CN108821634A - A kind of efficient cement water reducing agent and preparation method thereof - Google Patents
A kind of efficient cement water reducing agent and preparation method thereof Download PDFInfo
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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
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
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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
- C04B2103/302—Water reducers
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Abstract
The invention discloses a kind of efficient cement water reducing agents and preparation method thereof, belong to concrete additive technical field.Poly glycol monomethyl ether is added using acrylic acid as raw material in the present invention, through esterification, obtains macromonomer, citric acid-modified is added, the formation of hydrated calcium silicate gel is reduced, to obtain higher water-reducing rate；The present invention forms carboxyl anion using L-Aspartic acid as raw material, so that water-reducing agent remains to preferably disperse under hard water conditions, carries out water-reduction；Present invention introduces triethanolamines, improve the solubility on concrete particle surface, improve diminishing efficiency.The present invention solves the problems, such as that current water-reducing agent stability in hard water can poor, diminishing low efficiency.
Description
Technical field
The invention belongs to concrete additive technical fields, and in particular to a kind of efficient cement water reducing agent and its preparation side
Method.
Background technique
Concrete refers to the general designation of the cementing integral engineered composite material of aggregate by cementitious material.That usually says is mixed
One word of solidifying soil, which refers to, makees cementitious material, sand, masonry aggregate with cement；With water（Additive and admixture can be contained）Match by a certain percentage
Close, it is agitated obtained by cement concrete, also referred to as normal concrete, it is widely used in civil engineering.Make in cement mixture
When industry, in order to keep rapid operation effective, early stage demoulding is shortened the construction period, it is desirable that cement mixture has high fluidity, while cement
Mixture is capable of the loss of effective inhibition of slump, and there is sufficient early strength at hardening initial stage, this requires a kind of high-performance
Cement water reducing agent.Cement water reducing agent refers under conditions of concrete workability, cement consumption are constant, can be reduced mix
Water consumption, the additive for improving concrete pass through surface-active action, complexing, electrostatic repulsion forces or steric repulsion power
Deng hinder or destroy particle flocculent structure, so as to while saving cement consumption, guarantee concrete workability and
Intensity.With the development of concrete science, polymer chemistry and material molecule design theory constantly make further progress, to concrete
More stringent requirements are proposed for water-reducing agent.
Currently, can be mainly divided into four major class according to water-reducing agent diminishing and enhancing ability, water-reducing agent：First is that with Lignins
Based on ordinary water-reducing agent, such water-reducing agent is mostly powdery low air-entraining performance retarder, have micro- bleed, concrete can be improved
Impervious freeze thawing performance.But for the molecular structure of such water-reducing agent based on aromatic rings, flexibility is poor.Second is that being with naphthalene water reducer
The high efficiency water reducing agent of representative, this kind of water-reducing agent are resistance to by parent with environmentally protective and higher plasticity.But naphthalene water reducer is by molecule
The restriction of structure can not fundamentally improve the function of slump protection of concrete and the problem that volume is excessive.Third is that the high property of polycarboxylic acid
There is ultra-dispersed property to become the hot spot studied at present for energy water-reducing agent, this kind of water-reducing agent, and development is swift and violent.But it, can shadow intolerant to hard water
Ring volume.Fourth is that aliphatic sulfonic salt water-reducing agent, with excellent diminishing characteristic, wherein sulfonic group hydrophily is strong, can provide
Forceful electric power lotus, while also can be resistant to hard water.Aliphatic sulfonic salt water-reducing agent has been developed in recent years main non-naphthalene system's diminishing
One of agent, it is with acetone, formaldehyde, sodium sulfite, sodium pyrosulfite etc. for primary raw material, simple production process, production week
Phase is short.But mostly based on single sulfonic group and disulfonic acid base, water-reducing property is bad, while raw material has a pollution, irritant smell,
The requirement of green production is not met.Therefore a kind of efficient cement water reducing agent that water-reducing property is strong need to be developed.
Summary of the invention
The technical problems to be solved by the invention：Current water-reducing agent stability in hard water can poor, diminishing low efficiency aiming at the problem that,
A kind of efficient cement water reducing agent and preparation method thereof is provided.
