CN109265622A - A kind of no heat source high-performance controlled-release polycarboxylic acid water reducing agent and preparation method thereof - Google Patents
A kind of no heat source high-performance controlled-release polycarboxylic acid water reducing agent and preparation method thereof Download PDFInfo
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- CN109265622A CN109265622A CN201810869125.6A CN201810869125A CN109265622A CN 109265622 A CN109265622 A CN 109265622A CN 201810869125 A CN201810869125 A CN 201810869125A CN 109265622 A CN109265622 A CN 109265622A
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- reducing agent
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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
- 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
- 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
- C04B24/165—Macromolecular compounds comprising sulfonate or sulfate groups obtained by reactions only involving carbon-to-carbon unsaturated bonds containing polyether side chains
-
- 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
- C08F4/00—Polymerisation catalysts
- C08F4/40—Redox systems
-
- 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
Abstract
The invention discloses a kind of no heat source high-performance controlled-release polycarboxylic acid water reducing agents, it includes 100 parts of isopentene group polyoxyethylene ether, 6 ~ 10 parts of acrylic acid, 9 ~ 13 parts of acrylic acid hydroxyl ethyl esters, 5 ~ 9 parts of acrylic acid hydroxypropyl acrylates, 1 ~ 2 part of 2- acrylamide-2-methylpro panesulfonic acid, 1 ~ 2 part of methyl propylene sodium sulfonate, 0.5 ~ 1.5 part of sodium hypophosphite, 0.5 ~ 1 part of ammonium persulfate, 1 ~ 2 part of hydrogen peroxide and 140 ~ 180 parts of water；It also discloses the preparation method of no heat source high-performance controlled-release polycarboxylic acid water reducing agent.The beneficial effects of the present invention are: simple production process, initial water-reducing rate at low cost, with higher, slow release effect is obvious, is able to maintain free of losses in 1 ~ 3h of concrete, effectively solves the problems, such as that concrete slump loss is too fast, saving energy consumption.
Description
Technical field
The present invention relates to the field that is synthetically prepared of concrete poly carboxylic acid series water reducer, especially a kind of no heat source slow-release
High performance water reducing agent of polyocarboxy acid and preparation method thereof.
Background technique
At this stage, with the development of building trade, concrete quality is required higher and higher.But due to concrete former material
There are biggish differences for material, and in ready-mixed concrete operation, the slump-loss problem of fresh concrete is always to perplex engineering
The problem of construction.In concrete transportation and work progress, the too fast phenomenon of concrete slump loss frequent occurrence, especially
Prolonged conveying will lead to that concrete slump loss is excessive, influence the workability of concrete.Sometimes plus water remodeling can make reality
The effect of desired design is not achieved in the intensity of border concrete and the endurance qualities such as impervious.
Currently, by increase water-reducing agent dosage or construction before plus-minus aqua remold concrete can make concrete restore compared with
Good working performance, but will cause the isolation of concrete, bleeding in the dosage that stirring initial stage increases water-reducing agent, destroy concrete
Uniformity reduce the bending and compressive strength of concrete so that the intensity of concrete each section has differences；And in weather
When hot, prolonged transport will cause the evaporation of mixing water, reduce the ratio of mud of concrete.By retarder and polycarboxylic acids diminishing
Agent is compounded, and can satisfy the concrete works for needing retarding effect.But sometimes because the influence of certain reasons can generate
Setting time is too short or too long, is unable to satisfy the requirement of engineering construction.Before construction plus water remodeling concrete can not only improve coagulation
The ratio of mud of soil, the air content that also will increase concrete reduce the impermeability of concrete.The slump-loss pair of concrete in a word
The working performance and endurance quality of concrete cause large effect.Using conventional water-reducing agent, it is difficult to make fresh concrete
With preferable initial slump and slump-retaining, it is unable to satisfy the requirement of normal construction.
It is anti-typically to carry out free radical polymerization at 40~80 DEG C for the production technology of sustained-release polycarboxylic water reducer at present
It should synthesize, production cost is relatively high, and energy consumption is very big.
Summary of the invention
The purpose of the present invention is to overcome the shortcomings of the existing technology, provides a kind of simple production process, it is at low cost, have compared with
High initial water-reducing rate, slow release effect are obvious, are able to maintain free of losses in 1~3h of concrete, effectively solution concrete slump
Lose too fast problem, save energy consumption without heat source high-performance controlled-release polycarboxylic acid water reducing agent and preparation method thereof.
