CN107987223A - A kind of ester modified high-adaptability polycarboxylate water-reducer of alkyl acrylic and preparation method - Google Patents
A kind of ester modified high-adaptability polycarboxylate water-reducer of alkyl acrylic and preparation method Download PDFInfo
- Publication number
- CN107987223A CN107987223A CN201711239109.0A CN201711239109A CN107987223A CN 107987223 A CN107987223 A CN 107987223A CN 201711239109 A CN201711239109 A CN 201711239109A CN 107987223 A CN107987223 A CN 107987223A
- Authority
- CN
- China
- Prior art keywords
- parts
- water
- reducer
- small
- alkyl
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
- C04B24/24—Macromolecular compounds
- C04B24/26—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B24/2688—Copolymers containing at least three different monomers
- C04B24/2694—Copolymers containing at least three different monomers containing polyether side chains
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/38—Polymerisation using regulators, e.g. chain terminating agents, e.g. telomerisation
-
- C—CHEMISTRY; METALLURGY
- 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
- C08F4/00—Polymerisation catalysts
- C08F4/40—Redox systems
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Polymers & Plastics (AREA)
- Medicinal Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Materials Engineering (AREA)
- Ceramic Engineering (AREA)
- Structural Engineering (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
- Macromonomer-Based Addition Polymer (AREA)
Abstract
The present invention provides a kind of ester modified high-adaptability polycarboxylate water-reducer of alkyl acrylic and preparation method.The polycarboxylate water-reducer includes following parts by weight of component in addition to water：Polyether macromonomer：340 ~ 350 parts, sodium hypophosphite：3.0 ~ 6.0 parts, hydrogen peroxide：0.5 ~ 3.5 part, ammonium persulfate：1.0 ~ 2.0 parts, initiator：101 ~ 123.5 parts, minor comonomer solution：96 ~ 132 parts, alkyl acrylate：2.5 ~ 3.5 parts, industrial lye：10 ~ 25 parts；The method carries out as follows：1st, feed for the first time；2nd, feed for second；3rd, alkyl acrylate is added；4th, prepared by finished product.The present invention introduces long-chain esters class crosslinking agent and cation unsaturated monomer in the molecular structure of water-reducing agent, the poly- carboxyl water-reducing agent is had sustained release and anti-mud effect well, and the water-reducing agent volume is low, and water-reducing rate is high, has excellent slump holding capacity.
Description
Technical field：
The present invention relates to cement-based gelling material polycarboxylic admixture technical field, a kind of alkyl acrylic is related specifically to
Ester modified high-adaptability polycarboxylate water-reducer and preparation method.
Background technology：
Cement performance depends on C in clinker3S and C3A mineral contents, specific surface area, mineral admixture volume and kind, and it is many
The influence power of factor is followed successively by sandstone, cement, mineral admixture, correspond be concrete admixture fluctuate therewith compared with
Greatly.Strong absorption material inferior can accelerate hydrated cementitious, and water-reducing agent is wrapped up by cement granules or hydrated product, space steric effect
It is violent with electrical charge rejection effect decay.The larger method of concrete admixture fluctuation is solved, typically using second generation diminishing
Agent, i.e. naphthalene system, aliphatic, three kinds of sulfamate water reducer is independent or is used in combination, its water-reducing rate is relatively low, easily suppresses concrete
High performance.
For cement, mineral admixture, sandstone the material quality such as material it is changeable in the case of, concrete adaptability influence because
Element depends primarily upon the internal factor of concrete raw material stability, this is appropriate to the occasion using the poly- carboxylic of wide molecular weight distribution high-adaptability type
Sour water-reducing agent, the variation of backbone polymerization degree, in multigroup arrangement, short-chain branch anchoring group hydrophiling is designed as aqueous solvent layer, really
Protect alkyl acrylate and hydrolysis release carboxyl is remained under severe hydrated environment.
106220791 A of patent CN disclose a kind of polycarboxylate water-reducer of phosphorous acidic group, by the raw material of following parts by weight
It is made：70 ~ 80 parts of unsaturated polyether polymeric monomer, 0.3 ~ 1.0 part of hydrogen peroxide, 2 ~ 10 parts of carboxylic acid, 0 ~ 18 part of carboxylate, chain-transferring agent
0.5 ~ 1.5 part, prepare 0.1 ~ 0.2 part of 9 ~ 28 parts of deionized water X, the reducing agent of feed liquid A, prepare the deionized water Y of B liquid
18 ~ 26 parts, for dissolving 45 ~ 80 parts of the deionized water Z of unsaturated polyether polymeric monomer.The polycarboxylic acids of the phosphorous acidic group of the present invention subtracts
Aqua, because introducing phosphate on strand, water-reducing rate is high, and function of slump protection is good, has good sulfate resistance ability and resists
Mud ability.
