to weigh mass ratio:20-25:
25-30：Poplar Powder, maleic anhydride, sodium sulfanilate and the BPO of 1-1.5 is added in reaction kettle, after reacting 3h, in high speed
Under stirring, reaction temperature reduces by 10 DEG C, is added dropwise the concentrated sulfuric acid in 1h, after insulation reaction 2h, adds 0.5-0.8 parts of foaming
Agent and 0.2-0.3 parts of foaming control agents after reacting 1h, adjust solution PH, after being spin-dried for solvent with sodium carbonate/bicarbonate buffer solution
It stands；
（2）Take 60-80 parts of steps（1）5-8 parts of nano silicon dioxides, 8-10 parts of modified calcium carbonates, 0.2- are added in obtained particle
0.5 part of silane coupling agent, 1-2 parts of antioxidants grind 30 minutes, obtain a kind of slow-release concrete diminishing at room temperature
Agent.
Further, the preparation method of the modified calcium carbonate is that at room temperature, the polyvinyl chloride resin of butanone and hydroxyl is pressed
Mass ratio 80-100:10-15 is placed in a kettle, is stirred 1h, is added 500-600 parts of ordinary calcium carbonate, stir speed (S.S.) control
System after ten minutes, is added IPDI8-12 parts, stirs 15 minutes, obtain modified calcium carbonate, modified mobility in 300rpm, stirring
It obviously increases, is convenient for following process.
Further, the preparation method of foaming control agent is that control temperature of reaction kettle is 70 DEG C, and rotating speed 200rpm weighs matter
Amount is than being 80-100:10-15：The higher acrylic ester monomer of glass transition temperature, butyl acrylate, the acrylic acid of 2-4,
It takes in 1/8 addition reaction kettle, adds 100 parts of ethyl acetate and 0.3-0.8 parts of initiators, after reacting half an hour, be gradually added dropwise
Residual monomer heats up 5 DEG C, is taken out after insulation reaction 6h, obtains foaming control agent.
Further, the Poplar Powder grain size is in 80-100 mesh.
Further, the concentrated sulfuric acid rate of addition must be slow enough, and has to be added dropwise in high-speed stirred, avoids heat
Amount aggregation.
Further, the effect of the PH conditioning agents is the PH of control system 7 ± 0.3.
Further, the antioxidant is, by mass fraction be 1-2 part glycerine, after the mixing of 2-3 parts of vitamin C
The substance obtained.
Advantageous effect
1, nano silicon dioxide, modified calcium carbonate and silane coupled is added in the slow-release concrete water-reducing agent for preparing of the present invention
After being ground, certain polymerisation has occurred on surface for agent so that water-reducing agent have slow release effect, when in use, with
The increase used balances and is moved to the direction of release water-reducing agent particle, plays slow release effect, and the Water usage of the water-reducing agent
It reduces, and concrete extended shelf-life, it is prevented from caking；
2, the present invention is by being added modified calcium carbonate, by adjusting the polyvinyl chloride resin ratio of butanone and hydroxyl, is carried out to calcium carbonate
Modification so that modified calcium carbonate mobility obviously increases, and is convenient for following process.
Specific implementation mode
In order to keep the purpose of the present invention, technical solution and advantageous effect clearer, below in conjunction with experimental data, to this
The preferred embodiment of invention is described in detail, to facilitate the technical staff to understand.
