CN107311502A - A kind of early-strength high-performance polycarboxylate water-reducer and preparation method thereof - Google Patents

A kind of early-strength high-performance polycarboxylate water-reducer and preparation method thereof Download PDF

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Publication number
CN107311502A
CN107311502A CN201710580795.1A CN201710580795A CN107311502A CN 107311502 A CN107311502 A CN 107311502A CN 201710580795 A CN201710580795 A CN 201710580795A CN 107311502 A CN107311502 A CN 107311502A
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parts
reducer
water
early
strength high
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肖维录
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Sunshine Fu Erman Novel Material Science And Technology Ltd
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Sunshine Fu Erman Novel Material Science And Technology Ltd
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B40/00Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
    • C04B40/0028Aspects relating to the mixing step of the mortar preparation
    • C04B40/0039Premixtures of ingredients
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2103/00Function or property of ingredients for mortars, concrete or artificial stone
    • C04B2103/30Water reducers, plasticisers, air-entrainers, flow improvers
    • C04B2103/302Water reducers

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Curing Cements, Concrete, And Artificial Stone (AREA)

Abstract

It is as made from the raw material of following parts by weight the invention discloses a kind of early-strength high-performance polycarboxylate water-reducer and preparation method thereof:100 parts of poly carboxylic acid series water reducer, 10 15 parts of retarder, 12 16 parts of diethanol monoisopropanolamine maleate compound, 8 10 parts of diethanol monoisopropanolamine, 8 12 parts of sodium lignin sulfonate, 35 parts of 2 ethyl, 4 methylimidazole, 0.5 1.5 parts of TTAB, 10 20 parts of metasilicate pentahydrate sodium, 250 450 parts of water.Early-strength high-performance polycarboxylate water-reducer prepared by the present invention has Applicable temperature low, and preferably, not chloride ion-containing, shrinkage factor is low for various group partition inter-capacitives, and water-reducing rate is high, and guarantor's effect of collapsing is good, the low excellent properties of volume.

