CN105884978A - Coagulating early strength type polycarboxylate superplasticizer and preparing method thereof - Google Patents
Coagulating early strength type polycarboxylate superplasticizer and preparing method thereof Download PDFInfo
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Abstract
The invention discloses a coagulating early strength type polycarboxylate superplasticizer and a preparing method thereof. The superplasticizer is prepared from, by weight, 1-3 parts of quaternary ammonium salt cationic monomer with end double bonds, 190-210 parts of polyether monomer, 16-18 parts of unsaturated monocarboxylic acid and derivatives thereof, 1.5-2.0 parts of oxidizing agent, 0.1-0.3 part of first reducing agent, 0.1-0.3 part of second reducing agent, 0.8-0.9 part of chain transfer agent, 14-18 parts of alkaline modifier and 210-230 parts of water. The superplasticizer has a remarkable cement hydration reaction promoting function, can shorten molding template plastering and initial setting time obviously when applied to steam curing concrete, low-temperature environment concrete and concrete with early form removal requirement, and has a prominent early strength effect; meanwhile, thixotropic property is high, concrete construction progress can be accelerated, and template transfer rate can be increased.
Description
Technical field
The invention belongs to technical field of concrete additives, be specifically related to a kind of coagulant Early-strength polycarboxylate superplasticizer and system thereof
Preparation Method.
Background technology
Along with the quickening of concrete works project construction, the consumption of precast concrete product also presents ever-increasing trend.Phase
Than in normal concrete, precast concrete requires that concrete has preferable early strength development speed, to improve template turnover
Rate, or meet the strength development under cryogenic conditions, the production period of precast concrete is extended to even winter in late autumn, and right
Concrete durability also has higher requirement.Realize polycarboxylate water-reducer coagulant early powerful technological approaches and have two kinds: be a kind of
Being that synthetic polymer itself has good coagulant early epistasis energy, another is the polycarboxylate water-reducer that synthesis is conventional, passes through
Compound and reach coagulant early potent fruit.
CN101024565A is disclosed one and is obtained by accelerating components such as compounding anhydrous calcium chloride, triethanolamine, sodium benzoate
Strong composite water-reducing agent morning arrived, can improve comprcssive strength to a certain extent, but not mentioned whether has coagulant effect, and contains
Villaumite, has corrosion to armored concrete；Japan Patent JP6005050 discloses and a kind of uses the compound of sodium carbonate and aluminum sulfate
Type early strength agent, can improve the early strength of concrete, but be easily caused later stage degradation, and improve the alkali in concrete
Content, can accelerate alkali.In sum, use traditional inorganic salt or organic accelerating component, can make water reducer in
Alkalescence or strong basicity, be the most easily layered, and causes water reducer poor storage stability, and the later stage that simultaneously can make concrete is strong
Degree declines.
CN101376576B discloses a kind of early strength type polycarboxylic acid series high-performance dehydragent and preparation technology, this technical side
Case uses the Polyethylene Glycol monoether esters of acrylic acid polymeric monomer of two kinds of different chain numbers, (methyl) acrylic acid, allyl sulphonic acid
Sodium or methylpropene sodium sulfonate, there is the polyoxyalkylene acrylate esters monomer of defoaming function under nitrogen protective condition, take once
The mode fed intake carries out copolyreaction.CN101357834B discloses a kind of early-strength polycarboxylic acids plasticiser, and this invention is adopted
By the methoxy poly (ethylene glycol) carboxylic acid esters polymeric monomer of different molecular weight, (methyl) acrylic acid, 2-acrylamide-2-methyl-prop
Prepared by sulfonic acid and random/block ether copolymerization in the aqueous solution of 60 DEG C～90 DEG C.All there is early potent fruit in above technical scheme
Inconspicuous, and produce and early sacrifice part water-reducing property by force simultaneously, cause the problems such as cost increase.
Summary of the invention
It is an object of the invention to overcome prior art defect, it is provided that a kind of coagulant Early-strength polycarboxylate superplasticizer.
Another object of the present invention is to provide the preparation method of above-mentioned coagulant Early-strength polycarboxylate superplasticizer.
