CN109627394A - A kind of polycarboxylate concrete dehydragent and preparation method thereof being adapted to Machine-made Sand - Google Patents
A kind of polycarboxylate concrete dehydragent and preparation method thereof being adapted to Machine-made Sand Download PDFInfo
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- CN109627394A CN109627394A CN201811458283.9A CN201811458283A CN109627394A CN 109627394 A CN109627394 A CN 109627394A CN 201811458283 A CN201811458283 A CN 201811458283A CN 109627394 A CN109627394 A CN 109627394A
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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
- C08F283/065—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals on to unsaturated 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
- C04B24/16—Sulfur-containing compounds
- C04B24/161—Macromolecular compounds comprising sulfonate or sulfate groups
- C04B24/163—Macromolecular compounds comprising sulfonate or sulfate groups obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B24/165—Macromolecular compounds comprising sulfonate or sulfate groups obtained by reactions only involving carbon-to-carbon unsaturated bonds 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
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/58—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide containing oxygen in addition to the carbonamido oxygen, e.g. N-methylolacrylamide, N-(meth)acryloylmorpholine
-
- 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
-
- 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
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/58—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide containing oxygen in addition to the carbonamido oxygen, e.g. N-methylolacrylamide, N-(meth)acryloylmorpholine
- C08F220/585—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide containing oxygen in addition to the carbonamido oxygen, e.g. N-methylolacrylamide, N-(meth)acryloylmorpholine and containing other heteroatoms, e.g. 2-acrylamido-2-methylpropane sulfonic acid [AMPS]
Abstract
A kind of polycarboxylate concrete dehydragent and preparation method thereof being adapted to Machine-made Sand, by polymeric monomer isobutene alcohol polyoxyethylene ether and water, initiator sodium hydrogensulfite, after stirring is completely dissolved, it is heated to 55~70 DEG C, acrylic acid, the aqueous solution of high surface monomer 2- acrylamido dodecyl sodium sulfonate and the aqueous solution of initiator sodium peroxydisulfate is added dropwise respectively again, 2~3h is added dropwise；2-3h is kept the temperature after completion of dropwise addition, is cooled to room temperature to it, adjusts pH value to 6~7 to get a kind of polycarboxylate concrete dehydragent for being adapted to Machine-made Sand with organic alkali neutralization；New polycarboxylic acid water reducer of the invention can also be obviously improved concrete bleed effect, workability, wrapped, early strength, have a good application prospect to the wetability of Machine-made Sand.
Description
Technical field
The invention belongs to architecture engineering material technical field, in particular to a kind of polycarboxylate coagulation for being adapted to Machine-made Sand
Native water-reducing agent and preparation method thereof.
Background technique
Polycarboxylate water-reducer is the essential additive of one of concrete utilization.Polycarboxylate water-reducer is widely applied
In engineerings such as highway, bridge, dam, tunnel, skyscrapers.It is because of environmentally protective, nonflammable and non-explosive performance.With me
The continuous consumption of state's quality sand and stone resources, Machine-made Sand use are a kind of inexorable trends, Machine-made Sand be rock by Mechanical Crushing and
At mineral resources, equipment and the technique of Machine-made Sand in all parts of the country are not quite similar, and cause Machine-made Sand in appearance, chemical component, granulated
The aspect of performance such as shape, grain composition and special fine particle content are all different not to the utmost from natural sand.Machine-made Sand due to through crushing and
It obtains, surface corner angle are clearly demarcated, contain the problems such as fine powder amount is big, and surface wettability is poor, water-reducing agent especially polycarboxylate dehydragent one
Directly there is a problem of big, bad adaptability of loss etc., causes water-reducing rate low and function of slump protection is insufficient.Currently, because of Machine-made Sand bring
Concrete loss is big and bad adaptability this technical problem is not still well solved.CN201810273310.9 is reported
A kind of polycarboxylate water-reducer and preparation method thereof used for machine-made sand concrete is adopted as replacing part hydroxyl with phosphate radical
Base and the enol polyoxyethylene ether formed.With can obviously improve because the loss of Machine-made Sand bring concrete is big and bad adaptability
The problem of, intensity it is high and the advantages of can obviously reduce overall cost.But the polycarboxylate water-reducer still has the profit to Machine-made Sand