Description

A kind of early-strength high-performance polycarboxylate water-reducer and preparation method thereof
Technical field
The present invention relates to building material technical field, and in particular to a kind of early-strength high-performance polycarboxylate water-reducer and its system Preparation Method.
Background technology
Poly carboxylic acid series water reducer is combination property very excellent third generation water reducer, is begun to from late 1980s In developed country's production applications such as Japan, Germany, the U.S..It has that water-reducing rate is high, concrete slump gradual loss is small, volume It is low, many advantages, such as big, the feature of environmental protection is good is contributed to concrete strength, from high-speed railway, Line for Passenger Transportation to port and pier, airport again To city Concrete Mixing Station, it is essential as concrete that domestic many application enterprises start selection polycarboxylate water-reducer BSA.But due to polycarboxylate high performance water-reducing agent in the application of China, development time relatively short, its application technology Research is still in the starting stage, and the compounding classical theory and common experience by representative of naphthalene water reducer are no longer applicable, because Many new problems urgently to be resolved hurrily are encountered in this engineering practice.
Compared with the water reducer such as naphthalene system, melamine series, sulfamate, polycarboxylate water-reducer is due to its excellent property The representative of concrete admixture last word can be had become.China's research in recent years in polycarboxylate water-reducer and application aspect Fast development is achieved, but kind is relatively single, and application technical research also not enough fully, can not still meet different engineerings and difference Area is diversified to water reducer to be required.In construction, in order that the early strength rapid growth of concrete is, it is necessary to mixed A number of early strength water-reducing agent is filled in the mixture for coagulating soil.But, the combination property of Early-strength polycarboxylate superplasticizer is poor, For example air content is higher, and presetting period and final setting time are longer etc., it is impossible to meet the use requirement of some special occasions.
The content of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of volume is low, early strong effect is good, shrinkage factor is low, water-reducing rate The low early-strength high-performance polycarboxylate water-reducer of high, Applicable temperature.
Present invention also offers the preparation method of the early-strength high-performance polycarboxylate water-reducer.
To achieve the above object, the present invention provides following technical scheme:
A kind of early-strength high-performance polycarboxylate water-reducer, is as made from the raw material of following parts by weight:Polycarboxylic-acid diminishing 100 parts of agent, 10-15 parts of retarder, 12-16 parts of diethanol monoisopropanolamine maleate compound, diethanol monoisopropanolamine 8-10 parts, 8-12 parts of sodium lignin sulfonate, 3-5 parts of 2-ethyl-4-methylimidazole, TTAB 0.5-1.5 Part, 10-20 parts of metasilicate pentahydrate sodium, 250-450 parts of water.
Described, retarder is one kind in sodium gluconate, calgon and sodium tripolyphosphate.
Described, the solid content of poly carboxylic acid series water reducer is 40%.
Described, diethanol monoisopropanolamine maleate compound is obtained by the following method:In reactor Diethanol monoisopropanolamine and maleic anhydride are added, adds under catalyst, stirring condition and is decompressed to 0.4MPa, heat, temperature control System is at 95 DEG C, maintenance system constant temperature, and the acidity of a system is determined every 1h, to acid number without significant change when reaction stop;So After be cooled to room temperature, successively with saturated sodium carbonate solution and distillation water washing, obtain diethanol monoisopropanolamine maleated Compound.
Described, the mol ratio of diethanol monoisopropanolamine and maleic anhydride is 1.0:0.8.
Described, catalyst is the p-methyl benzenesulfonic acid of mass fraction 1.4%, and the addition of the catalyst is diethanol list The 0.5% of isopropanolamine quality.
A kind of preparation method of early-strength high-performance polycarboxylate water-reducer, is as made from following steps:
1) poly carboxylic acid series water reducer is well mixed with water;
2) retarder, diethanol monoisopropanolamine maleate compound and metasilicate pentahydrate sodium are added into step 1) mixing In uniform solution, 5-10min is stirred;Add diethanol monoisopropanolamine, sodium lignin sulfonate, 2- ethyl -4- methyl miaows Azoles and TTAB, stir 10-20min, obtain early-strength high-performance polycarboxylate water-reducer.
The volume of early-strength high-performance polycarboxylate water-reducer of the present invention is the 1-2wt% of gel material content in concrete.
Each component of the present invention has played cooperative effect well, and wherein poly carboxylic acid series water reducer, which rises, reduces concrete mixing use Water, promotion concrete early strength agent, micro- air-entraining effect;Sodium lignin sulfonate has diminishing, slow setting, bleed triple function, Ke Yiqi concurrently The effect of performance is wrapped up to improvement concrete;2-ethyl-4-methylimidazole, TTAB and five water metasilicic acids Sodium acts synergistically, and its early strong, antifreezing effect is excellent, and plasticizing capacity is good;Diethanol monoisopropanolamine maleate compound and two Ethanol monoisopropanolamine plays raising early age strength of concrete;Retarder plays deferred action;Water plays solvent action.