The concrete technical scheme of the present invention is as follows:
A kind of coagulant Early-strength polycarboxylate superplasticizer, is made up of the raw material components of following weight portion: have the quaternary ammonium of terminal double bond
Salt cationic monomer 1～3 weight portion, polyether monomer 190～210 weight portion, unsaturated monocarboxylic acid and derivant 16～18 thereof
Weight portion, oxidant 1.5～2.0 weight portion, the first reducing agent 0.1～0.3 weight portion, the second reducing agent 0.1～0.3 weight portion,
Chain-transferring agent 0.8～0.9 weight portion, alkaline conditioner 14～18 weight portion and water 210～230 weight portion, the first reducing agent and
The weight ratio of the second reducing agent is 1:1～3, wherein,
Polyether monomer is isobutene alcohol polyoxyethylene ether and/or the prenol polyoxyethylene of number-average molecular weight 3000～6000
Base ether；
The quaternaries cation monomer with terminal double bond is MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, acryloyl-oxy second
Base trimethyl ammonium chloride or diallyldimethylammonium chloride；
First reducing agent is 2-hydroxyl-2-sulfinatoacetic acid, 2-hydroxyl-2-sulfinatoacetic acid disodium salt, 2-hydroxyl-2-sulphur
Acidic group acetic acid or 2-hydroxyl-2-sulfonatoacetic acid disodium salt；
Second reducing agent is that azo two isobutyl imidazoline hydrochloride, azo diisobutyl amidine hydrochlorate, azo two N-hydroxyl are different
Butyl amidine hydrate, azo two N, N ' cyclobutyl isobutyl amidine hydrate or azo dimethyl N-2-hydroxyl butylacrylamide.
In a preferred embodiment of the invention, described unsaturated monocarboxylic acid and derivant thereof are acrylic acid, methyl-prop
Olefin(e) acid, 2-(Acryloyloxy)ethanol, hydroxyethyl methylacrylate, Hydroxypropyl acrylate, Hydroxypropyl methacrylate, acrylic acid first
At least one in ester, methyl methacrylate, acrylamide and Methacrylamide.
In a preferred embodiment of the invention, described oxidant is Ammonium persulfate., potassium peroxydisulfate, sodium peroxydisulfate or mistake
Hydrogen oxide.
In a preferred embodiment of the invention, described chain-transferring agent is that TGA, thioglycerin, 3-mercaptopropionic acid are different
Monooctyl ester, lauryl mercaptan, 3-mercaptopropionic acid or mercaptosuccinic acid..
In a preferred embodiment of the invention, described alkaline conditioner be sodium hydroxide solution, potassium hydroxide solution,
Ethanolamine, diethanolamine, triethanolamine, isopropanolamine, diisopropanolamine (DIPA), triisopropanolamine, dihydroxy ethyl ethylenediamine,
At least one in dihydroxypropyl ethylenediamine, tetrahydroxyethyl-ethylene diamine and tetrahydroxypropyl ethylenediamine.
It is further preferred that its pH value is 6～7.
The preparation method of a kind of above-mentioned coagulant Early-strength polycarboxylate superplasticizer, comprises the steps:
(1) will have quaternaries cation monomer, polyether monomer, oxidant and 148～160 weight portions of terminal double bond
Water mixes, then adjusts pH to 4～6 with part unsaturated monocarboxylic acid, in 15～30 DEG C of stirrings to dissolving；
(2) with remaining water, the first reducing agent, the second reducing agent, chain-transferring agent and remaining unsaturated monocarboxylic acid are divided
It is not configured to reductant solution, chain-transferring agent solution and unsaturated monocarboxylic acid solution；
(3) above-mentioned reductant solution, chain-transferring agent solution and unsaturated monocarboxylic acid solution are dripped in 3～4h simultaneously
To the material of step (1), after dropping at 35～40 DEG C insulation reaction 1～1.5h；
(4) after the material reaction of step (3) is complete, add in alkaline conditioner and pH to 6～7, obtain described coagulant
Early-strength polycarboxylate superplasticizer.