In order to solve the above technical problems, the present invention is using technical solution as described below：
A kind of efficient cement water reducing agent, including diminishing activating agent matrix, hard water resistance chelating additive, early strength additive；
The preparation method of the diminishing activating agent matrix, includes the following steps：
S1. acrylic acid in mass ratio 2 ~ 5 is taken：1 ~ 3 be added poly glycol monomethyl ether, add acrylic acid quality 2 ~ 4% to benzene two
Phenol obtains mixture, takes mixture in mass ratio 3 ~ 5：8 ~ 10 be added toluene, be passed through nitrogen protection, add mixture quality 1 ~
3% p-methyl benzenesulfonic acid is stirred, rotary evaporation, obtains rotary evaporation object；
S2. acrylic acid in mass ratio 3 ~ 5 is taken：7 ~ 9 are added N, and N '-dicyclohexylcarbodiimide is stirred, and acrylic acid matter is added
1 ~ 3 times of citric acid of amount, is stirred in 40 ~ 50 DEG C, add acrylic acid quality 3 ~ 7% to dimethylamino naphthyridine, be warming up to
60 ~ 70 DEG C are stirred, and vacuum distillation obtains vacuum distillation object, takes rotary evaporation object in mass ratio 3 ~ 6：4 ~ 7 are added vacuum distillation
Object mixes to get diminishing activating agent matrix.
The condition that is stirred of gained rotary evaporation object is in the step S1：Be warming up to 110 ~ 120 DEG C be stirred 4 ~
6h, rotary evaporation to get.
The preparation method of the hard water resistance chelating additive, includes the following steps：
（1）Take L-Aspartic acid in mass ratio 10 ~ 15：3~5：4 ~ 7 are added hydrochloric acid, phosphoric acid, obtain mixture a, take mixture a by matter
Measure ratio 3 ~ 7：10 ~ 15 addition deionized waters are stirred, and are kept the temperature, are cooled to room temperature, are freeze-dried, grind and sieve with 100 mesh sieve,
It collects sieving particle to wash 3 ~ 6 times through deionized water, obtains washings；
（2）Take sodium hydroxide in mass ratio 2 ~ 5：7 ~ 10 are added deionized water, add 1 ~ 3 times of sodium hydroxide quality of taurine
It is stirred, obtains stirring mixture, take washings in mass ratio 1 ~ 5：8 ~ 10 are added deionized waters, are warming up to 35 ~ 45 DEG C, then plus
Enter the stirring mixture of washings quality 30 ~ 50%, adjusts pH to 7 ~ 7.2, be stirred to get hard water resistance chelating additive.
The step step（1）In heat-retaining condition be：It is warming up to 150 ~ 160 DEG C of 2 ~ 5h of heat preservation.
The early strength additive is：Take triethanolamine in mass ratio 2 ~ 4：3 ~ 6 are added sodium sulphate mixing to get early strong addition
Agent.
A kind of preparation method of efficient cement water reducing agent, includes the following steps：
A. according to the mass fraction, take 6 ~ 9 parts of diminishing activating agent matrixes, 4 ~ 7 parts of acrylic acid, 2 ~ 5 parts of methylpropene sodium sulfonates, 80 ~
90 parts of water, obtain matrix object, are warming up to 50 ~ 60 DEG C, are added dropwise the ammonium persulfate of base matter amount 1 ~ 3%, and control time for adding 40 ~
50min is stirred, and is adjusted pH to 6 ~ 7, is cooled to room temperature, obtains cooled material；
B. according to the mass fraction, 20 ~ 30 parts of cooled materials, 3 ~ 8 parts of hard water resistance chelating additives, 0.03 ~ 0.05 part of morning is taken to add by force
Agent, 8 ~ 15 parts of montmorillonite mixing, dry, pulverize 200 meshes, collect sieving particle a to get efficient cement water reducing agent.
The condition that is stirred in the step A is：It is warming up to 60 ~ 70 DEG C and is stirred 3 ~ 5h.