Embodiment 1
A kind of preparation method of slow-release concrete water-reducing agent includes the following steps：
（1）At room temperature, by the polyvinyl chloride resin of butanone and hydroxyl in mass ratio 100:12 place in a kettle, stir 1h, then add
Entering 550 parts of ordinary calcium carbonate, stir speed (S.S.) control after ten minutes, is added IPDI10 parts, stirs 15 minutes in 300rpm, stirring,
Obtain modified calcium carbonate；
（2）It is 70 DEG C, rotating speed 200rpm to control temperature of reaction kettle, and it is 90 to weigh mass ratio:11：3 glass transition temperature compared with
High acrylic ester monomer, butyl acrylate, acrylic acid, take in 1/8 addition reaction kettle, be added 100 parts of ethyl acetate and
0.4 part of initiator after reacting half an hour, is gradually added dropwise residual monomer, heats up 5 DEG C, taken out after insulation reaction 6h, obtains foaming and adjusts
Save agent；
（3）Temperature of reaction kettle is controlled at 80 DEG C, 100 parts of water are added into reaction kettle, it is 110 to weigh mass ratio:22:28：1.2
Poplar Powder, maleic anhydride, sodium sulfanilate and BPO are added in reaction kettle, after reacting 3h, under high velocity agitation, reaction temperature
Degree reduces by 10 DEG C, is added dropwise the concentrated sulfuric acid in 1h, after insulation reaction 2h, adds 0.6 part of foaming agent and 0.25 part of foaming is adjusted
Agent is saved, after reacting 1h, solution PH is adjusted with sodium carbonate/bicarbonate buffer solution, is spin-dried for solvent, takes 75 parts of obtained particles, add
Enter 6 parts of nano silicon dioxides, 9 parts of modified calcium carbonates, 0.3 part of silane coupling agent, 1.5 parts of antioxidants grind 30 at room temperature
Minute, obtain a kind of slow-release concrete water-reducing agent.
Embodiment 2
A kind of preparation method of slow-release concrete water-reducing agent includes the following steps：
（1）At room temperature, by the polyvinyl chloride resin of butanone and hydroxyl in mass ratio 90:11 place in a kettle, stir 1h, then add
Enter 550 parts of ordinary calcium carbonate, stir speed (S.S.) control after ten minutes, is added IPDI8 parts, stirs 15 minutes, obtain in 300rpm, stirring
To modified calcium carbonate；
（2）It is 70 DEG C, rotating speed 200rpm to control temperature of reaction kettle, and it is 100 to weigh mass ratio:13：3 glass transition temperature compared with
High acrylic ester monomer, butyl acrylate, acrylic acid, take in 1/8 addition reaction kettle, be added 100 parts of ethyl acetate and
0.5 part of initiator after reacting half an hour, is gradually added dropwise residual monomer, heats up 5 DEG C, taken out after insulation reaction 6h, obtains foaming and adjusts
Save agent；
（3）Temperature of reaction kettle is controlled at 80 DEG C, 100 parts of water are added into reaction kettle, it is 100 to weigh mass ratio:23:28：1.2
Poplar Powder, maleic anhydride, sodium sulfanilate and BPO are added in reaction kettle, after reacting 3h, under high velocity agitation, reaction temperature
Degree reduces by 10 DEG C, is added dropwise the concentrated sulfuric acid in 1h, after insulation reaction 2h, adds 0.5 part of foaming agent and 0.25 part of foaming is adjusted
Agent is saved, after reacting 1h, solution PH is adjusted with sodium carbonate/bicarbonate buffer solution, is spin-dried for solvent, takes 70 parts of obtained particles, add
Enter 8 parts of nano silicon dioxides, 8 parts of modified calcium carbonates, 0.4 part of silane coupling agent, 1 part of antioxidant grinds 30 points at room temperature
Clock obtains a kind of slow-release concrete water-reducing agent.
Embodiment 3
A kind of preparation method of slow-release concrete water-reducing agent includes the following steps：
（1）At room temperature, by the polyvinyl chloride resin of butanone and hydroxyl in mass ratio 85:10 place in a kettle, stir 1h, then add
Enter 500 parts of ordinary calcium carbonate, stir speed (S.S.) control after ten minutes, is added IPDI8 parts, stirs 15 minutes, obtain in 300rpm, stirring
To modified calcium carbonate；
（2）It is 70 DEG C, rotating speed 200rpm to control temperature of reaction kettle, and it is 100 to weigh mass ratio:11：2 glass transition temperature compared with
High acrylic ester monomer, butyl acrylate, acrylic acid, take in 1/8 addition reaction kettle, be added 100 parts of ethyl acetate and
0.4 part of initiator after reacting half an hour, is gradually added dropwise residual monomer, heats up 5 DEG C, taken out after insulation reaction 6h, obtains foaming and adjusts
Save agent；
（3）Temperature of reaction kettle is controlled at 80 DEG C, 100 parts of water are added into reaction kettle, it is 110 to weigh mass ratio:20:30：1 poplar
Wood powder, maleic anhydride, sodium sulfanilate and BPO are added in reaction kettle, after reacting 3h, under high velocity agitation, reaction temperature
10 DEG C are reduced, is added dropwise the concentrated sulfuric acid in 1h, after insulation reaction 2h, 0.5 part of foaming agent is added and 0.2 part of foaming is adjusted
Agent after reacting 1h, adjusts solution PH with sodium carbonate/bicarbonate buffer solution, is spin-dried for solvent, take 80 parts of obtained particles, be added 5
Part nano silicon dioxide, 10 parts of modified calcium carbonates, 0.25 part of silane coupling agent, 1 part of antioxidant grind 30 points at room temperature
Clock obtains a kind of slow-release concrete water-reducing agent.
