CN102408526A - Low-air entraining slow-settling polycarboxylate water reducer and preparation method thereof - Google Patents
Low-air entraining slow-settling polycarboxylate water reducer and preparation method thereof Download PDFInfo
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- CN102408526A CN102408526A CN201110324015XA CN201110324015A CN102408526A CN 102408526 A CN102408526 A CN 102408526A CN 201110324015X A CN201110324015X A CN 201110324015XA CN 201110324015 A CN201110324015 A CN 201110324015A CN 102408526 A CN102408526 A CN 102408526A
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Abstract
The invention provides a low-air entraining slow-settling polycarboxylate water reducer and a preparation method thereof. A molecular structure of the water reducer is shown in the specification. The preparation method comprises the following steps of: adding propenyl polyethylene ether and a certain amount of water into an experimental device; heating to 50-90 DEG C; after dissolution, adding a certain amount of maleic anhydride, sodium methallyl sulfonate, acrylamide solution and initiator solution, and adding dropwise within 1-2 hours; keeping the reaction temperature at 50-90 DEG C; and continuing keeping the temperature for 1-6 hours; neutralizing with sodium hydroxide solution of a certain concentration; and adjusting the pH value between 6-8 to obtain the low-air entraining slow-settling polycarboxylate water reducer. Through the invention, the prepared low-air entraining slow-settling polycarboxylate water reducer has high water reducing ratio, good slump-loss retarding property, great fluidity of net cement paste, low fluidity loss of age net cement paste, obvious slow-settling effect, good low-air entraining effect, strong cement adaptability and stable performance, and is environment-friendly; and the synthesis process is easy to operate.
Description
Technical field
The invention belongs to technical field of concrete additives, relate to a kind of preparation method of low bleed retardation setting type polycarboxylate water-reducer.
Background technology
Polycarboxylate water-reducer is compared with other water reducers, and performance characteristics has: volume is low, and water-reducing rate is high, and slump-loss is little, advantages such as good workability, so high performance water reducing agent of polyocarboxy acid also becomes one of requisite component of high performance concrete.The performance of most of polycarboxylate water-reducers was more single in the past, and great majority will increase its application performance through composite other concrete admixtures, reach the requirement of concrete works.At present, the polycarboxylate water-reducer of development not only has workability preferably, water-reducing effect preferably, but also directly have some other better performance, and need not pass through preparation method, arrive the concrete performance demand.For example patent of invention CN201010185714.6 " a kind of multi-branched polycarboxylic water reducer with excellent function of slump protection and preparation method thereof " provides the 30%-60% that monomer a accounts for reaction-ure mixture; The 20%-50% of monomer b reaction-ure mixture; Monomer is the 10%-30% of reaction-ure mixture; The 5%-15% of monomer d reaction-ure mixture carries out polyreaction, is characterized in having excellent concrete plasticity and keeps performance.For example main employing of patent of invention CN201010576923.3 " a kind of preparation method of retardation setting type polycarboxylate water-reducer " obtains a kind of retardation setting type polycarboxylate water-reducer with the tired monomer of allylsulfonate, the tired monomer of vinylformic acid, the big monomer of Methylacrylic acid polyethylene glycol single armor ether ester and the big monomer of maleic anhydride graft beta-cyclodextrin through free-radical polymerized, and its unusual part is to have delayed coagulation preferably.
The present invention is through the relation between low bleed retardation setting type polycarboxylate water-reducer polycarboxylate water-reducer molecular structure and its application performance; Guaranteeing that the raw molecule structure of selection can increase or promote the application performance of polycarboxylate water-reducer under the low bleed retardation setting type polycarboxylate water-reducer good operation property condition.Under action of evocating, in the aqueous solution, carry out polyreaction.It is except having the water-reducing rate height, and protect plasticity is good, and flowing degree of net paste of cement is big, through the time flowing degree of net paste of cement loss little outside, also have retarding effect and low bleed effect preferably, concrete works is had bigger benefit.Low bleed retardation setting type polycarboxylate water-reducer is strong to the flexibility of cement, environmentally friendly, environmental protection, and synthesis technique is simple to operate, and product performance are stable.