Early-strength high-performance polycarboxylate water-reducer of the present invention has advantages below:(1) Applicable temperature is low, can be high in temperature Used under conditions of -15 DEG C;(2) various group partition inter-capacitives are preferable, it can be ensured that long period storage is uniform and stable;(3) group Not chloride ion-containing in point, it is to avoid to the action of rust of reinforcing bar;(4) deposited in component without severe corrosive or penetrating odor material Using safety and environmental protection;(5) shrinkage factor is low, effectively improves the endurance quality of concrete;(6) water-reducing rate is high, and water can be greatly reduced Gray scale, it is ensured that concrete strength;(7) protect effect of collapsing good, concrete construction performance is met well;(8) volume is low, with notable Economic and social benefit, be adapted to large-scale production.
Embodiment
With reference to specific embodiment, the present invention will be further described.
Raw material used in the present invention is commercially available, conventional purchase gained.
Embodiment 1
A kind of early-strength high-performance polycarboxylate water-reducer, is as made from the raw material of following parts by weight:Polycarboxylic-acid diminishing 100 parts of agent, 15 parts of retarder, 12 parts of diethanol monoisopropanolamine maleate compound, 8 parts of diethanol monoisopropanolamine, wood 12 parts of quality sodium sulfonate, 3 parts of 2-ethyl-4-methylimidazole, 1.5 parts of TTAB, metasilicate pentahydrate sodium 10 Part, 250 parts of water.
Described, retarder is sodium gluconate.
Described, the solid content of poly carboxylic acid series water reducer is 40%.
Described, diethanol monoisopropanolamine maleate compound is obtained by the following method:In reactor Diethanol monoisopropanolamine and maleic anhydride are added, adds under catalyst, stirring condition and is decompressed to 0.4MPa, heat, temperature control System is at 95 DEG C, maintenance system constant temperature, and the acidity of a system is determined every 1h, to acid number without significant change when reaction stop;So After be cooled to room temperature, successively with saturated sodium carbonate solution and distillation water washing, obtain diethanol monoisopropanolamine maleated Compound.
Described, the mol ratio of diethanol monoisopropanolamine and maleic anhydride is 1.0:0.8.
Described, catalyst is the p-methyl benzenesulfonic acid of mass fraction 1.4%, and the addition of the catalyst is diethanol list The 0.5% of isopropanolamine quality.
A kind of preparation method of early-strength high-performance polycarboxylate water-reducer, is as made from following steps:
1) poly carboxylic acid series water reducer is well mixed with water;
2) retarder, diethanol monoisopropanolamine maleate compound and metasilicate pentahydrate sodium are added into step 1) mixing In uniform solution, 5min is stirred;Add diethanol monoisopropanolamine, sodium lignin sulfonate, 2-ethyl-4-methylimidazole and TTAB, stirs 10-20min, obtains early-strength high-performance polycarboxylate water-reducer.
Embodiment 2
A kind of early-strength high-performance polycarboxylate water-reducer, is as made from the raw material of following parts by weight:Polycarboxylic-acid diminishing 100 parts of agent, 13 parts of retarder, 14 parts of diethanol monoisopropanolamine maleate compound, 9 parts of diethanol monoisopropanolamine, wood 10 parts of quality sodium sulfonate, 4 parts of 2-ethyl-4-methylimidazole, 1 part of TTAB, 15 parts of metasilicate pentahydrate sodium, 350 parts of water.
Described, retarder is calgon.
Described, the solid content of poly carboxylic acid series water reducer is 40%.
Described, diethanol monoisopropanolamine maleate compound is obtained by the following method:In reactor Diethanol monoisopropanolamine and maleic anhydride are added, adds under catalyst, stirring condition and is decompressed to 0.4MPa, heat, temperature control System is at 95 DEG C, maintenance system constant temperature, and the acidity of a system is determined every 1h, to acid number without significant change when reaction stop;So After be cooled to room temperature, successively with saturated sodium carbonate solution and distillation water washing, obtain diethanol monoisopropanolamine maleated Compound.
Described, the mol ratio of diethanol monoisopropanolamine and maleic anhydride is 1.0:0.8.
Described, catalyst is the p-methyl benzenesulfonic acid of mass fraction 1.4%, and the addition of the catalyst is diethanol list The 0.5% of isopropanolamine quality.
A kind of preparation method of early-strength high-performance polycarboxylate water-reducer, is as made from following steps:
1) poly carboxylic acid series water reducer is well mixed with water;
2) retarder, diethanol monoisopropanolamine maleate compound and metasilicate pentahydrate sodium are added into step 1) mixing In uniform solution, 8min is stirred;Add diethanol monoisopropanolamine, sodium lignin sulfonate, 2-ethyl-4-methylimidazole and TTAB, stirs 10-20min, obtains early-strength high-performance polycarboxylate water-reducer.
Embodiment 3
A kind of early-strength high-performance polycarboxylate water-reducer, is as made from the raw material of following parts by weight:Polycarboxylic-acid diminishing 100 parts of agent, 10 parts of retarder, 16 parts of diethanol monoisopropanolamine maleate compound, 10 parts of diethanol monoisopropanolamine, wood 8 parts of quality sodium sulfonate, 5 parts of 2-ethyl-4-methylimidazole, 0.5 part of TTAB, metasilicate pentahydrate sodium 20 Part, 450 parts of water.
Described, retarder is sodium tripolyphosphate.
Described, the solid content of poly carboxylic acid series water reducer is 40%.