The purpose of the present invention is achieved through the following technical solutions: a kind of no heat source sustained-release polycarboxylic high-performance diminishing
Agent, it includes 100 parts of isopentene group polyoxyethylene ether, 6~10 parts of acrylic acid, 9~13 parts of acrylic acid hydroxyl ethyl esters, 5~9 parts of propylenes
Sour hydroxypropyl acrylate, 1~2 part of 2- acrylamide-2-methylpro panesulfonic acid, 1~2 part of methyl propylene sodium sulfonate, 0.5~1.5 part Asia
Sodium phosphate, 0.5~1 part of ammonium persulfate, 1~2 part of hydrogen peroxide and 140~180 parts of water.
The isopentene group polyoxyethylene ether molecular weight is 2400, and hydrogen peroxide solution concentration is 30%.
The preparation method of the no heat source high-performance controlled-release polycarboxylic acid water reducing agent, it the following steps are included:
S1, suitable softened water is added into container, is then slowly added to isopentene group polyoxyethylene ether, stirring at normal temperature 20
~30min dissolves isopentene group polyoxyethylene ether sufficiently；
Sodium hypophosphite and hydrogen peroxide, 5~10min of stirring at normal temperature are added in S2, the solution into step S1；
S3, by acrylic acid, hydroxy-ethyl acrylate, acrylic acid hydroxypropyl acrylate, 2- acrylamide-2-methylpro panesulfonic acid, methyl
The addition of propylene sodium sulfonate is loaded in the vessel I of softened water, and is stirred evenly, and solution A is obtained；Ammonium persulfate addition is loaded with
It in the vessel II of softened water, and stirs evenly, obtains solution B；
S4, into the solution of step S2, while solution A and solution B is added dropwise, control solution A is added dropwise in 2.5h, controls
Solution B processed is 0.5h more late than solution A to be dripped off；
0.5h is kept the temperature after S5, titration, 30% sodium hydroxide solution is then added and adjusts pH value to 6~7, softening is added
It is 40% that water, which is diluted to solid content, finally obtains high-performance controlled-release polycarboxylic acid water reducing agent.
The invention has the following advantages that
(1) present invention uses two kinds of initiators of ammonium persulfate and hydrogen peroxide, utilizes the heat released in polymerization process
Promote system temperature to increase, be not necessarily to external source, economical environment-protective, and effectively control the generation of high temperature side reaction, reduces altogether
The by-product of poly- product, conversion rate of products is high, has water-reducing rate height, the good feature of function of slump protection.
(2) characteristic group is introduced into the molecular structure of polycarboxylate water-reducer by the present invention, makes it have required function
Can, such as sulfonic group dispersibility with higher, in the alkaline environment of cement slurry hydrolysis can occur for ester group, and releasing has
The carboxylate group of water-reducing effect plays the role of protecting and collapse, and amide group is in cement particle surface strong adsorption, and also hydrolyzable is released
Adsorption group is released, but its rate of release is slow compared with ester group, collapsed to play the role of later period guarantor.
(3) slow setting component is not introduced in preparation process, does not extend the setting time of concrete
(4) present invention is according to molecular design theory, using different raw material proportionings, it can be achieved that polycarboxylate water-reducer initially divides
Dissipate performance and through when retention property between regulation, this product can be used alone or with make after common polycarboxylic acids water reducing agent compositional
With can satisfy the demand of different engineerings.
Specific embodiment
The present invention will be further described below, and protection scope of the present invention is not limited to as described below:
A kind of no heat source high-performance controlled-release polycarboxylic acid water reducing agent, it include 100 parts of isopentene group polyoxyethylene ether, 6~
10 parts of acrylic acid, 9~13 parts of acrylic acid hydroxyl ethyl esters, 5~9 parts of acrylic acid hydroxypropyl acrylates, 1~2 part of 2- acrylamido -2- methyl-prop
Sulfonic acid, 1~2 part of methyl propylene sodium sulfonate, 0.5~1.5 part of sodium hypophosphite, 0.5~1 part of ammonium persulfate, 1~2 part of hydrogen peroxide
And 140~180 parts of water.
The isopentene group polyoxyethylene ether molecular weight is 2400, and hydrogen peroxide solution concentration is 30%.
The preparation method of the no heat source high-performance controlled-release polycarboxylic acid water reducing agent, it the following steps are included:
S1, suitable softened water is added into container, is then slowly added to isopentene group polyoxyethylene ether, stirring at normal temperature 20
~30min dissolves isopentene group polyoxyethylene ether sufficiently；
Sodium hypophosphite and hydrogen peroxide, 5~10min of stirring at normal temperature are added in S2, the solution into step S1；
S3, by acrylic acid, hydroxy-ethyl acrylate, acrylic acid hydroxypropyl acrylate, 2- acrylamide-2-methylpro panesulfonic acid, methyl
The addition of propylene sodium sulfonate is loaded in the vessel I of softened water, and is stirred evenly, and solution A is obtained；Ammonium persulfate addition is loaded with
It in the vessel II of softened water, and stirs evenly, obtains solution B；
S4, into the solution of step S2, while solution A and solution B is added dropwise, control solution A is added dropwise in 2.5h, controls
Solution B processed is 0.5h more late than solution A to be dripped off；
0.5h is kept the temperature after S5, titration, 30% sodium hydroxide solution is then added and adjusts pH value to 6~7, softening is added
It is 40% that water, which is diluted to solid content, finally obtains high-performance controlled-release polycarboxylic acid water reducing agent.