Summary of the invention
Through molecular design theory, the group that adopts some to have diminishing, slow setting, bleed and increase stability is incorporated in the molecular structure of polycarboxylate water-reducer, thereby obtains the molecular structure of low bleed retardation setting type polycarboxylate water-reducer.
Annotate: R
1, R
2, R
3, R
4Be H or CH
3
Propenyl Soxylat A 25-7, MALEIC ANHYDRIDE, methylpropene sodium sulfonate and acrylic amide are selected in this research for use, and persulphate is as initiator.The low bleed retardation setting type polycarboxylate water-reducer of preparation is through unsaturated monomer polymerization under action of evocating; Make polymkeric substance have the reactive group side chain of characteristic; Water-reducing effect is good, delayed coagulation is good thereby obtain to have, the polycarboxylate water-reducer of excellent properties such as low bleed.Has polyoxyethylene groups in the propenyl Soxylat A 25-7; Polyoxyethylene groups exists in low bleed retardation setting type polycarboxylate water-reducer molecular structure; Play space steric effect; Can under the less situation of polycarboxylate water-reducer volume, it have dispersiveness preferably to cement granules, meanwhile polyethers also has certain bleed effect and increases steady effect; MALEIC ANHYDRIDE generates maleic acid in water, has two carboxyls in its molecular structure, has water-reduction and stronger delayed coagulation preferably, also has certain guarantor effect of collapsing; Have sulfonic group in the molecular structure of methylpropene sodium sulfonate, sulfonic group exists in low bleed retardation setting type polycarboxylate water-reducer, mainly is the effect that further promotes water-reducing effect; Carboxamido-group in the acrylic amide can play bleed, disperse, increases steady effect in low bleed retardation setting type polycarboxylate water-reducer, but also can play certain adhesive aggregation effect to cement slurry, and the diminishing segregation phenomenon occurs.
Each set of dispense of raw material is than (weight part ratio) as follows:
Initiator 3-15 part
Propenyl Soxylat A 25-7 70-150 part
MALEIC ANHYDRIDE 7-30 part
Methylpropene sodium sulfonate 3-20 part
Acrylic amide 3-15 part
Sodium hydroxide 3-15 part
Water 175-375 part
The preparation technology that the present invention adopts is following:
(1) dissolution process: in already installed experimental installation, add propenyl polyvinyl ether and a certain amount of water, be heated to 50 ℃-90 ℃, dissolve;
(2) reaction process: in reaction unit, add a certain amount of MALEIC ANHYDRIDE, methylpropene sodium sulfonate, acrylamide soln and initiator solution in batches, in 1-2h, drip off, keep 50-90 ℃ of temperature of reaction, continue insulation 1-6h;
(3) N-process: neutralize with certain density sodium hydroxide solution, regulating pH value is between the 6-8, finally obtains the finished product of low bleed retardation setting type polycarboxylate water-reducer.
Advantage of the present invention is: according to the molecular structure of polycarboxylate water-reducer and the relation between the application performance; Pass through molecular design theory; The group that adopts some to have diminishing, slow setting, bleed and increase stability; Be incorporated in the molecular structure of polycarboxylate water-reducer, thereby obtain the molecular structure of low bleed retardation setting type polycarboxylate water-reducer.It is main raw material(s) that propenyl Soxylat A 25-7, MALEIC ANHYDRIDE, methylpropene sodium sulfonate and acrylic amide are selected in this research for use, and persulphate is as initiator.Low bleed retardation setting type polycarboxylate water-reducer has excellent performance; The concrete that can be used for mass concrete, the construction of hot climate condition; The concrete of parking for a long time or transporting at a distance is in many concrete workses such as high-strength high-performance concrete, high-flowing concrete and pump concrete.
The low bleed retardation setting type polycarboxylate water-reducer of the present invention's preparation has following characteristics: flowing degree of net paste of cement is big; Can reach 270mm-280mm; The 1h flowing degree of net paste of cement can reach 260mm-270mm; Through the time flowing degree of net paste of cement loss little, test according to standard GB/T 8077-2000 " concrete admixture homogeneity experimental technique "; Retarding effect is good, cement paste time of coagulation and check sample contrast, and the presetting period has prolonged 168min, and final setting time has been postponed 352min; Low bleed is made good use of, and the air content that fresh concrete records is about 2.7%; Water-reducing rate is high, can arrive about 30%; Protect plasticity is good; Cement adaptability is strong.