Embodiment 4
A kind of preparation method of slow-release concrete water-reducing agent includes the following steps：
（1）At room temperature, by the polyvinyl chloride resin of butanone and hydroxyl in mass ratio 100:15 place in a kettle, stir 1h, then add
Entering 600 parts of ordinary calcium carbonate, stir speed (S.S.) control after ten minutes, is added IPDI12 parts, stirs 15 minutes in 300rpm, stirring,
Obtain modified calcium carbonate；
（2）It is 70 DEG C, rotating speed 200rpm to control temperature of reaction kettle, and it is 100 to weigh mass ratio:15：2 glass transition temperature compared with
High acrylic ester monomer, butyl acrylate, acrylic acid, take in 1/8 addition reaction kettle, be added 100 parts of ethyl acetate and
0.3 part of initiator after reacting half an hour, is gradually added dropwise residual monomer, heats up 5 DEG C, taken out after insulation reaction 6h, obtains foaming and adjusts
Save agent；
（3）Temperature of reaction kettle is controlled at 80 DEG C, 100 parts of water are added into reaction kettle, it is 120 to weigh mass ratio:25:30：1.5
Poplar Powder, maleic anhydride, sodium sulfanilate and BPO are added in reaction kettle, after reacting 3h, under high velocity agitation, reaction temperature
Degree reduces by 10 DEG C, is added dropwise the concentrated sulfuric acid in 1h, after insulation reaction 2h, adds 0.5 part of foaming agent and 0.3 part of foaming is adjusted
Agent after reacting 1h, adjusts solution PH with sodium carbonate/bicarbonate buffer solution, is spin-dried for solvent, take 75 parts of obtained particles, be added 5
Part nano silicon dioxide, 10 parts of modified calcium carbonates, 0.25 part of silane coupling agent, 2 parts of antioxidants grind 30 points at room temperature
Clock obtains a kind of slow-release concrete water-reducing agent.
Experimental analysis：
1, water-reducing agent performance test
| Project | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Commercially available water-reducing agent |
| Water-reducing rate % | 30 | 29 | 32 | 27 | 14 |
| Compressive strength rate %（3d） | 166 | 164 | 170 | 159 | 142 |
| Compressive strength rate %（30d） | 155 | 154 | 149 | 148 | 112 |
As can be seen from the table, the water-reducing agent that prepared by the present invention is substantially reduced the usage amount of water, and the product mechanical property prepared
It is more excellent, routine use can be put into.
Finally illustrate, preferred embodiment above is only used to illustrate the technical scheme of the present invention and unrestricted, although logical
It crosses above preferred embodiment the present invention is described in detail, however, those skilled in the art should understand that, can be
Various changes are made to it in form and in details, defined by claims of the present invention.
Claims (7)
1. a kind of preparation method of slow-release concrete water-reducing agent, which is characterized in that the slow-release concrete water-reducing agent
Preparation method be：
（1）Temperature of reaction kettle is controlled at 80 DEG C, 100 parts of water are added into reaction kettle, it is 100-120 to weigh mass ratio:20-25:
25-30：Poplar Powder, maleic anhydride, sodium sulfanilate and the BPO of 1-1.5 is added in reaction kettle, after reacting 3h, in high speed
Under stirring, reaction temperature reduces by 10 DEG C, is added dropwise the concentrated sulfuric acid in 1h, after insulation reaction 2h, adds 0.5-0.8 parts of foaming
Agent and 0.2-0.3 parts of foaming control agents after reacting 1h, adjust solution PH, after being spin-dried for solvent with sodium carbonate/bicarbonate buffer solution
It stands；
（2）Take 60-80 parts of steps（1）5-8 parts of nano silicon dioxides, 8-10 parts of modified calcium carbonates, 0.2- are added in obtained particle
0.5 part of silane coupling agent, 1-2 parts of antioxidants grind 30 minutes, obtain a kind of slow-release concrete diminishing at room temperature
Agent.