Embodiment one:
Preparation method without heat source high-performance controlled-release polycarboxylic acid water reducing agent, it the following steps are included:
(1) 80 parts of softened waters are added into container, are then slowly added to 100 parts of isopentene group polyoxyethylene ether, room temperature stirs
20~30min is mixed, dissolves isopentene group polyoxyethylene ether sufficiently.
(2) 0.7 part of sodium hypophosphite of addition and 1.5 parts of hydrogen peroxide in the solution obtained to step (1), stirring at normal temperature 5~
10min；
(3) by 7.8 parts of acrylic acid, 12.5 parts of hydroxy-ethyl acrylates, 5.4 parts of acrylic acid hydroxypropyl acrylates, 1 part of 2- acrylamide
Base -2- methyl propane sulfonic acid, 1.5 parts of methyl propylene sodium sulfonates are added in 30 parts of softened waters, stir evenly, obtain solution A；By 0.7
Part ammonium persulfate is added in 40 parts of softened waters, stirs evenly, obtains solution B；
(4) into the solution of step S2, while solution A and solution B is added dropwise, control solution A is added dropwise in 2.5h, controls
Solution B is 0.5h more late than solution A to be dripped off；
(5) 0.5h is kept the temperature after titrating, 30% sodium hydroxide solution is then added and adjusts pH value to 6~7, softening is added
It is 40% that water, which is diluted to solid content, obtains high-performance controlled-release polycarboxylic acid water reducing agent.
Embodiment two:
Preparation method without heat source high-performance controlled-release polycarboxylic acid water reducing agent, it the following steps are included:
S1,80 parts of softened waters are added into container, are then slowly added to 100 parts of isopentene group polyoxyethylene ether, room temperature stirs
20~30min is mixed, dissolves isopentene group polyoxyethylene ether sufficiently.
0.6 part of sodium hypophosphite of addition and 1.3 parts of hydrogen peroxide in S2, the solution into step S1, stirring at normal temperature 5~
10min；
S3, by 6.7 parts of acrylic acid, 13 parts of hydroxy-ethyl acrylates, 6.7 parts of acrylic acid hydroxypropyl acrylates, 1.7 parts of 2- acrylamides
Base -2- methyl propane sulfonic acid, 1.6 parts of methyl propylene sodium sulfonates are added in 30 parts of softened waters, stir evenly, obtain solution A；By 0.8
Part ammonium persulfate is added in 40 parts of softened waters, stirs evenly, obtains solution B；
S4, into the solution of step S2, while solution A and solution B is added dropwise, control solution A is added dropwise in 2.5h, controls
Solution B is 0.5h more late than solution A to be dripped off；
0.5h is kept the temperature after S5, titration, 30% sodium hydroxide solution is then added and adjusts pH value to 6~7, softening is added
It is 40% that water, which is diluted to solid content, obtains high-performance controlled-release polycarboxylic acid water reducing agent.
Embodiment three:
Preparation method without heat source high-performance controlled-release polycarboxylic acid water reducing agent, it the following steps are included:
S1,80 parts of softened waters are added into container, are then slowly added to 100 parts of isopentene group polyoxyethylene ether, room temperature stirs
20~30min is mixed, dissolves isopentene group polyoxyethylene ether sufficiently.
1.5 parts of sodium hypophosphites of addition and 1.1 parts of hydrogen peroxide in S2, the solution into step S1, stirring at normal temperature 5~
10min；
S3, by 8.5 parts of acrylic acid, 10.8 parts of hydroxy-ethyl acrylates, 7.1 parts of acrylic acid hydroxypropyl acrylates, 1.4 parts of 2- acrylamides
Base -2- methyl propane sulfonic acid, 1.2 parts of methyl propylene sodium sulfonates are added in 30 parts of softened waters, stir evenly, obtain solution A；By 0.9
Part ammonium persulfate is added in 40 parts of softened waters, stirs evenly, obtains solution B；
S4, into the solution of step S2, while solution A and solution B is added dropwise, control solution A is added dropwise in 2.5h, controls
Solution B is 0.5h more late than solution A to be dripped off；
0.5h is kept the temperature after S5, titration, 30% sodium hydroxide solution is then added and adjusts pH value to 6~7, softening is added
It is 40% that water, which is diluted to solid content, obtains high-performance controlled-release polycarboxylic acid water reducing agent.