The present invention is compared with other methods, and advantageous effects are：
（1）The present invention is added poly glycol monomethyl ether through esterification and obtains macromonomer, simultaneously using acrylic acid as raw material
Introduce using acrylic acid as raw material, be added N, N '-dicyclohexylcarbodiimide, to dimethylamino naphthyridine through amidation process, then plus
Enter citric acid-modified, obtain the active main component of water-reducing agent, remaining macromonomer is compounded, forms diminishing activating agent
Matrix, later period are added acrylic acid, methylpropene sodium sulfonate etc. and carry out initiation polymerization, and diminishing activating agent matrix is grafted to polycarboxylic acids
On the water-reducing agent of class, efficient diminishing activating agent is obtained, wherein a large amount of hydroxyl, carboxyl isopolarity group have stronger water suction
Property, diminishing activating agent is adsorbed in cement particle surface, and hydrophilicity can make cement particle surface form one layer of solvation moisture film,
The flocculent structure of cement granules can be destroyed, release is wrapped in part mixing water therein, directly connecing between prevention cement granules
Touching, keeps cement granules fully dispersed, improves particle water wettability of the surface, so that concrete flowability increases, workability is good,
- COO in diminishing activating agent matrix simultaneously-Complex compound can be formed with the calcium ion in hydrolysis product of cement, delay hydroxide
The crystallization of calcium reduces the formation of hydrated calcium silicate gel, plays the role of dispersion and keeps, so that concrete slump loss subtracts
Small, setting time extends, and using the modification of citric acid so that be further introduced into carboxyl on water-reducing agent molecular side chain, improves water-reducing agent
Space steric effect, to obtain higher water-reducing rate；
（2）The present invention is added hydrochloric acid, phosphoric acid formation poly-aspartate, adds taurine to it using L-Aspartic acid as raw material
It is modified, obtains hard water resistance chelating additive, be the polyaminoacid with carboxylic side-chain, there is chelating and peptizaiton,
Containing peptide bond and carboxyl isoreactivity group is largely contained, there is good hydrophily and water solubility ,-COOH is in aqueous solution on side chain
In be easy to ionize, form carboxyl anion, complex reaction can occur with calcium bicarbonate, magnesium bicarbonate in hard water etc., be formed
Soluble ion carries out water-reduction so that water-reducing agent remains to preferably disperse under hard water conditions；
（3）Present invention introduces triethanolamine, the N atom in molecular structure has lone pair electrons, can react with calcium, iron ion etc.
Complex compound is generated, the solubility on concrete particle surface is improved, promotes the aquation of tricalcium aluminate and the generation of entringite, with
Sodium sulphate is compounded, and sulfate ion can react with the calcium hydroxide generated when hydrated cementitious, and it is superfine to generate granularity
Calcium sulfate, thus be easier to react with tricalcium aluminate and generate entringite, to accelerate hydration rate, and then improve hardening of cement
Early strength so that concrete density gets a promotion, while being added montmorillonite, water-reducing agent passes through ion exchange and ion pair
Interlayer is adsorbed with the montmorillonite of negative electrical charge, while C-H bond contained therein can also be nonpolar between montmorillonite layer
Stronger particle occurs Van der Waals force and adsorbs, and negative charge density increases due to having adsorbed anion between montmorillonite layer at this time
Add, the repulsion of interlayer is also increase accordingly, to expand interlamellar spacing, water-reducing agent is uniformly scattered in cement, is improved
Diminishing efficiency.
Specific embodiment
Diminishing activating agent matrix：S1. acrylic acid in mass ratio 2 ~ 5 is taken：1 ~ 3 is added poly glycol monomethyl ether, adds third
The hydroquinone of olefin(e) acid quality 2 ~ 4%, obtains mixture, takes mixture in mass ratio 3 ~ 5：8 ~ 10 are added toluene, are passed through nitrogen guarantor
Shield, adds the p-methyl benzenesulfonic acid of mixture quality 1 ~ 3%, is warming up to 110 ~ 120 DEG C and is stirred 4 ~ 6h, rotary evaporation must revolve
Turn evaporant；
S2. acrylic acid in mass ratio 3 ~ 5 is taken：7 ~ 9 are added N, and N '-dicyclohexylcarbodiimide is stirred 20 ~ 30min, are added
The citric acid that 1 ~ 3 times of acrylic acid quality is stirred 30 ~ 50min in 40 ~ 50 DEG C, add acrylic acid quality 3 ~ 7% to two
Methylamino pyridine is warming up to 60 ~ 70 DEG C and is stirred 10 ~ 12h, and vacuum distillation obtains vacuum distillation object, takes rotary evaporation object by matter
Measure ratio 3 ~ 6：4 ~ 7 are added vacuum distillation object mixing to get diminishing activating agent matrix.