The invention has the beneficial effects as follows:
1, the coagulant Early-strength polycarboxylate superplasticizer of the present invention has the prominent function promoting hydrated reaction of cement, is applied to
Steam-curing concrete, low temperature environment concrete and have a concrete of form removal requirement ahead of time, can be significantly shorter smearing of forming panel
Face and presetting period, there is the most potent fruit, the most also there is good thixotropic property, the construction of concrete can be accelerated
Progress, improves the turnover rate of template.
2, the preparation method of the coagulant Early-strength polycarboxylate superplasticizer of the present invention passes through molecule tailoring technology, to master, side chain radical
Group equimolecular structure be designed, reaction bed material in add part unsaturated monocarboxylic acid, regulation bed material in pH value in
Faintly acid, and use the combined oxidation reduction initiating system that activity is higher to cause Raolical polymerizable, overcome the strongest
Type water reducer water-reducing rate bad disadvantage the highest, slump-retaining, has prominent dispersive property.
3, the preparation method of the coagulant Early-strength polycarboxylate superplasticizer of the present invention is carried out completely under normal pressure and temperature, simple to operate,
With short production cycle, with low cost.
Detailed description of the invention
Below by way of detailed description of the invention technical scheme it is further detailed and describes.
Embodiment 1
Equipped with thermometer, agitator, peristaltic pump four-hole boiling flask in add 1.5 weight portion methylacryoyloxyethyl front threes
Ammonium chloride, 200 parts by weight of isobutylene polyoxyethylenated alcohol polymeric monomer (molecular weight Mw is 3000), 1.5 weight portion over cures
Acid ammonium and 156 weight parts waters, add 7 parts by weight of acrylic acid, and regulation bed material pH value is 4～5, stirs at 20 DEG C.
After to be dissolved, by 0.15 weight portion 2-hydroxyl-2-sulfinatoacetic acid, 0.15 weight portion azo two isobutyl imidazoline hydrochloride
The chain tra nsfer that the water of the reductant solution, 0.8 weight portion TGA and 25 weight portions that are made into the water of 25 weight portions is made into
The unsaturated monocarboxylic acid solution that the water of agent solution and the acrylic acid of 10 weight portions and 15 weight portions is made into, is simultaneously added dropwise above-mentioned
Reductant solution, chain-transferring agent solution and unsaturated monocarboxylic acid solution, time for adding is 3 hours, after completion of dropwise addition
Insulation reaction 1 hour at 35～40 DEG C.After having reacted, it is neutralized to pH value with 16 weight portion 32% sodium hydroxide
6～7, thus obtain coagulant Early-strength polycarboxylate superplasticizer PCE-1.
Embodiment 2
Equipped with thermometer, agitator, peristaltic pump four-hole boiling flask in add 2 parts by weight propylene acyloxyethyl trimethyl ammonia chloride
Ammonium, 200 parts by weight of isobutylene polyoxyethylenated alcohol polymeric monomer (molecular weight Mw is 4000), 1.6 weight portion sodium peroxydisulfates and
158 weight parts waters, add 6 weight parts of methacrylic acid, and regulation bed material pH value is 4～5, stirs at 25 DEG C.Treat
After dissolving, by 0.25 weight portion 2-hydroxyl-2-sulfinatoacetic acid disodium salt, 0.30 weight portion azo diisobutyl amidine hydrochloric acid
The chain that reductant solution that the water of salt and 25 weight portions is made into, the water of 0.9 weight portion 3-mercaptopropionic acid 25 weight portion are made into turns
Move the unsaturated monocarboxylic acid solution that the water of agent solution and the methacrylic acid of 10 weight portions and 15 weight portions is made into, drip simultaneously
Adding above-mentioned reductant solution, chain-transferring agent solution and unsaturated monocarboxylic acid solution, time for adding is 3 hours, dropping knot
After bundle at 35～40 DEG C insulation reaction 1 hour.After having reacted, it is neutralized to pH value 6～7 with 15 weight portion triethanolamine,
Thus obtain coagulant Early-strength polycarboxylate superplasticizer PCE-2.