2. a kind of preparation method of slow-release concrete water-reducing agent according to claim 1, which is characterized in that described
The preparation method of modified calcium carbonate is, at room temperature, by the polyvinyl chloride resin of butanone and hydroxyl 80-100 in mass ratio:10-15 is placed
In a kettle, 1h is stirred, 500-600 parts of ordinary calcium carbonate is added, stir speed (S.S.) control is stirred 10 minutes in 300rpm
Afterwards, IPDI8-12 parts are added, stirs 15 minutes, obtains modified calcium carbonate, modified mobility obviously increases, and adds convenient for follow-up
Work.
3. a kind of preparation method of slow-release concrete water-reducing agent according to claim 1, which is characterized in that foaming is adjusted
The preparation method of section agent is that control temperature of reaction kettle is 70 DEG C, rotating speed 200rpm, and it is 80-100 to weigh mass ratio:10-15：2-4
The higher acrylic ester monomer of glass transition temperature, butyl acrylate, acrylic acid, take in 1/8 addition reaction kettle, then add
Enter 100 parts of ethyl acetate and 0.3-0.8 parts of initiators, after reacting half an hour, residual monomer is gradually added dropwise, heats up 5 DEG C, heat preservation is anti-
It is taken out after answering 6h, obtains foaming control agent.
4. a kind of preparation method of slow-release concrete water-reducing agent according to claim 1, which is characterized in that described
Poplar Powder grain size is in 80-100 mesh.
5. a kind of preparation method of slow-release concrete water-reducing agent according to claim 1, which is characterized in that described
Concentrated sulfuric acid rate of addition must be slow enough, and has to be added dropwise in high-speed stirred, and heat is avoided to assemble.
6. a kind of preparation method of slow-release concrete water-reducing agent according to claim 1, which is characterized in that the PH
The effect of conditioning agent is the PH of control system 7 ± 0.3.
7. a kind of preparation method of slow-release concrete water-reducing agent according to claim 1, which is characterized in that described
Antioxidant is the substance obtained after by mass fraction be 1-2 parts of glycerine, 2-3 parts of vitamin C mixes.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110563373A (en) * | 2019-08-29 | 2019-12-13 | 中国电力科学研究院有限公司 | Dispersing agent for nano silicon dioxide and preparation method |
| CN112723901A (en) * | 2021-01-28 | 2021-04-30 | 尹兵 | Cement foamed concrete and preparation process thereof |
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| CN101050081A (en) * | 2006-04-07 | 2007-10-10 | 武汉市保立化学品有限责任公司 | High performance water reducing agent in new type comb shaped molecular structure |
| FR2944023B1 (en) * | 2009-04-01 | 2013-01-11 | Chryso | PROCESS FOR THE PREPARATION OF SUPERPLASTIFIERS |
| CN104177562A (en) * | 2014-07-30 | 2014-12-03 | 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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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101050081A (en) * | 2006-04-07 | 2007-10-10 | 武汉市保立化学品有限责任公司 | High performance water reducing agent in new type comb shaped molecular structure |
| FR2944023B1 (en) * | 2009-04-01 | 2013-01-11 | Chryso | PROCESS FOR THE PREPARATION OF SUPERPLASTIFIERS |
| CN104177562A (en) * | 2014-07-30 | 2014-12-03 | 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 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110563373A (en) * | 2019-08-29 | 2019-12-13 | 中国电力科学研究院有限公司 | Dispersing agent for nano silicon dioxide and preparation method |
| CN112723901A (en) * | 2021-01-28 | 2021-04-30 | 尹兵 | Cement foamed concrete and preparation process thereof |
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| Publication number | Publication date |
|---|---|
| CN108675665B (en) | 2021-02-02 |
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