Hard water resistance chelating additive：（1）Take L-Aspartic acid in mass ratio 10 ~ 15：3~5：4 ~ 7 are added mass fraction 36%
Hydrochloric acid, mass fraction be 85% phosphoric acid, obtain mixture a, take mixture a in mass ratio 3 ~ 7：10 ~ 15 are added deionized water,
It is stirred 30 ~ 50min, 150 ~ 160 DEG C of 2 ~ 5h of heat preservation is warming up to, is cooled to room temperature, is freeze-dried, ground 100 mesh
Sieve is collected sieving particle and is washed 3 ~ 6 times through deionized water, obtains washings；
（2）Take sodium hydroxide in mass ratio 2 ~ 5：7 ~ 10 are added deionized water, add 1 ~ 3 times of sodium hydroxide quality of ox sulphur
Acid is stirred 10 ~ 20min, obtains stirring mixture, takes washings in mass ratio 1 ~ 5：8 ~ 10 are added deionized water, are warming up to
35 ~ 45 DEG C, the stirring mixture of washings quality 30 ~ 50% is added, adjusts pH to 7 ~ 7.2, is stirred 1 ~ 3h to get anti-
Hard water chelates additive.
Early strength additive：Take triethanolamine in mass ratio 2 ~ 4：3 ~ 6 are added sodium sulphate mixing to get early strength additive.
A kind of preparation method of efficient cement water reducing agent, includes the following steps：
A. according to the mass fraction, take 6 ~ 9 parts of diminishing activating agent matrixes, 4 ~ 7 parts of acrylic acid, 2 ~ 5 parts of methylpropene sodium sulfonates, 80 ~
90 parts of water, obtain matrix object, are warming up to 50 ~ 60 DEG C, are added dropwise the ammonium persulfate of base matter amount 1 ~ 3%, and control time for adding 40 ~
50min, then be warming up to 60 ~ 70 DEG C and be stirred 3 ~ 5h, pH to 6 ~ 7 is adjusted, is cooled to room temperature, obtains cooled material；
B. according to the mass fraction, 20 ~ 30 parts of cooled materials, 3 ~ 8 parts of hard water resistance chelating additives, 0.03 ~ 0.05 part of morning is taken to add by force
Agent, 8 ~ 15 parts of montmorillonite mixing, dry, pulverize 200 meshes, collect sieving particle a to get efficient cement water reducing agent.
Diminishing activating agent matrix：S1. acrylic acid in mass ratio 2 is taken：1 is added poly glycol monomethyl ether, adds acrylic acid
The hydroquinone of quality 2%, obtains mixture, takes mixture in mass ratio 3：8 are added toluene, are passed through nitrogen protection, add mixing
The p-methyl benzenesulfonic acid of amount of substance 1% is warming up to 110 DEG C and is stirred 4h, and rotary evaporation obtains rotary evaporation object；
S2. acrylic acid in mass ratio 3 is taken：7 are added N, and N '-dicyclohexylcarbodiimide is stirred 20min, and acrylic acid is added
The citric acid that 1 times of quality is stirred 30min in 40 DEG C, add acrylic acid quality 3% to dimethylamino naphthyridine, be warming up to
60 DEG C are stirred 10h, and vacuum distillation obtains vacuum distillation object, takes rotary evaporation object in mass ratio 3：4, which are added vacuum distillation object, mixes
It closes to get diminishing activating agent matrix.
Hard water resistance chelating additive：（1）Take L-Aspartic acid in mass ratio 10：3：The hydrochloric acid of 4 addition mass fractions 36%,
The phosphoric acid that mass fraction is 85%, obtains mixture a, takes mixture a in mass ratio 3：10 are added deionized water, are stirred
30min is warming up to 150 DEG C of heat preservation 2h, is cooled to room temperature, and freeze-drying grinds and sieves with 100 mesh sieve, and collects sieving particle warp
Deionized water is washed 3 times, and washings is obtained；
（2）Take sodium hydroxide in mass ratio 2：7 are added deionized water, add 1 times of sodium hydroxide quality of taurine, and stirring is mixed
10min is closed, stirring mixture is obtained, takes washings in mass ratio 1：8 are added deionized water, are warming up to 35 DEG C, add washings
The stirring mixture of quality 30% adjusts pH to 7, is stirred 1h to get hard water resistance chelating additive.
Early strength additive：Take triethanolamine in mass ratio 2：3 are added sodium sulphate mixing to get early strength additive.