106008853 A of patent CN disclose a kind of preparation side of the poly- carboxyl water-reducing agent of phosphorous vinegar base of anti-mud collapse protection type
Method, comprises the following steps that：L) preparation of the poly- carboxyl water-reducing agent performed polymer containing halogen：By the unsaturated monomer containing halogen,
Unsaturated acids minor comonomer, unsaturated polyether polymeric monomer or unsaturated esters polymeric monomer are in initiator, reducing agent and chain-transferring agent
Under the action of, carry out redox Raolical polymerizable and obtain the poly- carboxyl water-reducing agent performed polymer containing halogen；2) will contain
The poly- carboxyl water-reducing agent performed polymer of halogen carries out Arbuzov with alkyl phosphate and reacts to obtain the copolymerization product of phosphoric acid ester group,
PH value is adjusted, up to poly- carboxyl based water reducer.
105542091 A of patent CN provide a kind of poly- carboxyl series high-performance of the cation with anti-mud effect that be sustained and subtract
Aqua and preparation method thereof.The present invention is with unsaturated carboxyl, polyether macromonomer, cation unsaturated monomer, unsaturated esters, friendship
It is raw material to join agent, chain-transferring agent, oxidant and reducing agent, and at normal temperatures, no heat source successfully synthesizes the sustained release anti-mud of cationic
Poly- carboxyl high-performance water reducing agent.
The content of the invention：
It is an object of the invention to provide a kind of ester modified high-adaptability polycarboxylate water-reducer of alkyl acrylic and preparation method.
The design philosophy of the present invention is that long-chain esters class crosslinking agent and cation are introduced in the molecular structure of water-reducing agent
Unsaturated monomer, makes the poly- carboxyl water-reducing agent have sustained release and anti-mud effect well, and the water-reducing agent volume is low, and water-reducing rate is high,
With excellent slump holding capacity.And stringent collocation short-chain branch hydrophilic radical, built from hydrophilic minor comonomer and reducing agent
Hydrophilic solvent layer, and control alkyl acrylate, to ensure carboxyl initial polymerization reaction speed, then plus alkyl acrylate
In contain micro p-hydroxyanisole (MEHQ), this polymerization inhibitor controls the number of free radical in polymeric solution, prevents to a certain degree
Form the short small-molecular-weight polycarboxylate water-reducer molecule of main chain.
To achieve the above object, the technical scheme is that:
A kind of ester modified high-adaptability polycarboxylate water-reducer of alkyl acrylic, it is characterised in that：The polycarboxylate water-reducer bag
Containing parts by weight of component as follows in addition to water：
Polyether macromonomer：340 ~ 350 parts, sodium hypophosphite：3.0 ~ 6.0 parts,
Hydrogen peroxide：0.5 ~ 3.5 part, ammonium persulfate：1.0 ~ 2.0 parts,
Initiator：101 ~ 123.5 parts, minor comonomer solution：96 ~ 132 parts,
Alkyl acrylate：2.5 ~ 3.5 parts, industrial lye：10 ~ 25 parts；
Wherein：Initiator is made of 1.0 ~ 3.5 parts of reducing agents and 100 ~ 120 parts of water, minor comonomer solution by 35 ~ 40 parts of acrylic acid,
1.0 ~ 2.0 parts of acrylamides and 60 ~ 90 parts of water compositions.
The polyether macromonomer is allyl polyethenoxy ether, methyl allyl polyoxyethylene ether, prenol polyoxy
One or more of compositions of vinethene, vinyl butyl ether polyoxyethylene ether, the polyether macromonomer is from the angle of slump retaining
Judge, preferably one or two kinds of compositions of isoamyl alcohol polyoxyethylene ether, vinyl butyl ether polyoxyethylene ether；The polyethers is big
Monomer judges from the strong angle of anti-negative electricity adsorbate ability, preferably the isoamyl alcohol polyoxyethylene ether of 2400 molecular weight, ethene
One or two kinds of compositions of base butyl ether polyoxyethylene ether.
The hydrogen peroxide is that mass percent is 27.5% industrial grade hydrogen peroxide.
The reducing agent is sodium dithionite, sodium formaldehyde sulphoxylate, ascorbic acid, sodium hydrogensulfite, Jiao Ya
Sodium sulphate, sodium hypophosphite, Dextrose Monohydrate, one or more of compositions of maltodextrin, preferably in weak property reducing agent, i.e., it is anti-
Bad hematic acid, sodium hydrogensulfite, sodium pyrosulfite, Dextrose Monohydrate, one or more of compositions of maltodextrin, it is preferably neutral and
The combination of weak reductant, i.e. mass ratio 1：5 ascorbic acid and the two of maltodextrin kinds of compositions.
The alkyl acrylate is tridecyl acrylate, perfluor alkyl ethyl acrylate, acrylate alkane
One or more of compositions of methyl acrylate, octadecyl Polyoxyethylene Methyl acryate.
