CN107056992A - A kind of feature ethers polycarboxylic acid water reducing agent and preparation method thereof - Google Patents
A kind of feature ethers polycarboxylic acid water reducing agent and preparation method thereof Download PDFInfo
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- CN107056992A CN107056992A CN201611268217.6A CN201611268217A CN107056992A CN 107056992 A CN107056992 A CN 107056992A CN 201611268217 A CN201611268217 A CN 201611268217A CN 107056992 A CN107056992 A CN 107056992A
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- reducing agent
- feature
- polycarboxylic acid
- water reducing
- ethers polycarboxylic
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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
-
- 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
- C04B24/2652—Nitrogen containing polymers, e.g. polyacrylamides, polyacrylonitriles
- C04B24/2658—Nitrogen containing polymers, e.g. polyacrylamides, polyacrylonitriles containing polyether side chains
-
- 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
- C04B24/2664—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of ethylenically unsaturated dicarboxylic acid polymers, e.g. maleic anhydride copolymers
- C04B24/267—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of ethylenically unsaturated dicarboxylic acid polymers, e.g. maleic anhydride copolymers containing polyether side chains
-
- 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
- C04B24/2688—Copolymers containing at least three different monomers
- C04B24/2694—Copolymers containing at least three different monomers 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
- C08F2/00—Processes of polymerisation
- C08F2/38—Polymerisation using regulators, e.g. chain terminating agents, e.g. telomerisation
-
- 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
- C04B2103/0045—Polymers chosen for their physico-chemical characteristics
- C04B2103/0059—Graft (co-)polymers
-
- 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
Abstract
The present invention relates to a kind of feature ethers polycarboxylic acid water reducing agent and preparation method thereof, the water reducer is prepared by the raw material of following weight percentage through aqueous free radical polymerisation：Modified polyether polymeric monomer 75~90%, unsaturated carboxylic acid and its derivative 5~15%, the unsaturated monomer 0.5~10% with amide group, initiator 0.8~2%, reducing agent 0.05~0.5%, chain-transferring agent 0.05~0.8%.Polycarboxylate water-reducer prepared by the present invention can show significantly to disperse retentivity during concrete use, initial stage, concrete slump loss was small, and early age strength of concrete can be greatly improved, properties of product are stable, it is a kind of water reducer product with multifunctionality, be particularly suitable for use in pile tube class precast concrete product, with good market application foreground.
Description
Technical field
The invention belongs to building material technical field, it is related to a kind of feature ethers polycarboxylic acid water reducing agent and its preparation side
Method.
Background technology
Now with the propulsion of domestic a large amount of infrastructure, constantly expand for high-performance, the demand of strong concrete
Greatly.And application of the polycarboxylate water-reducer in high performance concrete especially precast concrete product has turned into raising concreter
The important measures of the property made and intensity index.Compared with normal concrete, precast concrete product is to early strength and strength development
Rate requires higher, to meet in the short period the need for form removal maintenance, so as to improve the service efficiency of template.Meanwhile, to accelerate
Efficiency of construction under low temperature environment, it is also necessary to it is required that precast concrete has early strong performance.
General early strength concrete often uses traditional additive product such as naphthalene water reducer, aliphatic water reducing agent, amino
Sulfonate based water reducer and melamine system water reducer, but these water reducers be applied to precast concrete produce when exist
Various problems, wherein most importantly bad adaptability and there is deferred action.Can then be had using Early-strength polycarboxylate superplasticizer
Effect improves the early strength of precast concrete, accelerates the striking time of concrete component, improves production efficiency, and early-strength is poly-
The use of carboxylic acid water reducer can effectively improve the volume of flyash and slag in concrete, and reduction Portland cement is used
Amount, realizes ultralow water-cement ratio.Although the species currently used for the polycarboxylate water-reducer of production precast concrete is various,
All there are different problems in actual applications in various water reducers, such as volume is high, bad adaptability and function it is single.