Embodiment
Following embodiment has more at large described the process of low bleed retardation setting type polycarboxylate water-reducer produced according to the present invention, and the umber in the preparation process is a weight part.
Embodiment 1
In the four-hole boiling flask that TM, numerical control whisking appliance, tap funnel, prolong are installed, add 140 parts of propenyl polyvinyl ethers and 76 parts of water, heating in water bath to 50 ℃-90 ℃ is to dissolving fully; In reaction unit, add 25 parts of MALEIC ANHYDRIDEs and 85 parts of water, 20 parts of methylpropene sodium sulfonates and 53 parts of water, 12 parts of acrylic amides and 47 parts of water and 12 parts of ammonium persulphates and 42 parts of water in batches, in 1-2h, drip off, continue insulation 1-6h; With 25%-35% sodium hydroxide solution neutralization test product, regulating pH value is between the 6-8, can obtain the finished product of low bleed retardation setting type polycarboxylate water-reducer.
Embodiment 2
In the four-hole boiling flask that TM, numerical control whisking appliance, tap funnel, prolong are installed, add 90 parts of propenyl polyvinyl ethers and 50 parts of water, heating in water bath is to 50-90 ℃, to dissolving fully; Add 12 parts of MALEIC ANHYDRIDEs and 67 parts of water, 9 parts of methylpropene sodium sulfonates and 39 parts of water, 5 parts of acrylic amides and 36 parts of water and 3 parts of ammonium persulphates and 30 parts of water in batches, in 1-2h, drip off, continue insulation 1-6h; With 25%-35% sodium hydroxide solution neutralization test product, regulating pH value is between the 6-8, can obtain the finished product of low bleed retardation setting type polycarboxylate water-reducer.
Embodiment 3
In the four-hole boiling flask that TM, numerical control whisking appliance, tap funnel, prolong are installed, add 110 parts of propenyl polyvinyl ethers and 65 parts of water, heating in water bath is to 50-90 ℃, to dissolving fully; In reaction unit, add 17 parts of MALEIC ANHYDRIDEs and 72 parts of water, 15 parts of methylpropene sodium sulfonates and 47 parts of water, 9 parts of acrylic amides and 40 parts of water and 7 parts of ammonium persulphates and 35 parts of water in batches, in 1-2h, drip off, continue insulation 1-6h; With 25-35% sodium hydroxide solution neutralization test product, regulating pH value is between the 6-8, can obtain the finished product of low bleed retardation setting type polycarboxylate water-reducer.
Method of use:
Required sand, stone and the cement of elder generation's weighing; They are put in the agitator kettle stir; Add an amount of low bleed retardation setting type polycarboxylate water-reducer and water then; Fully stir 3min, can obtain required fresh concrete, can carry out mix and test with reference to GB/T 8076-2000 " concrete admixture "; Cement paste, sand-cement slurry carry out mix with reference to the relevant regulations of GB/T 8077-2000 " concrete admixture homogeneity experimental technique " to be used and tests.The volume of low bleed retardation setting type polycarboxylate water-reducer is converted into solid content and accounts for 0.2% of cement quality.In use; May be owing to factors such as the silt content of environment for use temperature, cement type, sandstone and weighing error are different; Certain application performance difference can in use be arranged, should carry out suitable consumption adjustment according to practical situation, in the hope of best application performance.
Claims (5)
1. one kind low bleed retardation setting type polycarboxylate water-reducer; It is characterized in that: the group that adopts some to have diminishing, slow setting, bleed and increase stability; Be incorporated in the molecular structure of polycarboxylate water-reducer, thereby obtain the molecular structure of low bleed retardation setting type polycarboxylate water-reducer
R
1, R
2, R
3, R
4Be H or CH
3
Select propenyl Soxylat A 25-7, MALEIC ANHYDRIDE, methylpropene sodium sulfonate and acrylic amide for use; Persulphate is as initiator; The low bleed retardation setting type polycarboxylate water-reducer of preparation is through unsaturated monomer polymerization under action of evocating; The reactive group side chain that makes polymkeric substance have characteristic, water-reducing effect is good, delayed coagulation is good thereby obtain to have, the polycarboxylate water-reducer of low bleed.