It is moist, water-reducing rate is low, it is wrapped difference the problems such as；CN106749963A discloses a kind of bleed for pure machine-made sand concrete can
Control type poly carboxylic acid series water reducer and preparation method thereof, this method pass through alkyl phenol polyoxyethylene ether monomer and unsaturated carboxylic acid monomer
Carry out esterification generate unsaturated carboxylic acid-alkyl phenol polyoxyethylene ether carboxylate monomer, then by unsaturated carboxylic acid monomer, no
Saturated carboxylic acid-alkyl phenol polyoxyethylene ether carboxylate monomer, unsaturated polyether monomer and unsaturated sulfonic acid monomer passes through oxidation
Reduction initiating system carries out aqueous solution copolymerization reaction and is prepared to obtain bleed controllable type poly carboxylic acid series water reducer
Water-reducing agent is applied in pure machine-made sand concrete, have water-reducing rate is high, adaptability is good, bubble diameter is small, closed stablity, bleed can
The advantages that control, but just can play a role wetting, adjustment effect after the hydrolysis of its polymeric monomer nonylphenol polyoxyethylene ether, especially
Package, water-reducing rate etc. to initial stage concrete gravel are influenced by certain.CN104788629B discloses a kind of polycarboxylic acids diminishing
Agent and its normal temperature preparation method.Organo-silicon coupling agent and lignosulfonates are introduced in polycarboxylic acids synthesis as wetability group
Point, there is good water conservation cohesiveness in concrete especially machine-made sand concrete application, but organosilicon composition can not be very
Improve water-reducing agent well to sandstone package and Problem of Wettability.CN108409193A discloses a kind of strong coagulation of Machine-made Sand C120 superelevation
The preparation method of native polycarboxylic admixture, the additive include water reducing type polycarboxylate water-reducer, viscosity reduction type polycarboxylate water-reducer,
The components such as retarder, defoaming agent can be effectively improved Machine-made Sand super high strength concrete due to Machine-made Sand disproportionately graded itself, granulated
Concrete caused by looks difference, which easily pump, to be isolated and low water binder ratio, large dosage glue material bring viscosity is excessive, fluidity is small, pumpable
The problems such as property is poor, can satisfy the requirement of super high-rise building pumping construction, but have to wetability and early strength improvement result
Limit.
Summary of the invention
In order to overcome the above-mentioned deficiencies of the prior art, the purpose of the present invention is to provide a kind of poly- carboxylics for being adapted to Machine-made Sand
Hydrochlorate cement water reducing agent and preparation method thereof, has that wetability is good, bleed effect is good, and the slump is kept with high water reducing rate etc.
Advantage.
To achieve the goals above, the technical solution adopted by the present invention is that:
A kind of polycarboxylate concrete dehydragent being adapted to Machine-made Sand, using the method for aqueous solution polymerization, by matching below
Than being synthesized:
Isobutene alcohol polyoxyethylene ether (HPEG, 2400), mass parts are 240 parts；
Acrylic acid (AA), mass parts are 18.5~32.5 parts；
2- acrylamido dodecyl sodium sulfonate (AMC12S), mass parts are 4.0~10.0 parts；
Distilled water: mass parts are 360 parts；
Initiator: sodium hydrogensulfite, mass parts are 5.8~11.5 parts, and sodium peroxydisulfate, mass parts are 5.8~11.5 parts, are made
Used time sodium hydrogensulfite and sodium peroxydisulfate mass ratio remain 1:1.
A kind of preparation method for the polycarboxylate concrete dehydragent being adapted to Machine-made Sand, includes the following steps:
(1) distilled water of 240 parts of quality of HPEG and amount of distilled water is put into the reaction vessel with stirring, stirring is complete
After dissolution, initiator sodium hydrogensulfite is added, after heating, heat preservation；
(2) acrylic acid (AA), 2- acrylamide are sequentially added in the distilled water that a quality is 60 parts of total amount of distilled water
Base dodecyl sodium sulfonate (AMC12S after dissolution) is mixed it is known as that component 1 is added dropwise；
Initiator sodium peroxydisulfate is added in the distilled water that another quality is 60 parts of total amount of distilled water, is known as dripping after dissolution
Add component 2；
(3) dropwise addition component 1 and dropwise addition group in above-mentioned steps (2) is added dropwise in the reaction vessel described in step (1) simultaneously
Divide 2, is reacted, preserving heat after reaction ends are cooled to room temperature to it；
(4) it is to obtain a kind of polycarboxylate concrete diminishing for being adapted to Machine-made Sand that organic base, which is added, and adjusts pH to 6~7
Agent.
The organic base is monoethanolamine or diethanol amine.
Temperature rises to 55~75 DEG C in the step (1).
Reaction temperature is 55~75 DEG C, 2~3h of time for adding, 2~3h of preserving heat after reaction ends in the step (3).
