CN105949404A - Preparation method of slump retaining agent capable of releasing controllable polycarboxylic acid - Google Patents
Preparation method of slump retaining agent capable of releasing controllable polycarboxylic acid Download PDFInfo
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- CN105949404A CN105949404A CN201610394873.4A CN201610394873A CN105949404A CN 105949404 A CN105949404 A CN 105949404A CN 201610394873 A CN201610394873 A CN 201610394873A CN 105949404 A CN105949404 A CN 105949404A
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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
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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
- C04B24/24—Macromolecular compounds
- C04B24/26—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B24/2605—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing polyether side chains
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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
- C04B2103/308—Slump-loss preventing agents
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- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention discloses a preparation method of a slump retaining agent capable of releasing controllable polycarboxylic acid and relates to the technical field of chemical additives for building materials. The preparation method includes the following steps that 1, 144-180 parts of unsaturated polyoxyethylene ether monomer and 144-180 parts of deionized water are added, by mass, to a three-mouth flask, stirring is performed till dissolution is completed, heating is performed to reach 45-60 DEG C during stirring, and heat preservation is performed; 2, 1.0-2.0 parts of a chain transfer agent and 0.5-1.5 parts of an initiator are dissolved, by mass, in 30-60 parts of deionized water to prepare a solution A; 3, 2-20 parts of unsaturated acid and 20-30 parts of unsaturated ester are dissolved, by mass, in 10-20 parts of deionized water to prepare a solution B; 4, after the step 1 is completed, the solution A and the solution B are simultaneously dropwise added to the three-mouth flask, the adding times are respectively 180-210 minutes and 150-180 minutes, reaction continues for 60-80 minutes, deionized water is added, dilution is performed till the theoretical solid content of 40% is reached, a finished product is obtained. The preparation method can meet the requirement for slump keeping time according to construction, and several slump retaining agents can be flexibly compounded to meet different construction requirements.
Description
Technical field
The present invention relates to construction material chemical addition agent technical field, be specifically related to a kind of preparation method discharging controllable type polycarboxylic acid slump retaining agent.
Background technology
Polycarboxylate water-reducer is as a kind of green environment amenable concrete chemical admixture, because the water-reducing property of its excellence is gradually widely used by industry.Traditional polycarboxylate water-reducer is generally attained by good dispersion effect or water-reducing property, but it has limitation in concrete long time service property retention.Therefore to solve this problem, it is used retarder and compounds with water reducer, but the problem so bringing setting time and early strength.In order to more preferably solve the work retentivity problem of concrete, Chinese scholars has researched and developed slump retaining agent.
But; owing to the cement type of China is various; admixture is extremely complex; in the actual application of concrete; the problems such as concrete big, the bleeding isolation of loss often occur, simultaneously along with the difference of construction site transportation range, the damage state difference that collapses of concrete is the biggest; therefore, to have the concrete slump retaining agent of controllable adsorption significant in research.
Summary of the invention
The technical problem to be solved is to provide a kind of retention time being regulated and controled slump retaining agent by modifying ingredients and preparation method, with the preparation method of the release controllable type polycarboxylic acid slump retaining agent of the requirement of the flowing concrete of satisfied different transportation ranges.
For solving above-mentioned technical problem, the technical solution used in the present invention is: a kind of preparation method discharging controllable type polycarboxylic acid slump retaining agent, it is characterised in that:
It comprises the steps:
1) press mass fraction and unsaturation polyoxyethylene ether monomer 144-180 part, in deionized water 144-180 part addition there-necked flask, stirring extremely dissolving, period are heated to 45-60 DEG C of insulation；
2) by mass fraction chain-transferring agent 1.0-2.0 part and initiator 0.5-1.5 part is dissolved in the deionized water of 30-60 part and is configured to A liquid；
3) pressing mass fraction by 2-20 part unsaturated acids, 20-30 part beta-unsaturated esters is dissolved in the deionized water of 10-20 part and is configured to B liquid；
4) until step 1) complete after, in there-necked flask, drip A, B liquid simultaneously, its time for adding is respectively 180-210min, 150-180min, terminates after continuing reaction 60-80min, adds deionized water and is diluted to theoretical solid containing being 40% to get product；
Wherein, described unsaturated acids be acrylic acid, methacrylic acid, fumaric acid, maleic anhydride one or more compound.