The content of the invention
The technical problems to be solved by the invention are that there is provided a kind of performance is excellent for above shortcomings in the prior art
Different feature ethers polycarboxylic acid water reducing agent and preparation method thereof, the polycarboxylate water-reducer strong adaptability, vdiverse in function, Neng Gouming
Aobvious to improve early strength, be particularly suitable for use in pile tube class precast concrete product, and its preparation method technique is simple, reaction condition
It is easily controlled, relatively low is required to production equipment.
In order to solve the above technical problems, the technical scheme that the present invention is provided is：
A kind of feature ethers polycarboxylic acid water reducing agent is provided, it is free through the aqueous solution by the raw material of following weight percentage
Base polymerisation is prepared：
The modified polyether polymeric monomer is methacrylic polyoxyethylene of the number-average molecular weight in the range of 1500~6000
The one or two kinds of of ether, poly glycol monomethyl ether.
By such scheme, the unsaturated carboxylic acid and its derivative are acrylic acid, methacrylic acid, maleic acid, richness
At least one of horse acid.
By such scheme, the unsaturated monomer with amide group is acrylamide, the one of N hydroxymethyl acrylamide
Plant or two kinds.
By such scheme, the initiator is hydrogen peroxide, ammonium persulfate, sodium peroxydisulfate, potassium peroxydisulfate, benzoyl peroxide first
At least one of acyl.
By such scheme, the reducing agent is sodium sulfite, sodium hydrogensulfite, potassium sulfite, potassium bisulfite, sulfuric acid Asia
At least one of iron, sodium formaldehyde sulfoxylate, vitamin C.
By such scheme, the chain-transferring agent is mercaptoethanol, TGA, mercaprol, mercaptopropionic acid, metering system
At least one of sodium sulfonate.
The present invention also provides the preparation method of above-mentioned functions ethers polycarboxylic acid water reducing agent, and it comprises the following steps：It will change
Property polyether macromonomer and deionized water be added in reactor, open agitator and electrical heating, after polymeric monomer is completely dissolved plus
Enter and be added dropwise after initiator, 10~20min by unsaturated carboxylic acid and its derivative, the unsaturated monomer with amide group, chain tra nsfer
The A that agent and deionized water are made into expects, and is expected by the B that reducing agent and deionized water are made into, time for adding control expects 2.5 in A~
3h, B expect 3~3.5h, and 1~2h of aging at temperature is controlled after completion of dropwise addition, finally add alkali to adjust pH value to 6~8, stop heating and are down to
Room temperature produces the feature ethers polycarboxylic acid water reducing agent.
The present invention also provides application of the above-mentioned functions ethers polycarboxylic acid water reducing agent in pile tube class precast concrete product.
The beneficial effects of the present invention are：Polycarboxylate water-reducer prepared by the present invention being capable of table during concrete use
Reveal significantly scattered retentivity, initial stage, concrete slump loss was small, and can greatly improve early age strength of concrete, product
Can be stable, it is a kind of with multi-functional water reducer product, be particularly suitable for use in pile tube class precast concrete product, with good
Market application foreground；In addition, the inventive method preparation technology is relatively easy, reaction condition is easily controllable, will to production equipment
Relatively low, non-pollutant discharge is sought, environmental protection is conducive to energy-saving and emission-reduction and environmental protection.
Embodiment
To make those skilled in the art more fully understand technical scheme, the present invention is made with reference to embodiment
It is described in further detail.The embodiments described below are only a part of embodiment of the present invention, rather than whole embodiments.
Based on embodiments of the invention, those of ordinary skill in the art obtained under the premise of creative work is not made it is all its
Its embodiment belongs to protection scope of the present invention.
Losec 501, Losec 608, Losec MPEG (number-average molecular weight 1500~6000) used in the present embodiment are Wuhan Losec
Chemical Co., Ltd. produces.