The 2- acrylamido dodecyl sodium sulfonate can be bought, and can also be synthesized, Homemade method is as follows:
2- acrylamido dodecyl sodium sulfonate the preparation method is as follows: in a kettle be added 33.6kg 1- 12
The acrylonitrile (excess) of alkene, the dehydrating agent of 5.6kg and 150kg is cooled to 0 DEG C hereinafter, under stiring, the smoke of 21.4kg is added dropwise
Sulfuric acid (50%), control reaction temperature is no more than 5 DEG C during being added dropwise, and oleum reacts 30min again after adding, then heat up
To 25 DEG C, reaction for 24 hours, after the reaction time reaches, reaction mixture is cooled to 5 DEG C hereinafter, filter out excessive acrylonitrile, will
Products therefrom successively uses acrylonitrile and acetone washing, and vacuum drying obtains white powder 2- acrylamido dodecyl sodium sulfonate,
Conversion ratio 87%.
Beneficial effects of the present invention:
A kind of polycarboxylate water-reducer being adapted to Machine-made Sand of the invention is on the basis of keeping good water-reducing property to machine
Sand processed has many advantages, such as significant wetability, improves the wrapped of concrete, the holding slump, raising early strength, can overcome
Polycarboxylate water-reducer is sensitive to Machine-made Sand, accelerates the construction speed of machine-made sand concrete.
Specific embodiment
Below with reference to embodiment, invention is further described in detail.
Embodiment 1
24g isobutene alcohol polyoxyethylene ether (2400) are added into the reaction vessel equipped with blender, 24g distillation is added
Water stirs to dissolve, and is redissolved 0.58g sodium hydrogensulfite, rises to 55 DEG C to temperature, starts while component 1 is added dropwise (to be steamed by 6g
Acrylic acid 1.85g, 2- acrylamido dodecyl sodium sulfonate 0.4g is successively dissolved in distilled water to form) and be added dropwise component 2 (steamed by 6g
It dissolves initiator sodium peroxydisulfate 0.58g in distilled water to form)；2.0h is added dropwise, keeps the temperature 3h, is cooled to room temperature to reactant, with a second
Hydramine adjusts pH value between 6~7, obtains a kind of polycarboxylate water-reducer for being adapted to Machine-made Sand.
Embodiment 2
24g isobutene alcohol polyoxyethylene ether (2400) are added into the reaction vessel equipped with blender, 24g distillation is added
Water stirs to dissolve, and is redissolved 1.15g sodium hydrogensulfite, rises to 70 DEG C to temperature, starts while component 1 is added dropwise (to be steamed by 6g
Acrylic acid 3.25g, 2- acrylamido dodecyl sodium sulfonate 0.60g is successively dissolved in distilled water to form) and component 2 is added dropwise (by 6g
It dissolves initiator ammonium persulfate 1.15g in distilled water to form)；3.0h is added dropwise, keeps the temperature 2.0h, is cooled to room temperature to reactant, uses
Diethanol amine adjusts pH value between 6~7, obtains a kind of polycarboxylate water-reducer for being adapted to Machine-made Sand.
Embodiment 3
24g isobutene alcohol polyoxyethylene ether (2400) are added into the reaction vessel equipped with blender, 24g distillation is added
Water stirs to dissolve, and is redissolved 0.85g sodium hydrogensulfite, rises to 60 DEG C to temperature, starts while component 1 is added dropwise (to be steamed by 6g
Acrylic acid 2.25g, 2- acrylamido dodecyl sodium sulfonate 1.0g is successively dissolved in distilled water to form) and be added dropwise component 2 (steamed by 6g
It dissolves initiator potassium persulfate 0.85g in distilled water to form)；2.5h is added dropwise, 60 DEG C of heat preservation 2h are cooled to room temperature to reactant, are used
Monoethanolamine adjusts pH value between 6~7, obtains a kind of polycarboxylate water-reducer for being adapted to Machine-made Sand.
Comparative example:
24g isobutene alcohol polyoxyethylene ether (2400) are added into the reaction vessel equipped with blender, 24g distillation is added
Water stirs to dissolve, and rises to 70 DEG C to temperature, starts while component 1 is added dropwise (by successively dissolving acrylic acid in 6g distilled water
2.20g, methallylsulfonic acid sodium 0.45g are formed) and component 2 is added dropwise (by dissolving initiator ammonium persulfate in 6g distilled water
0.80g is formed)；2h is added dropwise, keeps the temperature 3h, is cooled to room temperature to reactant, between sodium hydroxide adjusting pH value to 6~7, obtains
A kind of common polycarboxylate water-reducer.
The performance test results of embodiment compare:
According to GB/T8077-2000, examination criteria detects (volume 1.8%), test experience the result is as follows:
Test result is as it can be seen that embodiment and comparative example can find that the mortar specimen early stage that the water-reducing agent of early strong monomer is added is anti-
Compressive Strength is above the effect of the water-reducing agent of comparative example, and the polycarboxylate water-reducer after illustrating to be added early strong monomer is keeping certain
With preferable early strong effect, it can be achieved that early strong purpose on the basis of water-reducing rate.