Embodiment 3
Equipped with thermometer, agitator, peristaltic pump four-hole boiling flask in add 3 weight portion diallyldimethylammonium chlorides,
200 parts by weight of isobutylene polyoxyethylenated alcohol polymeric monomer (molecular weight Mw is 5000), 1.9 weight portion potassium peroxydisulfates and 158
Weight parts water, adds 5 parts by weight of acrylic acid hydroxyl ethyl esters, and regulation bed material pH value is 5～6, stirs at 30 DEG C.Treat molten
Xie Hou, by 0.18 weight portion 2-hydroxyl-2-sulfonatoacetic acid, 0.2 weight portion azo two N-hydroxyisobutyl amidine hydrate with
The chain-transferring agent that the water of reductant solution, 0.8 weight portion thioglycerin and 25 weight portions that the water of 25 weight portions is made into is made into is molten
The unsaturated monocarboxylic acid solution that the water of liquid and the 2-(Acryloyloxy)ethanol of 12 weight portions and 15 weight portions is made into, is simultaneously added dropwise
Stating reductant solution, chain-transferring agent solution and unsaturated monocarboxylic acid solution, time for adding is 3 hours, after completion of dropwise addition
Insulation reaction 1 hour at 35～40 DEG C.After having reacted, after being cooled to 30 DEG C, it is neutralized to 18 weight portion ethylenediamines
PH value 6～7, thus obtain coagulant Early-strength polycarboxylate superplasticizer PCE-3.
Embodiment 4
Equipped with thermometer, agitator, peristaltic pump four-hole boiling flask in add 1 weight portion methylacryoyloxyethyl trimethyl
Ammonium chloride, 200 parts by weight of isobutylene polyoxyethylenated alcohol polymeric monomer (molecular weight Mw is 6000), 1.5 weight portion hydrogen peroxide
And 149 weight parts waters, adding 7 parts by weight of acrylic acid methyl ester, regulation bed material pH value is 4～5, stirs at 15 DEG C.
After to be dissolved, by 0.13 weight portion 2-hydroxyl-2-sulfonatoacetic acid disodium salt, azo two N, the N ' cyclobutyl of 0.25 weight portion
Reductant solution that the water of isobutyl amidine hydrate and 25 weight portions is made into, 0.8 weight portion 3-isooctyl mercaptopropionate and 25
Chain-transferring agent solution that the water of weight portion is made into and the unsaturation that the water of the acrylic acid methyl ester. of 10 weight portions and 15 weight portions is made into
Monocarboxylic acid solution, is simultaneously added dropwise above-mentioned reductant solution, chain-transferring agent solution and unsaturated monocarboxylic acid solution, during dropping
Between be 3 hours, after completion of dropwise addition at 35～40 DEG C be incubated 1 hour.After having reacted, with 14 parts by weight of isopropyl alcohol amine
It is neutralized to pH value 6～7, thus obtains coagulant Early-strength polycarboxylate superplasticizer PCE-4.
Embodiment 5
The above-mentioned coagulant Early-strength polycarboxylate superplasticizer that embodiments of the invention 1 to 4 are given is " mixed according to GB/T8077-2012
Solidifying soil additive homogeneity test method " relevant criterion that specifies carries out paste flowing degree test, and cement is Fujian good fortune cement
42.5R, control sample is certain Products external, and code name is PCE-0, and testing result is as shown in the table:
Concrete mix is cement: flyash: breeze: sand: stone=330:70:40:698:1126.Wherein: cement is Fujian good fortune P.O
42.5R, flyash is II grade of ash, and sand is the medium sand of modulus of fineness 2.7, and stone is particle diameter 5～20 continuous grading rubble, proportioning
For weight portion；Going out the machine slump at 70 ± 20mm, design strength is C50；With reference to GB8076-2008, " concrete is additional
Agent " the relevant regulations test mobility of concrete and setting time.Shown in test result see table:
Skilled person will appreciate that, when the component of the present invention and technical parameter change in following ranges, still be able to obtain with