Described beta-unsaturated esters is that one or more in acrylic acid methyl ester., 2-(Acryloyloxy)ethanol, Hydroxypropyl acrylate, methyl methacrylate, hydroxyethyl methylacrylate, Hydroxypropyl methacrylate compound.
Further technical scheme is, described unsaturated polyoxyethylene ether monomer is isopentenol polyoxyethylene ether or methyl thiazolinyl polyoxyethylene ether, and its molecular weight is 2400-3000.
Further technical scheme is, described chain-transferring agent is that one or more in methallylsulfonic acid sodium, TGA, mercaptopropionic acid, mercaptoethanol compound.
Further technical scheme also resides in, and described initiator is that one or more in Ammonium persulfate., potassium peroxydisulfate, sodium peroxydisulfate, hydrogen peroxide compound.
Use and have the beneficial effects that produced by technique scheme: be to control initial charge density by regulation composition with preparation process in the principle of the invention, successfully control the slump retaining agent initial adsorption amount at cement particle surface, the hydrolysis rate difference controlling side chain lengths and beta-unsaturated esters is combined simultaneously, we successfully synthesize the slump retaining agent of different time sections release, scheme 1 is gradually reduced to the initial water-reducing rate of scheme 5, later stage keeps performance gradually to strengthen, according to the construction requirement to the slump retention time, several slump retaining agent can be compounded neatly, meet different construction needs.
Accompanying drawing explanation
The present invention is further detailed explanation with detailed description of the invention below in conjunction with the accompanying drawings.
Fig. 1 is that the slump retaining agent charge density of different initial charge density is with hydrolysis time situation of change figure；
Detailed description of the invention
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described, it is clear that described embodiment is only a part of embodiment of the present invention rather than whole embodiments.Based on the embodiment in the present invention, the every other embodiment that those of ordinary skill in the art are obtained under not making creative work premise, broadly fall into the scope of protection of the invention.
Elaborate a lot of detail in the following description so that fully understanding the present invention, but the present invention can also use other to be different from alternate manner described here to be implemented, those skilled in the art can do similar popularization in the case of intension of the present invention, and therefore the present invention is not limited by following public specific embodiment.
Present invention teaches a kind of preparation method discharging controllable type polycarboxylic acid slump retaining agent, it comprises the steps:
1) press mass fraction and unsaturation polyoxyethylene ether monomer 144-180 part, in deionized water 144-180 part addition there-necked flask, stirring extremely dissolving, period are heated to 45-60 DEG C of insulation；
2) by mass fraction chain-transferring agent 1.0-2.0 part and initiator 0.5-1.5 part is dissolved in the deionized water of 30-60 part and is configured to A liquid；
3) just it is dissolved in by mass fraction in the deionized water of 10-20 part and is configured to B liquid；
4) until step 1) complete after, in there-necked flask, drip A, B liquid simultaneously, its time for adding is respectively 180-210min, 150-180min, terminates after continuing reaction 60-80min, adds deionized water and is diluted to theoretical solid containing being 40% to get product；
Wherein, described unsaturated acids be acrylic acid, methacrylic acid, fumaric acid, maleic anhydride one or more compound.
Described beta-unsaturated esters is that one or more in acrylic acid methyl ester., 2-(Acryloyloxy)ethanol, Hydroxypropyl acrylate, methyl methacrylate, hydroxyethyl methylacrylate, Hydroxypropyl methacrylate compound.
Wherein, described unsaturated polyoxyethylene ether monomer is isopentenol polyoxyethylene ether or methyl thiazolinyl polyoxyethylene ether, and its molecular weight is 2400-3000.
Wherein, described chain-transferring agent is that one or more in methallylsulfonic acid sodium, TGA, mercaptopropionic acid, mercaptoethanol compound.
Wherein, described initiator is that one or more in Ammonium persulfate., potassium peroxydisulfate, sodium peroxydisulfate, hydrogen peroxide compound.
Embodiment 1
1) pressing mass fraction will be for isopentenol polyoxyethylene ether (2400 molecular weight), and deionized water 144 parts adds in there-necked flask, and stirring is to dissolving, and period is heated to 45 DEG C of insulations；
2) by mass fraction, 1.0 parts of methallylsulfonic acid sodium chain-transferring agents and 0.8 part of ammonium persulfate initiator are dissolved in the deionized water of 30 parts and are configured to A liquid；
3) by mass fraction 17.28 parts of acrylic acid are dissolved in the deionized water of 10 parts and are configured to B liquid；Making acrylic acid amount account for whole anchoring group mass fraction is 100%.