Described, diethanol monoisopropanolamine maleate compound is obtained by the following method:In reactor Diethanol monoisopropanolamine and maleic anhydride are added, adds under catalyst, stirring condition and is decompressed to 0.4MPa, heat, temperature control System is at 95 DEG C, maintenance system constant temperature, and the acidity of a system is determined every 1h, to acid number without significant change when reaction stop;So After be cooled to room temperature, successively with saturated sodium carbonate solution and distillation water washing, obtain diethanol monoisopropanolamine maleated Compound.
Described, the mol ratio of diethanol monoisopropanolamine and maleic anhydride is 1.0:0.8.
Described, catalyst is the p-methyl benzenesulfonic acid of mass fraction 1.4%, and the addition of the catalyst is diethanol list The 0.5% of isopropanolamine quality.
A kind of preparation method of early-strength high-performance polycarboxylate water-reducer, is as made from following steps:
1) poly carboxylic acid series water reducer is well mixed with water;
2) retarder, diethanol monoisopropanolamine maleate compound and metasilicate pentahydrate sodium are added into step 1) mixing In uniform solution, 10min is stirred;Add diethanol monoisopropanolamine, sodium lignin sulfonate, 2-ethyl-4-methylimidazole And TTAB, 10-20min is stirred, early-strength high-performance polycarboxylate water-reducer is obtained.
Comparative example
A kind of polycarboxylate water-reducer, is as made from the raw material of following parts by weight:100 parts of poly carboxylic acid series water reducer, slow setting 13 parts of agent, 10 parts of sodium lignin sulfonate, 4 parts of 2-ethyl-4-methylimidazole, 1 part of TTAB, the inclined silicon of five water Sour 15 parts of sodium, 350 parts of water.
Described, retarder is calgon.
Described, the solid content of poly carboxylic acid series water reducer is 40%.
Described, catalyst is the p-methyl benzenesulfonic acid of mass fraction 1.4%, and the addition of the catalyst is diethanol list The 0.5% of isopropanolamine quality.
A kind of preparation method of polycarboxylate water-reducer, is as made from following steps:
1) poly carboxylic acid series water reducer is well mixed with water;
2) retarder and metasilicate pentahydrate sodium are added into step 1) in well mixed solution, stir 8min;Add wood Quality sodium sulfonate, 2-ethyl-4-methylimidazole and TTAB, stir 10-20min, obtain polycarboxylic acids diminishing Agent.
Flowing degree of net paste of cement and its retention property
Flowing degree of net paste of cement and fluidity gradual loss are according to GB/8077-2000《Concrete admixture homogeneity is tested Method》Carry out.Using P.0.42.5R cement, W/C=0.29.Result of the test is as shown in table 1.
The flowing degree of net paste of cement of table 1 and its retention property
Packet Volume/% 5min/mm 30min/mm 60min/mm
Embodiment 1 1.2 285 270 255
Embodiment 2 1.2 290 280 265
Embodiment 3 1.2 285 275 250
Comparative example 1.2 185 140 120
As it can be seen from table 1 compared with comparative example, early-strength high-performance polycarboxylic acids prepared by 1-3 of the embodiment of the present invention subtracts The mobility and fluidity of aqua keep effect to be had a distinct increment under the collective effect of each component.
Early-strength high-performance polycarboxylate water-reducer performance test results
Polycarboxylate water-reducer prepared by the embodiment 1-3 early-strength high-performance polycarboxylate water-reducers prepared and comparative example 1 Mix with batch concrete, detected respectively according to concerned countries standard by the 1.5wt% of gel material content.
Water-reducing rate, bleeding rate ratio, air content, setting time difference are according to GB8076-2008《Concrete admixture》Surveyed Fixed and calculating.Concrete sample make, maintenance and detection etc. are according to GB/T50080-2002《Normal concrete mix physical performance is tried Test method standard》、GB/T50081-2002《Standard for test methods of mechanical properties of ordinary concrete》Carry out.Result of the test such as table 2 It is shown.
The early-strength high-performance polycarboxylate water-reducer performance test results of table 2
As can be seen from Table 2, early-strength high-performance polycarboxylate water-reducer meets made from 1-3 of the embodiment of the present invention GB8076-2008《Concrete admixture》Index of correlation requirement in standard on early-strength high-performance water reducer.With comparative example Compare, in water-reducing rate, compressive strength rate, receipts under the collective effect of early-strength type high-performance polycarboxylic acids water reducing agent each component Advantageous above the key indexs such as shrinkage ratio, early-strength type high-performance polycarboxylic acids water reducing agent using effect is excellent, into This is with the obvious advantage, is worth a wide range of and promotes.
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, Er Qie In the case of without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter From the point of view of which point, embodiment all should be regarded as exemplary, and be nonrestrictive, the scope of the present invention is by appended power Profit is required rather than described above is limited, it is intended that all in the implication and scope of the equivalency of claim by falling Change is included in the present invention.
Moreover, it will be appreciated that although the present specification is described in terms of embodiments, not each embodiment is only wrapped Containing an independent technical scheme, this narrating mode of specification is only that for clarity, those skilled in the art should Using specification as an entirety, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art It may be appreciated other embodiment.