The technique effect that above-described embodiment is same or like:
A kind of coagulant Early-strength polycarboxylate superplasticizer, pH value is 6～7, is made up of the raw material components of following weight portion: have
Quaternaries cation monomer 1～3 weight portion of terminal double bond, polyether monomer 190～210 weight portion, unsaturated unitary carboxylic
Acid and derivant 16～18 weight portion, oxidant 1.5～2.0 weight portion, the first reducing agent 0.1～0.3 weight portion, second
Reducing agent 0.1～0.3 weight portion, chain-transferring agent 0.8～0.9 weight portion, alkaline conditioner 14～18 weight portion and water 210～230
Weight portion, the weight ratio of the first reducing agent and the second reducing agent is 1:1～3, wherein,
Polyether monomer is isobutene alcohol polyoxyethylene ether and/or the prenol polyoxyethylene of number-average molecular weight 3000～6000
Base ether；
The quaternaries cation monomer with terminal double bond is MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, acryloyl-oxy second
Base trimethyl ammonium chloride or diallyldimethylammonium chloride；
First reducing agent is 2-hydroxyl-2-sulfinatoacetic acid, 2-hydroxyl-2-sulfinatoacetic acid disodium salt, 2-hydroxyl-2-sulphur
Acidic group acetic acid or 2-hydroxyl-2-sulfonatoacetic acid disodium salt；
Second reducing agent is that azo two isobutyl imidazoline hydrochloride, azo diisobutyl amidine hydrochlorate, azo two N-hydroxyl are different
Butyl amidine hydrate, azo two N, N ' cyclobutyl isobutyl amidine hydrate or azo dimethyl N-2-hydroxyl butylacrylamide；
Unsaturated monocarboxylic acid and derivant thereof be acrylic acid, methacrylic acid, 2-(Acryloyloxy)ethanol, hydroxyethyl methylacrylate,
Hydroxypropyl acrylate, Hydroxypropyl methacrylate, acrylic acid methyl ester., methyl methacrylate, acrylamide and metering system
At least one in amide.
Oxidant is Ammonium persulfate., potassium peroxydisulfate, sodium peroxydisulfate or hydrogen peroxide.
Chain-transferring agent is TGA, thioglycerin, 3-isooctyl mercaptopropionate, lauryl mercaptan, 3-mercaptopropionic acid or sulfur
For malic acid.
Alkaline conditioner is sodium hydroxide solution, potassium hydroxide solution, ethanolamine, diethanolamine, triethanolamine, isopropanol
Amine, diisopropanolamine (DIPA), triisopropanolamine, dihydroxy ethyl ethylenediamine, dihydroxypropyl ethylenediamine, tetrahydroxyethyl-ethylene diamine and four
At least one in hydroxypropylethylendiamine diamine.
The preparation method of a kind of above-mentioned coagulant Early-strength polycarboxylate superplasticizer, comprises the steps:
(1) will have quaternaries cation monomer, polyether monomer, oxidant and 148～160 weight portions of terminal double bond
Water mixes, then adjusts pH to 4～6 with part unsaturated monocarboxylic acid, in 15～30 DEG C of stirrings to dissolving；
(2) with remaining water, the first reducing agent, the second reducing agent, chain-transferring agent and remaining unsaturated monocarboxylic acid are divided
It is not configured to reductant solution, chain-transferring agent solution and unsaturated monocarboxylic acid solution；
(3) above-mentioned reductant solution, chain-transferring agent solution and unsaturated monocarboxylic acid solution are dripped in 3～4h simultaneously
To the material of step (1), after dropping at 35～40 DEG C insulation reaction 1～1.5h；
(4) after the material reaction of step (3) is complete, add in alkaline conditioner and pH to 6～7, obtain described coagulant
Early-strength polycarboxylate superplasticizer.
The above, only presently preferred embodiments of the present invention, therefore the scope that the present invention implements can not be limited according to this, i.e. depend on
The equivalence change that the scope of the claims of the present invention and description are made with modify, all should still belong in the range of the present invention contains.