4) until step 1) complete after, in there-necked flask, drip A, B liquid simultaneously, its time for adding is respectively 180min, 150min, terminates after continuing reaction 60min, adds deionized water and is diluted to theoretical solid containing being 40% to get product.
Embodiment 2
1) press mass fraction and 144 parts of isopentenol polyoxyethylene ether (2400 molecular weight), in deionized water 144 parts addition there-necked flask, stirring extremely dissolving, period are heated to 50 DEG C of insulations；
2) by mass fraction, 2.0 parts of methallylsulfonic acid sodium chain-transferring agents and 0.8 part of Ammonium persulfate., 0.5 part of hydrogen peroxide initiator are dissolved in the deionized water of 30 parts and are configured to A liquid；
3) by mass fraction, 4 parts of acrylic acid, 2.8 parts of maleic anhydrides, 23.2 parts of 2-(Acryloyloxy)ethanols are dissolved in the deionized water of 20 parts and are configured to B liquid；Making acrylic acid amount account for whole anchoring group mass fraction is 20%；
4) until step 1) complete after, in there-necked flask, drip A, B liquid simultaneously, its time for adding is respectively 180min, 150min, terminates after continuing reaction 60, adds deionized water and is diluted to theoretical solid containing being 40% to get product.
Embodiment 3
1) press mass fraction and 144 parts of isopentenol polyoxyethylene ether (2400 molecular weight), in deionized water 144 parts addition there-necked flask, stirring extremely dissolving, period are heated to 60 DEG C of insulations；
2) by mass fraction, 2.0 parts of methallylsulfonic acid sodium chain-transferring agents and 0.8 part of ammonium persulfate initiator are dissolved in the deionized water of 60 parts and are configured to A liquid；
3) by mass fraction, acrylic acid, 2.6 parts of br dilute anhydrides, 26 parts of Hydroxypropyl acrylates of 2.88 parts are dissolved in the deionized water of 20 parts and are configured to B liquid；Making acrylic acid amount account for whole anchoring group mass fraction is 15%；
4) until step 1) complete after, in there-necked flask, drip A, B liquid simultaneously, its time for adding is respectively 210min, 180min, terminates after continuing reaction 60min, adds deionized water and is diluted to theoretical solid containing being 40% to get product.
Embodiment 4
1) press mass fraction and 180 parts of methyl thiazolinyl polyoxyethylene ether (3000 molecular weight), in deionized water 180 parts addition there-necked flask, stirring extremely dissolving, period are heated to 50 DEG C of insulations；
2) by mass fraction, 1.5 parts of methallylsulfonic acid sodium chain-transferring agents and 1 part of ammonium persulfate initiator are dissolved in the deionized water of 45 parts and are configured to A liquid；
3) by mass fraction, 2.1 parts of methacrylic acids, 2.45 parts of br dilute anhydrides, 26 parts of Hydroxypropyl acrylates are dissolved in the deionized water of 15 parts and are configured to B liquid；It is 10% that acrylic acid amount accounts for whole anchoring group mass fraction
4) until step 1) complete after, in there-necked flask, drip A, B liquid simultaneously, its time for adding is respectively 210min, 180min, terminates after continuing reaction 60, adds deionized water and is diluted to theoretical solid containing being 40% to get product.
Embodiment 5
1) press mass fraction and 180 parts of methyl thiazolinyl polyoxyethylene ether (3000 molecular weight), in deionized water 180 parts addition there-necked flask, stirring extremely dissolving, period are heated to 60 DEG C of insulations；
2) by mass fraction, 2.0 parts of methallylsulfonic acid sodium chain-transferring agents and 0.8 part of ammonium persulfate initiator are dissolved in the deionized water of 30 parts and are configured to A liquid；
3) by mass fraction, 4.9 parts of br dilute anhydrides, 28.8 parts of Hydroxypropyl methacrylates are dissolved in the deionized water of 15 parts and are configured to B liquid；Making acrylic acid amount account for whole anchoring group mass fraction is 0%.