Embodiment 1
Weigh 165g modified polyethers polymeric monomer (Losec 501) and 200g deionized waters are added in reactor, open stirring
Device and electrical heating carry out the dissolving of polymeric monomer, after polymeric monomer is completely dissolved, and add 6g hydrogenperoxide steam generators (concentration 30wt%),
The A being made into by 16g acrylic acid, 10g acrylamides, 0.8g TGAs and 20g deionized waters is added dropwise after 10~20min
Material and 0.5g vitamin Cs expect that time for adding control expects that 2.5~3h, B expect 3~3.5h in A with the B that 60g deionized waters are made into；A、B
After material is added dropwise to complete, temperature control is subjected to 1~2h of aging at 40 DEG C or so, finally adds the NaOH aqueous solution to adjust the pH value of product
To 6~8, the feature ethers polycarboxylic acid water reducing agent that solid content is 40% or so is obtained.
Embodiment 2
Weigh 150g modified polyethers polymeric monomer (Losec 608) and 200g deionized waters are added in reactor, open stirring
Device and electrical heating carry out the dissolving of polymeric monomer, after polymeric monomer is completely dissolved, and add 5.5g hydrogenperoxide steam generators, by 10~
20min, is gone while being added dropwise by 14g acrylic acid, 10g fumaric acid, 8gN- NMAs, 1.4g TGAs and 20g
A material and 0.8g vitamin Cs that ionized water is made into and the B that 60g deionized waters are made into expect that time for adding control expects 2.5~3h, B in A
Expect 3~3.5h；After A, B material are added dropwise to complete, temperature control is subjected to 1~2h of aging at 40 DEG C or so, finally adds the NaOH aqueous solution
The pH value of product is adjusted to 6~8, the feature ethers polycarboxylic acid water reducing agent that solid content is 40% or so is obtained.
Embodiment 3
Weigh 180g modified polyether polymeric monomers (Losec MPEG) and 200g deionized waters are added in reactor, open stirring
Device and electrical heating carry out the dissolving of polymeric monomer, after polymeric monomer is completely dissolved, and add 3g ammonium persulfates, by 10~20min, together
When be added dropwise the A material that are made into by 12g acrylic acid, 6gN- NMAs, 1.2g mercaptopropionic acids and 20g deionized waters and
0.8g vitamin Cs expect that time for adding control expects that 2.5~3h, B expect 3~3.5h in A with the B that 60g deionized waters are made into；A, B gob
Plus after the completion of, temperature control is subjected to 1~2h of aging at 75 DEG C or so, finally plus NaOH aqueous solution regulation product pH value to 6
~8, obtain the feature ethers polycarboxylic acid water reducing agent that solid content is 40% or so.
Embodiment 4
Weigh 170g modified polyethers polymeric monomer (Losec 501) and 200g deionized waters are added in reactor, open stirring
Device and electrical heating carry out the dissolving of polymeric monomer, after polymeric monomer is completely dissolved, and add 4g potassium peroxydisulfates, by 10~20min, together
When be added dropwise matched somebody with somebody by 13.5g methacrylic acids, 8g maleic acids, 8g acrylamides, 1.5g mercaptopropionic acids and 20g deionized waters
Into the B that is made into of A material and 1.2g vitamin Cs and 60g deionized waters expect, time for adding control A expect 2.5~3h, B expect 3~
3.5h；After A, B material are added dropwise to complete, temperature control is subjected to 1~2h of aging at 60 DEG C or so, finally adds the regulation production of the NaOH aqueous solution
The pH value of product obtains the feature ethers polycarboxylic acid water reducing agent that solid content is 40% or so to 6~8.
Embodiment 5
Weigh 164g modified polyethers polymeric monomer (Losec 501) and 200g deionized waters are added in reactor, open stirring
Device and electrical heating carry out the dissolving of polymeric monomer, after polymeric monomer is completely dissolved, and add 3.8g sodium peroxydisulfates, by 10~20min,
The A material being made into by 18g acrylic acid, 14g acrylamides, 1.3g TGAs and 20g deionized waters and 0.9g mistakes are added dropwise simultaneously
Ammonium sulfate expects that time for adding control expects that 2.5~3h, B expect 3~3.5h in A with the B that 60g deionized waters are made into；A, B gob are added
Cheng Hou, by temperature control 55 DEG C or so carry out 1~2h of aging, finally plus ethylenediamine and deionized water regulation product pH value to
6~8, obtain the feature ethers polycarboxylic acid water reducing agent that solid content is 40% or so.