A kind of preparation method of efficient cement water reducing agent, includes the following steps：
A. according to the mass fraction, 6 parts of diminishing activating agent matrixes, 4 parts of acrylic acid, 2 parts of methylpropene sodium sulfonates, 80 parts of water are taken, are obtained
Matrix object is warming up to 50 DEG C, and the ammonium persulfate of base matter amount 1% is added dropwise, and controls time for adding 40min, then be warming up to 60 DEG C and stir
Mixing 3h is mixed, pH to 6 is adjusted, is cooled to room temperature, obtains cooled material；
B. according to the mass fraction, take 20 parts of cooled materials, 3 parts of hard water resistance chelating additives, 0.03 part of early strength additive, 8 parts of illiteracies de-
Stone mixing, dry, pulverize 200 meshes, collect sieving particle a to get efficient cement water reducing agent.
Diminishing activating agent matrix：S1. acrylic acid in mass ratio 4 is taken：2 are added poly glycol monomethyl ether, add acrylic acid
The hydroquinone of quality 3%, obtains mixture, takes mixture in mass ratio 4：9 are added toluene, are passed through nitrogen protection, add mixing
The p-methyl benzenesulfonic acid of amount of substance 2% is warming up to 115 DEG C and is stirred 5h, and rotary evaporation obtains rotary evaporation object；
S2. acrylic acid in mass ratio 4 is taken：8 are added N, and N '-dicyclohexylcarbodiimide is stirred 25min, and acrylic acid is added
The citric acid that 2 times of quality is stirred 40min in 45 DEG C, add acrylic acid quality 5% to dimethylamino naphthyridine, be warming up to
65 DEG C are stirred 11h, and vacuum distillation obtains vacuum distillation object, takes rotary evaporation object in mass ratio 5：5, which are added vacuum distillation object, mixes
It closes to get diminishing activating agent matrix.
Hard water resistance chelating additive：
（1）Take L-Aspartic acid in mass ratio 13：4：5 are added the hydrochloric acid of mass fraction 36%, mass fraction as 85% phosphoric acid, obtain
Mixture a takes mixture a in mass ratio 5：13 are added deionized waters, are stirred 40min, are warming up to 155 DEG C of heat preservation 4h, cold
But to room temperature, freeze-drying grinds and sieves with 100 mesh sieve, and collects sieving particle and washs 5 times through deionized water, obtains washings；
（2）Take sodium hydroxide in mass ratio 4：8 are added deionized water, add 2 times of sodium hydroxide quality of taurine, and stirring is mixed
15min is closed, stirring mixture is obtained, takes washings in mass ratio 4：9 are added deionized water, are warming up to 40 DEG C, add washings
The stirring mixture of quality 40% adjusts pH to 7.1, is stirred 2h to get hard water resistance chelating additive.
Early strength additive：Take triethanolamine in mass ratio 3：5 are added sodium sulphate mixing to get early strength additive.
A kind of preparation method of efficient cement water reducing agent, includes the following steps：
A. according to the mass fraction, 8 parts of diminishing activating agent matrixes, 5 parts of acrylic acid, 3 parts of methylpropene sodium sulfonates, 85 parts of water are taken, are obtained
Matrix object is warming up to 55 DEG C, and the ammonium persulfate of base matter amount 2% is added dropwise, and controls time for adding 45min, then be warming up to 65 DEG C and stir
Mixing 4h is mixed, pH to 6.5 is adjusted, is cooled to room temperature, obtains cooled material；
B. according to the mass fraction, take 25 parts of cooled materials, 6 parts of hard water resistance chelating additives, 0.04 part of early strength additive, 13 parts of illiteracies de-
Stone mixing, dry, pulverize 200 meshes, collect sieving particle a to get efficient cement water reducing agent.
Diminishing activating agent matrix：S1. acrylic acid in mass ratio 5 is taken：3 are added poly glycol monomethyl ether, add acrylic acid
The hydroquinone of quality 4%, obtains mixture, takes mixture in mass ratio 5：10 are added toluene, are passed through nitrogen protection, add mixed
The p-methyl benzenesulfonic acid for closing amount of substance 3%, is warming up to 120 DEG C and is stirred 6h, rotary evaporation obtains rotary evaporation object；
S2. acrylic acid in mass ratio 5 is taken：9 are added N, and N '-dicyclohexylcarbodiimide is stirred 30min, and acrylic acid is added
The citric acid that 3 times of quality is stirred 50min in 50 DEG C, add acrylic acid quality 7% to dimethylamino naphthyridine, be warming up to
70 DEG C are stirred 12h, and vacuum distillation obtains vacuum distillation object, takes rotary evaporation object in mass ratio 6：7, which are added vacuum distillation object, mixes
It closes to get diminishing activating agent matrix.