4) until step 1) complete after, in there-necked flask, drip A, B liquid simultaneously, its time for adding is respectively 180min, 150min, terminates after continuing reaction 60, adds deionized water and is diluted to theoretical solid containing being 40% to get product；
Embodiment 6
1) press mass fraction and 160 parts of methyl thiazolinyl polyoxyethylene ether (3000 molecular weight), in deionized water 150 parts addition there-necked flask, stirring extremely dissolving, period are heated to 60 DEG C of insulations；
2) by mass fraction, 1.5 parts of methallylsulfonic acid sodium chain-transferring agents and 1.5 parts of ammonium persulfate initiator are dissolved in the deionized water of 45 parts and are configured to A liquid；
3) by mass fraction, 4.9 parts of br dilute anhydrides, 28.8 parts of Hydroxypropyl methacrylates are dissolved in the deionized water of 20 parts and are configured to B liquid；Making acrylic acid amount account for whole anchoring group mass fraction is 0%.
4) until step 1) complete after, in there-necked flask, drip A, B liquid simultaneously, its time for adding is respectively 200min, 160min, terminates after continuing reaction 75min, adds deionized water and is diluted to theoretical solid containing being 40% to get product；
In above-described embodiment, embodiment 1-5 is to be added according to the ratio of acrylic acid consumption reasonable opinion adsorption group.
Slump retaining agent concrete applicating evaluating:
Testing concrete performance is carried out, main investigation concrete gradual loss situation according to GB/T 50,080 2002 " Standard for test methods of properties of ordinary concrete mixture standard " and GB/T 50,081 2002 " standard for test methods of mechanical properties of ordinary concrete ".
The solid volume of folding of the 0.2% of fixing additive is constant, for ease of distinguishing, embodiment 1,2,3,4,5 is respectively designated as BT-100 (P2), BT-20, BT-15, BT-10, BT-0.Investigate P2, P2+BT-20, P2+BT-15, the impact on concrete slump gradual loss of the five kinds of additives of P2+BT-10, P2+BT-0.Wherein BT-100 is ordinary water-reducing agent, BT-x (x=100,20,15,10,0) represents that in the slump retaining agent synthesized, acrylic acid quality accounts for the percent in whole synthesis with anchoring group raw material total amount, such as, the raw material in P2 with anchorage effect only has acrylic acid, named BT-100.+ BT-x equally, represents that water reducer and slump retaining agent are the additive that 7:3 carries out compounding according to the solid ratio of folding.Five kinds of additives sign data such as table 1 to concrete slump gradual loss
The different Fresh Concrete with Admixtures performance comparison data of table 1
By table 1 data it can be seen that along with in BT-X the increase of X content, i.e. acrylic acid account for the increase of whole anchoring group quality, product initial dispersion ability also significantly improves, but the holding performance of concrete is significantly reduced.Pure water reducer i.e. P2 initial extension degree is more than 600mm, and 60min is almost without fluidity；Anchoring group does not has acrylic acid i.e. compounding for BT-0 Yu P2 additive minimum 500mm of initial extension degree, but after 120min, concrete slump is almost without loss, and function of slump protection is fine.In order to analyze reason further, we have carried out the test of charge density under different hydration time section equally.
The charge density that corresponding concrete performance is carried out characterizes
The slump retaining agent charge density of characterization result different initial charge density as shown in Figure 1 is with hydrolysis time situation of change.
As can be seen from Figure 1, along with acrylic acid accounts for the raising of whole anchoring group mass percent (0%AA-100%AA), initial charge density improves the most therewith, the 2mmol/g of BT-100 is brought up to from the 0.3mmol/g of BT-0, it coincide with the initial flow degree situation of table 1 concrete, charge density is big, and initial adsorption dispersibility is strong.BT-15, BT-20 initial charge density is respectively 0.74mmol/g, 1.25mmol/g more than 0.7mmol/g (great many of experiments speculates that 0.7mmol/g may be for improving a CCP of absorption driving force), initial dispersion absorption also there is certain contribution, so concrete initial flow degree is the biggest, but later stage holding capacity is more weak.BT-10 charge density when 30min has reached 0.81mmol/g, thus it is speculated that adsorbing driving force after 30min and disclosure satisfy that its scattered adsorption on cement granules, during 60min, holding capacity is preferable.BT-0 charge density when 60min has reached 0.72mmol/g, beginning can be adsorbed in a large number and is dispersed in cement particle surface, play the effect that dispersion keeps, although divergence has declined during 60min, but also can keep state during 60min when 120min, keep effect favourable in the 60min-120min time period.