Claims (7)

1. a kind of early-strength high-performance polycarboxylate water-reducer, it is characterised in that be as made from the raw material of following parts by weight:Poly- carboxylic Sour 100 parts of based water reducer, 10-15 parts of retarder, 12-16 parts of diethanol monoisopropanolamine maleate compound, diethanol list 8-10 parts of isopropanolamine, 8-12 parts of sodium lignin sulfonate, 3-5 parts of 2-ethyl-4-methylimidazole, TTAB 0.5-1.5 parts, 10-20 parts of metasilicate pentahydrate sodium, 250-450 parts of water.
2. early-strength high-performance polycarboxylate water-reducer according to claim 1, it is characterised in that the retarder is glucose One kind in sour sodium, calgon and sodium tripolyphosphate.
3. early-strength high-performance polycarboxylate water-reducer according to claim 1, it is characterised in that the poly carboxylic acid series water reducer Solid content be 40%.
4. early-strength high-performance polycarboxylate water-reducer according to claim 1, it is characterised in that the diethanol list isopropanol Amine maleate compound is obtained by the following method:Diethanol monoisopropanolamine and maleic acid are added in reactor Acid anhydride, adds under catalyst, stirring condition and is decompressed to 0.4MPa, heat, temperature control is in 95 DEG C, maintenance system constant temperature, every 1h Determine a system acidity, to acid number without significant change when reaction stop;Room temperature is subsequently cooled to, saturated sodium carbonate is used successively Solution and distillation water washing, obtain diethanol monoisopropanolamine maleate compound.
5. early-strength high-performance polycarboxylate water-reducer according to claim 4, it is characterised in that the diethanol list isopropanol The mol ratio of amine and maleic anhydride is 1.0:0.8.
6. early-strength high-performance polycarboxylate water-reducer according to claim 4, it is characterised in that the catalyst is quality point The p-methyl benzenesulfonic acid of number 1.4%, the addition of the catalyst is the 0.5% of diethanol monoisopropanolamine quality.
7. a kind of preparation method of early-strength high-performance polycarboxylate water-reducer any one of claim 1-6, its feature exists In being as made from following steps:
1) poly carboxylic acid series water reducer is well mixed with water;
2) retarder, diethanol monoisopropanolamine maleate compound and metasilicate pentahydrate sodium are added into step 1) it is well mixed Solution in, stir 5-10min;Add diethanol monoisopropanolamine, sodium lignin sulfonate, 2-ethyl-4-methylimidazole and TTAB, stirs 10-20min, obtains early-strength high-performance polycarboxylate water-reducer.
CN201710580795.1A 2017-07-17 2017-07-17 A kind of early-strength high-performance polycarboxylate water-reducer and preparation method thereof Pending CN107311502A (en)

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CN108997151A (en) * 2018-08-30 2018-12-14 济南大学 The preparation method and products obtained therefrom of a kind of beta-unsaturated esters of alcohol-containing amine groups and application
CN109354654A (en) * 2018-08-30 2019-02-19 济南大学 A kind of Early-strength polycarboxylate superplasticizer and preparation method thereof
CN109776017A (en) * 2019-02-15 2019-05-21 山东鲁班建设集团总公司 A kind of composite concrete antifreeze and preparation method thereof
CN110317589A (en) * 2018-03-28 2019-10-11 中国石油天然气集团有限公司 Early strength agent and preparation method thereof, cement paste for well cementation
CN113831093A (en) * 2021-10-08 2021-12-24 深圳市京基混凝土有限公司 High slump retaining recycled concrete and preparation method thereof
CN115745470A (en) * 2022-11-11 2023-03-07 河海大学 Cement-based material interface reinforcing agent and preparation method and application thereof

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CN109354654A (en) * 2018-08-30 2019-02-19 济南大学 A kind of Early-strength polycarboxylate superplasticizer and preparation method thereof
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CN109776017A (en) * 2019-02-15 2019-05-21 山东鲁班建设集团总公司 A kind of composite concrete antifreeze and preparation method thereof
CN113831093A (en) * 2021-10-08 2021-12-24 深圳市京基混凝土有限公司 High slump retaining recycled concrete and preparation method thereof
CN115745470A (en) * 2022-11-11 2023-03-07 河海大学 Cement-based material interface reinforcing agent and preparation method and application thereof
CN115745470B (en) * 2022-11-11 2023-07-21 河海大学 Cement-based material interface reinforcing agent and preparation method and application thereof

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Application publication date: 20171103