Embodiment 6
The gained feature ethers polycarboxylic acid water reducing agent of above-described embodiment 1~5 is carried out corresponding cement paste, mortar and
Concrete test, example detection result is as follows：
1st, flowing degree of net paste of cement effect
Paste flowing degree experiment is with reference to GB/T8077-2000《Methods for testing uniformity of concrete admixture》Carry out, control
Example now sells performance preferably polycarboxylate water-reducer using certain additive company, and each net slurry fluidity determining experiment is in identical bar
Carried out under part, selected reference cement is Portland cement.
The solid content of above additive (water reducer) is all 40%.
As can be seen that five kinds of feature ethers polycarboxylic acid water reducing agents and certain additive that the present invention is synthesized from above table
Company, which now sells performance preferably polycarboxylate water-reducer and compared, has preferably initial paste flowing degree and 1h paste flowing degrees.
2nd, the measure of glue sand mechanical property
Mechanical Properties of Cement Mortar is with reference to GB/T 17671-1999《Strength of cement mortar (ISO methods)》Carry out, reference examples make
Performance preferably polycarboxylate water-reducer is now sold with certain additive company, glue sand match ratio is：Cement：450g, normal sand：1350g、
Water：The polycarboxylate water-reducer that 147.3g, 40% contain admittedly：4.5g, cement mortar experiment is carried out under the same conditions, selected
Reference cement is Portland cement (Yadong PO42.5).
It can be seen that from above table：Five kinds of feature ethers polycarboxylic acid water reducing agents that the present invention is synthesized and certain additive
Company now sells performance preferably polycarboxylate water-reducer and compared, the effect for each age strength of cement mortar that is significantly improved.
3rd, concrete performance is determined
The measure of concrete water-reducing ratio, the slump and rheological parameters' change with time amount and mechanical property is according to GB 8076-2008《It is mixed
Solidifying soil additive》With GB/T 50080-2002《Standard for test methods of properties of ordinary concrete mixture standard》And GB/T 50081-
2002《Normal concrete mechanical test method》Carry out, the size of concrete anti-compression test specimen is 150mm × 150mm in experiment
×150mm。
C45 concrete mixs are：Cement：Flyash：Miberal powder：Sand：Big stone：Handstone：Water：Finished product water reducer=
325：125：80：760：750：280：180：5.76, finished product water reducer volume is glue material (concrete and coal ash+miberal powder)
1.6wt%, the proportioning of finished product water reducer is：By mass parts, 9 parts of+2 parts of polycarboxylate water-reducer+0.03 part of sodium gluconate bleeds
Agent k12, wherein cement are Yadong PO42.5 cement, and flyash is II grade of ash, and concrete performance result is as follows.
As can be seen from the above table：Five kinds of feature ethers polycarboxylic acid water reducing agents that the present invention is synthesized subtract in concrete application
Water, guarantor collapse, better than certain additive company now sells performance preferably polycarboxylate water-reducer on each age strength, especially in concrete
Improved a lot in early strength.
Claims (8)
1. a kind of feature ethers polycarboxylic acid water reducing agent, it is characterised in that it is by the raw material of following weight percentage through water-soluble
Liquid Raolical polymerizable is prepared：
The modified polyether polymeric monomer is methyl allyl polyoxyethylene ether of the number-average molecular weight in the range of 1500~6000, poly-
The one or two kinds of of glycol monoethyl ether.
2. feature ethers polycarboxylic acid water reducing agent according to claim 1, it is characterised in that the unsaturated carboxylic acid and its
Derivative is at least one of acrylic acid, methacrylic acid, maleic acid, fumaric acid.
3. feature ethers polycarboxylic acid water reducing agent according to claim 1, it is characterised in that it is described with amide group not
Saturation monomer is acrylamide, the one or two kinds of of N hydroxymethyl acrylamide.