Claims (7)
1. a coagulant Early-strength polycarboxylate superplasticizer, it is characterised in that: it is made up of the raw material components of following weight portion: tool
There are quaternaries cation monomer 1～3 weight portion of terminal double bond, polyether monomer 190～210 weight portion, unsaturated unitary
Carboxylic acid and derivant 16～18 weight portion thereof, oxidant 1.5～2.0 weight portion, the first reducing agent 0.1～0.3 weight portion,
Two reducing agent 0.1～0.3 weight portions, chain-transferring agent 0.8～0.9 weight portion, alkaline conditioner 14～18 weight portion and water 210～230
Weight portion, the weight ratio of the first reducing agent and the second reducing agent is 1:1～3, wherein,
Polyether monomer is isobutene alcohol polyoxyethylene ether and/or the prenol polyoxyethylene of number-average molecular weight 3000～6000
Base ether；
The quaternaries cation monomer with terminal double bond is MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, acryloyl-oxy second
Base trimethyl ammonium chloride or diallyldimethylammonium chloride；
First reducing agent is 2-hydroxyl-2-sulfinatoacetic acid, 2-hydroxyl-2-sulfinatoacetic acid disodium salt, 2-hydroxyl-2-sulphur
Acidic group acetic acid or 2-hydroxyl-2-sulfonatoacetic acid disodium salt；
Second reducing agent is that azo two isobutyl imidazoline hydrochloride, azo diisobutyl amidine hydrochlorate, azo two N-hydroxyl are different
Butyl amidine hydrate, azo two N, N ' cyclobutyl isobutyl amidine hydrate or azo dimethyl N-2-hydroxyl butylacrylamide.
2. a kind of coagulant Early-strength polycarboxylate superplasticizer as claimed in claim 1, it is characterised in that: described unsaturated one
Unit's carboxylic acid and derivant thereof are acrylic acid, methacrylic acid, 2-(Acryloyloxy)ethanol, hydroxyethyl methylacrylate, acrylic acid hydroxyl
In propyl ester, Hydroxypropyl methacrylate, acrylic acid methyl ester., methyl methacrylate, acrylamide and Methacrylamide
At least one.
3. a kind of coagulant Early-strength polycarboxylate superplasticizer as claimed in claim 1, it is characterised in that: described oxidant is
Ammonium persulfate., potassium peroxydisulfate, sodium peroxydisulfate or hydrogen peroxide.
4. a kind of coagulant Early-strength polycarboxylate superplasticizer as claimed in claim 1, it is characterised in that: described chain-transferring agent
For TGA, thioglycerin, 3-isooctyl mercaptopropionate, lauryl mercaptan, 3-mercaptopropionic acid or mercaptosuccinic acid..
5. a kind of coagulant Early-strength polycarboxylate superplasticizer as claimed in claim 1, it is characterised in that: described alkalescence regulation
Agent is sodium hydroxide solution, potassium hydroxide solution, ethanolamine, diethanolamine, triethanolamine, isopropanolamine, diisopropanol
Amine, triisopropanolamine, dihydroxy ethyl ethylenediamine, dihydroxypropyl ethylenediamine, tetrahydroxyethyl-ethylene diamine and tetrahydroxypropyl ethylenediamine
In at least one.
6. the coagulant Early-strength polycarboxylate superplasticizer as described in any claim in claim 1 to 5, it is characterised in that:
Its pH value is 6～7.
7. a preparation method for coagulant Early-strength polycarboxylate superplasticizer described in any claim in claim 1 to 6,
It is characterized in that: comprise the steps:
(1) will have quaternaries cation monomer, polyether monomer, oxidant and 148～160 weight portions of terminal double bond
Water mixes, then adjusts pH to 4～6 with part unsaturated monocarboxylic acid, in 15～30 DEG C of stirrings to dissolving；
(2) with remaining water, the first reducing agent, the second reducing agent, chain-transferring agent and remaining unsaturated monocarboxylic acid are divided
It is not configured to reductant solution, chain-transferring agent solution and unsaturated monocarboxylic acid solution；
(3) above-mentioned reductant solution, chain-transferring agent solution and unsaturated monocarboxylic acid solution are dripped in 3～4h simultaneously
To the material of step (1), after dropping at 35～40 DEG C insulation reaction 1～1.5h；
(4) after the material reaction of step (3) is complete, add in alkaline conditioner and pH to 6～7, obtain described coagulant
Early-strength polycarboxylate superplasticizer.
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