Hard water resistance chelating additive：
（1）Take L-Aspartic acid in mass ratio 15：5：7 are added the hydrochloric acid of mass fraction 36%, mass fraction as 85% phosphoric acid, obtain
Mixture a takes mixture a in mass ratio 7：15 are added deionized waters, are stirred 50min, are warming up to 160 DEG C of heat preservation 5h, cold
But to room temperature, freeze-drying grinds and sieves with 100 mesh sieve, and collects sieving particle and washs 6 times through deionized water, obtains washings；
（2）Take sodium hydroxide in mass ratio 5：10 are added deionized water, add 3 times of sodium hydroxide quality of taurine, stir
20min is mixed, stirring mixture is obtained, takes washings in mass ratio 5：10 are added deionized water, are warming up to 45 DEG C, add washing
The stirring mixture of amount of substance 50% adjusts pH to 7.2, is stirred 1 ~ 3h to get hard water resistance chelating additive.
Early strength additive：Take triethanolamine in mass ratio 4：6 are added sodium sulphate mixing to get early strength additive.
A kind of preparation method of efficient cement water reducing agent, includes the following steps：
A. according to the mass fraction, 9 parts of diminishing activating agent matrixes, 7 parts of acrylic acid, 5 parts of methylpropene sodium sulfonates, 90 parts of water are taken, are obtained
Matrix object is warming up to 60 DEG C, and the ammonium persulfate of base matter amount 3% is added dropwise, and controls time for adding 50min, then be warming up to 70 DEG C and stir
Mixing 5h is mixed, pH to 7 is adjusted, is cooled to room temperature, obtains cooled material；
B. according to the mass fraction, take 30 parts of cooled materials, 8 parts of hard water resistance chelating additives, 0.05 part of early strength additive, 15 parts of illiteracies de-
Stone mixing, dry, pulverize 200 meshes, collect sieving particle a to get efficient cement water reducing agent.
Comparative example 1：It is essentially identical with the preparation method of embodiment 1, it has only the difference is that lacking diminishing activating agent matrix.
Comparative example 2：It is essentially identical with the preparation method of embodiment 1, it has only the difference is that lacking hard water resistance chelating additive.
Comparative example 3：It is essentially identical with the preparation method of embodiment 1, it has only the difference is that lacking early strength additive.
Comparative example 4：The cement water reducing agent of Dazhou City company production.
Embodiment is tested with the resulting cement water reducing agent of comparative example according to GB/T50081-2002 standard, is tested
The results are shown in Table 1：
Table 1：
| Test item | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 |
| Water-reducing rate（%） | 33 | 31 | 30 | 27 | 29 | 29 | 14.5 |
| Bleeding rate（%） | 18 | 20 | 19 | 19 | 21 | 22 | 41 |
| Air content（%） | 1.5 | 1.6 | 1.7 | 1.9 | 2.0 | 1.8 | 3.2 |
Sample 3g is weighed in 200mL beaker, adds water 97g, be heated to 60-65 DEG C and is put after stirring 5min with glass bar to room
Temperature.It takes supernatant liquor 25mL to pour into test tube, adds in the water for being put in 2 DEG C of 65 DEG C of scholars after artificial hard water 25mL shakes up and keep
1h.Test tube is taken out after 1h, and carries out visual examination immediately, carries out resistance to hard water test after being cooled back to room temperature.Test result
As shown in table 2：
Table 2：
| Test item | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 |
| Whether sediment is had | It is no | It is no | It is no | It is no | Slightly | It is no | Have |
In summary, efficient cement water reducing agent of the invention is more preferable compared to commercial product effect, is worth promoting.