2. the preparation method of an a kind of low bleed retardation setting type polycarboxylate water-reducer as claimed in claim 1.
3. the preparation technology of the present invention's employing is following:
In experimental installation, add propenyl polyvinyl ether and a certain amount of water; Be heated to 50-90 ℃; The dissolving back successively adds a certain amount of MALEIC ANHYDRIDE, methylpropene sodium sulfonate, acrylamide soln and initiator solution; In 1-2h, drip off, keep 50-90 ℃ of temperature of reaction, continue insulation 1-6h.
4. neutralize with certain density sodium hydroxide solution, regulating pH value is between the 6-8, finally obtains the finished product of low bleed retardation setting type polycarboxylate water-reducer.
5. each set of dispense of raw material is than (weight part ratio) as follows:
Initiator 3-15 part
Propenyl Soxylat A 25-7 70-150 part
MALEIC ANHYDRIDE 7-30 part
Methylpropene sodium sulfonate 3-20 part
Acrylic amide 3-15 part
Sodium hydroxide 3-15 part
Water 175-375 part.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104016616A (en) * | 2014-06-24 | 2014-09-03 | 湖北恒利建材科技有限公司 | Novel high-strength and energy-saving polycarboxylate superplasticizer and preparation method thereof |
| CN104761688A (en) * | 2015-03-23 | 2015-07-08 | 东北大学 | An early-strength type polycarboxylic acid water reducer and a preparing method thereof |
| CN106749963A (en) * | 2016-11-29 | 2017-05-31 | 中建商品混凝土（福建）有限公司 | A kind of bleed controllable type poly carboxylic acid series water reducer for pure machine-made sand concrete and preparation method thereof |
| CN108298862A (en) * | 2018-03-30 | 2018-07-20 | 王敏 | A kind of preparation method of mortar thickening agent |
| CN111439947A (en) * | 2020-03-26 | 2020-07-24 | 浙江和业科技有限公司 | Low-air-entraining slow-setting type polycarboxylate superplasticizer and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101538134A (en) * | 2009-04-14 | 2009-09-23 | 大连市建筑科学研究设计院股份有限公司 | Polyether class polycarboxylic acid high-efficiency water reducing agent and preparation method thereof |
-
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- 2011-10-24 CN CN201110324015XA patent/CN102408526A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101538134A (en) * | 2009-04-14 | 2009-09-23 | 大连市建筑科学研究设计院股份有限公司 | Polyether class polycarboxylic acid high-efficiency water reducing agent and preparation method thereof |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104016616A (en) * | 2014-06-24 | 2014-09-03 | 湖北恒利建材科技有限公司 | Novel high-strength and energy-saving polycarboxylate superplasticizer and preparation method thereof |
| CN104016616B (en) * | 2014-06-24 | 2016-03-30 | 湖北恒利建材科技有限公司 | A kind of high-strength energy-saving type polycarboxylate water-reducer and preparation method thereof |
| CN104761688A (en) * | 2015-03-23 | 2015-07-08 | 东北大学 | An early-strength type polycarboxylic acid water reducer and a preparing method thereof |
| CN106749963A (en) * | 2016-11-29 | 2017-05-31 | 中建商品混凝土（福建）有限公司 | A kind of bleed controllable type poly carboxylic acid series water reducer for pure machine-made sand concrete and preparation method thereof |
| CN106749963B (en) * | 2016-11-29 | 2019-11-26 | 中建商品混凝土（福建）有限公司 | A kind of bleed controllable type poly carboxylic acid series water reducer and preparation method thereof for pure machine-made sand concrete |
| CN108298862A (en) * | 2018-03-30 | 2018-07-20 | 王敏 | A kind of preparation method of mortar thickening agent |
| CN111439947A (en) * | 2020-03-26 | 2020-07-24 | 浙江和业科技有限公司 | Low-air-entraining slow-setting type polycarboxylate superplasticizer and preparation method thereof |
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Application publication date: 20120411 |