The product that above 3 embodiments are obtained and current sustained-release polycarboxylic slump retaining agent sample P C1 comparison, carry out water
Cement paste test and concrete test:
Test 1: cement paste test
Cement paste test is carried out according to GB8077-2012 " Methods for testing uniformity of concrete admixture ", and cement uses
Lafarge P.O42.5, every group of test raw material are cement 500g, water 145g.The experimental results are shown inthe following table:
As can be seen from the above table, high-performance controlled-release polycarboxylic acid water reducing agent prepared by the present invention has good initial point
Property and excellent flowing degree of net paste of cement holding capacity are dissipated, product slow-release time is up to 3h, and slow release speed is uniform.
Test 2: concrete test
Concrete slump and divergence test are according to " the normal concrete mix performance test side GB/T50080-2016
Method standard " it carries out, test is tested with common C30 concrete, and cement uses Lafarge P.O42.5, and admixture dosage is glue
The 0.18% of gel material dosage.1m3Concrete mix are as follows: cement 265kg, second class powered coal ash 75kg, machine sand 890kg, stone
1020kg, water 165kg.The experimental results are shown inthe following table:
As can be seen from the above table, high-performance controlled-release polycarboxylic acid water reducing agent of the invention is higher compared with having under low-dosage
Water-reducing rate, function of slump protection is excellent, and the slump is hardly lost in 3h.For the product preparation process without heating, room temperature can be into
Row, at low cost, high comprehensive performance are suitable for large area applications.
Claims (3)
1. a kind of no heat source high-performance controlled-release polycarboxylic acid water reducing agent, it is characterised in that: it includes 100 parts of isopentene group polyoxy second
Alkene ether, 6 ~ 10 parts of acrylic acid, 9 ~ 13 parts of acrylic acid hydroxyl ethyl esters, 5 ~ 9 parts of acrylic acid hydroxypropyl acrylates, 1 ~ 2 part of 2- acrylamido -2- first
Base propane sulfonic acid, 1 ~ 2 part of methyl propylene sodium sulfonate, 0.5 ~ 1.5 part of sodium hypophosphite, 0.5 ~ 1 part of ammonium persulfate, 1 ~ 2 part of hydrogen peroxide
And 140 ~ 180 parts of water.
2. a kind of no heat source high-performance controlled-release polycarboxylic acid water reducing agent according to claim 1, it is characterised in that: described different
Pentenyl polyoxyethylene ether molecular weight is 2400, and hydrogen peroxide solution concentration is 30%.
3. the preparation method without heat source high-performance controlled-release polycarboxylic acid water reducing agent described according to claim 1 ~ any one of 2,
It is characterized by: it the following steps are included:
S1, suitable softened water is added into container, is then slowly added to isopentene group polyoxyethylene ether, stirring at normal temperature 20 ~
30min dissolves isopentene group polyoxyethylene ether sufficiently；
Sodium hypophosphite and hydrogen peroxide, 5 ~ 10min of stirring at normal temperature are added in S2, the solution into step S1；
S3, by acrylic acid, hydroxy-ethyl acrylate, acrylic acid hydroxypropyl acrylate, 2- acrylamide-2-methylpro panesulfonic acid, methyl propylene
Sodium sulfonate addition is loaded in the vessel I of softened water, and is stirred evenly, and solution A is obtained；Ammonium persulfate addition is loaded with softening
It in the vessel II of water, and stirs evenly, obtains solution B；
S4, into the solution of step S2, while solution A and solution B is added dropwise, control solution A is added dropwise in 2.5h, controls molten
Liquid B is 0.5h more late than solution A to be dripped off；
0.5h is kept the temperature after S5, titration, 30% sodium hydroxide solution is then added and adjusts pH value to 6 ~ 7, it is dilute that softened water is added
Releasing to solid content is 40%, finally obtains high-performance controlled-release polycarboxylic acid water reducing agent.
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| CN113402194A (en) * | 2021-07-26 | 2021-09-17 | 中铁十一局集团桥梁有限公司 | Water reducing agent, preparation method thereof and concrete |
| CN114349915A (en) * | 2022-01-21 | 2022-04-15 | 太原市天鼎恒砼外加剂科技发展有限公司 | Polycarboxylate superplasticizer and preparation method thereof |
| CN114478945A (en) * | 2022-02-24 | 2022-05-13 | 漯河市昊源新材料有限公司 | Slow-release slump-retaining viscosity-reducing polycarboxylic acid water reducer and preparation method thereof |
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Application publication date: 20190125 |