Claims (7)
1. a kind of efficient cement water reducing agent, which is characterized in that including diminishing activating agent matrix, hard water resistance chelating additive, morning
Strong additive；
The preparation method of the diminishing activating agent matrix, includes the following steps：
S1. acrylic acid in mass ratio 2 ~ 5 is taken：1 ~ 3 be added poly glycol monomethyl ether, add acrylic acid quality 2 ~ 4% to benzene two
Phenol obtains mixture, takes mixture in mass ratio 3 ~ 5：8 ~ 10 be added toluene, be passed through nitrogen protection, add mixture quality 1 ~
3% p-methyl benzenesulfonic acid is stirred, rotary evaporation, obtains rotary evaporation object；
S2. acrylic acid in mass ratio 3 ~ 5 is taken：7 ~ 9 are added N, and N '-dicyclohexylcarbodiimide is stirred, and acrylic acid matter is added
1 ~ 3 times of citric acid of amount, is stirred in 40 ~ 50 DEG C, add acrylic acid quality 3 ~ 7% to dimethylamino naphthyridine, be warming up to
60 ~ 70 DEG C are stirred, and vacuum distillation obtains vacuum distillation object, takes rotary evaporation object in mass ratio 3 ~ 6：4 ~ 7 are added vacuum distillation
Object mixes to get diminishing activating agent matrix.
2. efficient cement water reducing agent according to claim 1, which is characterized in that gained rotary evaporation in the step S1
The condition that is stirred of object is：Be warming up to 110 ~ 120 DEG C and be stirred 4 ~ 6h, rotary evaporation to get.
3. efficient cement water reducing agent according to claim 1, which is characterized in that the system of the hard water resistance chelating additive
Preparation Method includes the following steps：
（1）Take L-Aspartic acid in mass ratio 10 ~ 15：3~5：4 ~ 7 are added hydrochloric acid, phosphoric acid, obtain mixture a, take mixture a by matter
Measure ratio 3 ~ 7：10 ~ 15 addition deionized waters are stirred, and are kept the temperature, are cooled to room temperature, are freeze-dried, grind and sieve with 100 mesh sieve,
It collects sieving particle to wash 3 ~ 6 times through deionized water, obtains washings；
（2）Take sodium hydroxide in mass ratio 2 ~ 5：7 ~ 10 are added deionized water, add 1 ~ 3 times of sodium hydroxide quality of taurine
It is stirred, obtains stirring mixture, take washings in mass ratio 1 ~ 5：8 ~ 10 are added deionized waters, are warming up to 35 ~ 45 DEG C, then plus
Enter the stirring mixture of washings quality 30 ~ 50%, adjusts pH to 7 ~ 7.2, be stirred to get hard water resistance chelating additive.
4. efficient cement water reducing agent according to claim 3, which is characterized in that the step step（1）In heat preservation
Condition is：It is warming up to 150 ~ 160 DEG C of 2 ~ 5h of heat preservation.
5. efficient cement water reducing agent according to claim 1, which is characterized in that the early strength additive is：Take three second
Hydramine in mass ratio 2 ~ 4：3 ~ 6 are added sodium sulphate mixing to get early strength additive.
6. a kind of preparation method of the efficient cement water reducing agent as described in claim 1 ~ 5 any one, which is characterized in that should
Preparation method includes the following steps：
A. according to the mass fraction, take 6 ~ 9 parts of diminishing activating agent matrixes, 4 ~ 7 parts of acrylic acid, 2 ~ 5 parts of methylpropene sodium sulfonates, 80 ~
90 parts of water, obtain matrix object, are warming up to 50 ~ 60 DEG C, are added dropwise the ammonium persulfate of base matter amount 1 ~ 3%, and control time for adding 40 ~
50min is stirred, and is adjusted pH to 6 ~ 7, is cooled to room temperature, obtains cooled material；
B. according to the mass fraction, 20 ~ 30 parts of cooled materials, 3 ~ 8 parts of hard water resistance chelating additives, 0.03 ~ 0.05 part of morning is taken to add by force
Agent, 8 ~ 15 parts of montmorillonite mixing, dry, pulverize 200 meshes, collect sieving particle a to get efficient cement water reducing agent.
7. the preparation method of efficient cement water reducing agent according to claim 6, which is characterized in that in the step A
The condition of being stirred is：It is warming up to 60 ~ 70 DEG C and is stirred 3 ~ 5h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810942700.0A CN108821634B (en) | 2018-08-17 | 2018-08-17 | High-efficiency concrete water reducing agent and preparation method thereof |
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| CN113801274A (en) * | 2021-09-17 | 2021-12-17 | 临沂大学 | Poly-like amino acid and preparation method and application thereof |
| CN114262105A (en) * | 2021-12-28 | 2022-04-01 | 普宁市吉润混凝土有限公司 | Carbon neutralization wastewater recycling treatment method and concrete containing wastewater |
| US11629074B2 (en) * | 2018-02-23 | 2023-04-18 | Unique Equipment Solutions Llc | Method for activation of concrete mixing water |
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