Claims (6)
1. a kind of polycarboxylate concrete dehydragent for being adapted to Machine-made Sand, which is characterized in that using the method for aqueous solution polymerization,
It is synthesized according to the following ratio:
Isobutene alcohol polyoxyethylene ether, mass parts are 240 parts；
Acrylic acid, mass parts are 18.5~32.5 parts；
2- acrylamido dodecyl sodium sulfonate, mass parts are 4.0~10.0 parts；
Distilled water: mass parts are 360 parts；
Initiator: sodium hydrogensulfite, mass parts are 5.8~11.5 parts, and sodium peroxydisulfate, mass parts are 5.8~11.5 parts, when use
Sodium hydrogensulfite and sodium peroxydisulfate mass ratio remain 1:1.
2. based on a kind of preparation method for the polycarboxylate concrete dehydragent for being adapted to Machine-made Sand described in claim 1, packet
Include following steps:
(1) distilled water of 240 parts of quality of HPEG and amount of distilled water is put into the reaction vessel with stirring, stirring is completely dissolved
Afterwards, initiator sodium hydrogensulfite is added, temperature rises to 55~75 DEG C, heat preservation；
(2) acrylic acid, 2- acrylamido dodecane are sequentially added in the distilled water that a quality is 60 parts of total amount of distilled water
Base sulfonic acid after dissolution is mixed is known as that component 1 is added dropwise；
Initiator sodium peroxydisulfate is added in the distilled water that another quality is 60 parts of total amount of distilled water, dropwise addition group is known as after dissolution
Divide 2；
(3) dropwise addition component 1 and dropwise addition component 2 in above-mentioned steps (2) is added dropwise in the reaction vessel described in step (1) simultaneously,
Reaction temperature be 55~75 DEG C, 2~3h of time for adding, after keep the temperature 2~3h, be cooled to room temperature to it；
(4) it is to obtain a kind of polycarboxylate concrete dehydragent for being adapted to Machine-made Sand that organic base, which is added, and adjusts pH to 6~7.
3. a kind of preparation method of polycarboxylate concrete dehydragent for being adapted to Machine-made Sand according to claim 2,
It is characterized in that, the organic base is monoethanolamine or diethanol amine.
4. a kind of preparation method of polycarboxylate concrete dehydragent for being adapted to Machine-made Sand according to claim 2,
It is characterized in that, temperature rises to 55~75 DEG C in the step (1).
5. a kind of preparation method of polycarboxylate concrete dehydragent for being adapted to Machine-made Sand according to claim 2,
It is characterized in that, reaction temperature is 55~75 DEG C, 2~3h of time for adding, 2~3h of preserving heat after reaction ends in the step (3).
6. a kind of preparation method of polycarboxylate concrete dehydragent for being adapted to Machine-made Sand according to claim 2,
It being characterized in that, the 2- acrylamido dodecyl sodium sulfonate can be bought, it can also synthesize, Homemade method is as follows:
2- acrylamido dodecyl sodium sulfonate the preparation method is as follows: in a kettle be added 33.6kg 1- laurylene,
The dehydrating agent of 5.6kg and the acrylonitrile of 150kg are cooled to 0 DEG C hereinafter, under stiring, the oleum of 21.4kg is added dropwise, are added dropwise
Control reaction temperature is no more than 5 DEG C in the process, and oleum reacts 30min after adding again, then heats to 25 DEG C, reacts for 24 hours,
After the reaction time reaches, reaction mixture is cooled to 5 DEG C hereinafter, filter out excessive acrylonitrile, products therefrom is successively used
Acrylonitrile and acetone washing, vacuum drying, obtain white powder 2- acrylamido dodecyl sodium sulfonate, conversion ratio 87%.
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| CN111153627A (en) * | 2020-01-03 | 2020-05-15 | 同济大学 | Anti-mud additive suitable for machine-made sand concrete and compounding method thereof |
| CN112920342A (en) * | 2021-02-04 | 2021-06-08 | 江苏超力建材科技有限公司 | Early-strength polycarboxylate superplasticizer and preparation method thereof |
| CN113527589A (en) * | 2021-06-24 | 2021-10-22 | 运城市泓翔建材有限公司 | Polycarboxylate superplasticizer suitable for machine-made sand and preparation method thereof |
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| CN113527589A (en) * | 2021-06-24 | 2021-10-22 | 运城市泓翔建材有限公司 | Polycarboxylate superplasticizer suitable for machine-made sand and preparation method thereof |
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