We are by the control of initial charge density, successfully control the slump retaining agent initial adsorption amount at cement particle surface, the hydrolysis rate difference controlling side chain lengths and beta-unsaturated esters is combined simultaneously, we successfully synthesize the slump retaining agent of different time sections release, scheme 1 is gradually reduced to the initial water-reducing rate of scheme 5, and the later stage keeps performance gradually to strengthen, according to the construction requirement to the slump retention time, several slump retaining agent can be compounded neatly, meet different construction needs.
Claims (4)
1. the preparation method discharging controllable type polycarboxylic acid slump retaining agent, it is characterised in that:
It comprises the steps:
1) mass fraction is pressed by unsaturation polyoxyethylene ether monomer 144-180 part, deionized water
144-180 part adds in there-necked flask, and stirring is to dissolving, and period is heated to 45-60 DEG C
Insulation；
2) by mass fraction, chain-transferring agent 1.0-2.0 part and initiator 0.5-1.5 part are dissolved in
The deionized water of 30-60 part is configured to A liquid；
3) press mass fraction and 2-20 part unsaturated acids, 20-30 part beta-unsaturated esters are dissolved in 10-20
The deionized water of part is configured to B liquid；
4) until step 1) complete after, in there-necked flask, drip A, B liquid, its dropping simultaneously
Time is respectively 180-210min, 150-180min, terminates after continuing reaction 60-80min,
Add deionized water and be diluted to theoretical solid containing being 40% to get product；
Wherein, described unsaturated acids is acrylic acid, methacrylic acid, fumaric acid, maleic
One or more of dicarboxylic anhydride compound.
Described beta-unsaturated esters be acrylic acid methyl ester., 2-(Acryloyloxy)ethanol, Hydroxypropyl acrylate,
One in methyl methacrylate, hydroxyethyl methylacrylate, Hydroxypropyl methacrylate or
Multiple compounding.
A kind of preparation discharging controllable type polycarboxylic acid slump retaining agent the most according to claim 1
Method, it is characterised in that: described unsaturated polyoxyethylene ether monomer is prenol polyoxyethylene
Ether or methyl thiazolinyl polyoxyethylene ether, its molecular weight is 2400-3000.
A kind of preparation discharging controllable type polycarboxylic acid slump retaining agent the most according to claim 1
Method, it is characterised in that: described chain-transferring agent be methallylsulfonic acid sodium, TGA,
One or more in mercaptopropionic acid, mercaptoethanol compound.
A kind of preparation discharging controllable type polycarboxylic acid slump retaining agent the most according to claim 1
Method, it is characterised in that: described initiator be Ammonium persulfate., potassium peroxydisulfate, sodium peroxydisulfate,
One or more in hydrogen peroxide compound.
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| CN106519140A (en) * | 2016-11-15 | 2017-03-22 | 湖北工业大学 | Delayed-release alkali-resistant polycarboxylic acid slump retaining agent master batch |
| CN106883354A (en) * | 2017-03-06 | 2017-06-23 | 水利部交通运输部国家能源局南京水利科学研究院 | A kind of powdery polycarboxylic-acid slump retaining agent and preparation method thereof |
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| CN108395138A (en) * | 2018-04-08 | 2018-08-14 | 赵顺全 | A kind of accelerator for cement slurry |
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| CN109912751A (en) * | 2017-12-13 | 2019-06-21 | 山西黄腾化工有限公司 | A kind of water-reducing agent and preparation method thereof |
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| CN106496446A (en) * | 2016-11-15 | 2017-03-15 | 湖北工业大学 | A kind of method of expired HEA Material synthesis polycarboxylic acid slump retaining agent masterbatch |
| CN106519140A (en) * | 2016-11-15 | 2017-03-22 | 湖北工业大学 | Delayed-release alkali-resistant polycarboxylic acid slump retaining agent master batch |
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| CN109912751A (en) * | 2017-12-13 | 2019-06-21 | 山西黄腾化工有限公司 | A kind of water-reducing agent and preparation method thereof |
| CN108395138A (en) * | 2018-04-08 | 2018-08-14 | 赵顺全 | A kind of accelerator for cement slurry |
| CN111170671A (en) * | 2018-11-13 | 2020-05-19 | 北京市建筑工程研究院有限责任公司 | Preparation method of slump-retaining solid polycarboxylate superplasticizer |
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