4. feature ethers polycarboxylic acid water reducing agent according to claim 1, it is characterised in that the initiator is peroxidating
At least one of hydrogen, ammonium persulfate, sodium peroxydisulfate, potassium peroxydisulfate, benzoyl peroxide.
5. feature ethers polycarboxylic acid water reducing agent according to claim 1, it is characterised in that the reducing agent is sulfurous acid
At least one of sodium, sodium hydrogensulfite, potassium sulfite, potassium bisulfite, ferrous sulfate, sodium formaldehyde sulfoxylate, vitamin C.
6. feature ethers polycarboxylic acid water reducing agent according to claim 1, it is characterised in that the chain-transferring agent is sulfydryl
At least one of ethanol, TGA, mercaprol, mercaptopropionic acid, methylpropene sodium sulfonate.
7. a kind of preparation method of any described feature ethers polycarboxylic acid water reducing agents of claim 1-6, it is characterised in that bag
Include following steps：Modified polyether polymeric monomer and deionized water are added in reactor, agitator and electrical heating is opened, treats big list
Body is added after being completely dissolved to be added dropwise after initiator, 10~20min by unsaturated carboxylic acid and its derivative, the insatiable hunger with amide group
The A material being made into monomer, chain-transferring agent and deionized water, and expected by the B that reducing agent and deionized water are made into, time for adding control
System expects that 2.5~3h, B expect 3~3.5h in A, and 1~2h of aging at temperature is controlled after completion of dropwise addition, finally adds alkali to adjust pH value to 6~8,
Stopping heating being down to room temperature and produces the feature ethers polycarboxylic acid water reducing agent.
8. a kind of any described feature ethers polycarboxylic acid water reducing agents of claim 1-6 are in pile tube class precast concrete product
Application.
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| CN107602762A (en) * | 2017-09-29 | 2018-01-19 | 济南大学 | For one kind with N, N methylene-bisacrylamides are micro- cross-linked polycarboxylic's high efficiency water reducing agent of cross-linking monomer and preparation method thereof |
| CN109912750A (en) * | 2017-12-12 | 2019-06-21 | 山西黄腾化工有限公司 | A kind of water-reducing agent and preparation method thereof |
| CN111302700A (en) * | 2020-04-21 | 2020-06-19 | 苏州市兴邦化学建材有限公司 | Quick plasticizer for low water-cement ratio concrete and preparation method thereof |
| CN111410721A (en) * | 2020-04-23 | 2020-07-14 | 重庆牧野实业有限公司 | Preparation method of novel polycarboxylate superplasticizer |
| CN111548073A (en) * | 2020-06-04 | 2020-08-18 | 广州市建筑科学研究院有限公司 | Anti-shrinkage prefabricated part concrete and preparation method and application thereof |
| CN113121754A (en) * | 2021-05-06 | 2021-07-16 | 钱倩 | Concrete workability modifier, preparation method thereof, concrete admixture and concrete |
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| CN111302700A (en) * | 2020-04-21 | 2020-06-19 | 苏州市兴邦化学建材有限公司 | Quick plasticizer for low water-cement ratio concrete and preparation method thereof |
| CN111410721A (en) * | 2020-04-23 | 2020-07-14 | 重庆牧野实业有限公司 | Preparation method of novel polycarboxylate superplasticizer |
| CN111548073A (en) * | 2020-06-04 | 2020-08-18 | 广州市建筑科学研究院有限公司 | Anti-shrinkage prefabricated part concrete and preparation method and application thereof |
| CN111548073B (en) * | 2020-06-04 | 2022-06-07 | 广州市建筑科学研究院有限公司 | Anti-shrinkage prefabricated part concrete and preparation method and application thereof |
| CN113121754A (en) * | 2021-05-06 | 2021-07-16 | 钱倩 | Concrete workability modifier, preparation method thereof, concrete admixture and concrete |
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Application publication date: 20170818 |