A kind of preparation method of the ester modified high-adaptability polycarboxylate water-reducer of alkyl acrylic, it is characterised in that：The side
Method carries out as follows：
1st, feed for the first time：340 ~ 350 parts of polyether macromonomers, 3.0 ~ 6.0 parts of sodium hypophosphites and 200 ~ 250 parts of water are added to
In reaction kettle, lasting stirring, until solution measures temperature in the kettle, control temperature is 10 ~ 25 without obvious bulk or sheet material
DEG C, disposably put into 0.5 ~ 3.5 part of hydrogen peroxide and 1.0 ~ 2.0 parts of ammonium persulfates；
2nd, feed for second：In charging 2-5 minutes, it is molten to start 101 ~ 123.5 parts of initiators of dropwise addition, 96 ~ 132 parts of minor comonomers successively
Liquid, initiator starts that minor comonomer solution is added dropwise after adding in 6-10 minutes, when minor comonomer solution time for adding is a small, initiator
When time for adding is a+0.5 small；
3rd, alkyl acrylate is added：After when minor comonomer dropwise addition a/3 is small, 2.5 ~ 3.5 parts of alkyl acrylates are disposably put into, it is small
When a/2 is small before monomer solution, 2/3rds mass number of minor comonomer solution is added dropwise, when a/2 is small after minor comonomer solution, is added dropwise small
/ 3rd mass number of monomer solution；
4th, prepared by finished product：After completion of dropwise addition, when curing 0.5-1 is small, question response material temperature in kettle is less than 40 DEG C, is slowly added to 10
~ 25 parts of industrial lyes, and moisturizing to gross mass is 1000 parts, stands, gets product after stirring evenly.
When the minor comonomer solution time for adding a is 2.0-4.0 small.
Compared with prior art, the positive effect of the present invention is:
1st, the present invention introduces long-chain esters class crosslinking agent and cation unsaturated monomer in the molecular structure of water-reducing agent, makes this
Poly- carboxyl water-reducing agent has sustained release and anti-mud effect well, and the water-reducing agent volume is low, and water-reducing rate is high, has excellent slump
Spend holding capacity；
2nd, this method is strictly arranged in pairs or groups short-chain branch hydrophilic radical, hydrophilic solvent layer is built from hydrophilic minor comonomer and reducing agent, and control
Alkyl acrylate processed, to ensure carboxyl initial polymerization reaction speed, containing micro to hydroxyl in the alkyl acrylate then added
Base methyl phenyl ethers anisole (MEHQ), this polymerization inhibitor control the number of free radical in polymeric solution to a certain degree, prevent to be formed short small of main chain
Molecular weight polycarboxy's diminishing agent molecule；
3rd, the amide group of the polyhydroxy of maltodextrin used in the present invention, acrylamide, belongs to hydrophilic radical, can structure
A hydrophilic short solvent anchor layer is built, to ensure the hydrolysis of alkyl acrylate；
4th, the sodium hypophosphite chain-transferring agent used in this method, its feature are that chain transfer ability is weak, can be formed main chain compared with
Long polycarboxylate water-reducer molecule, to reduce the initial adsorption amount of water-reducing agent, and resists thing of the strong adsorbate to polyethers long-chain branch
Manage intercalation absorption；
5th, small monomer solution takes frequency conversion speed to be added dropwise in this method synthesis technique, and sodium hypophosphite is made except performance chain-transferring agent
With can also make strong anchoring group；Strong reductant and weak reductant in being used in reducing agent, middle strong reductant and excessive weak reduction
Agent matching is to ensure water-reducing agent extent of polymerization, and organic weak reductant small molecule more than needed is except lubricating action is played, also as excellent
First adsorbent is filled in adsorbate, ensures the diminishing effect of diminishing agent molecule.
Specific embodiment
Clear, complete description is further carried out to technical scheme with reference to embodiment.
Embodiment 1：
The ester modified high-adaptability polycarboxylate water-reducer of alkyl acrylic, is polymerized by following each components, and gross mass part is 1000,
Preparation method is specific as follows：
1st, feed for the first time：By the isoamyl alcohol polyoxyethylene ether of 341 part of 2400 molecular weight, 4.0 parts of sodium hypophosphites and 200 parts
Water is added in reaction kettle, lasting stirring, until solution is without obvious bulk or sheet material；Temperature in the kettle is measured, controls temperature
At 12 DEG C, 3.2 part of 27.5% industrial grade hydrogen peroxide and 1.0 parts of ammonium persulfates are disposably put into；
2nd, feed for second：In charging 2-5 minutes, start that initiator, minor comonomer solution is added dropwise successively；Initiator is by 2.0 parts of matter
Measure ratio 1：5 ascorbic acid and maltodextrin and 100 parts of water compositions；Initiator after adding starts that small list is added dropwise in 6-10 minutes
Liquid solution, minor comonomer solution are made of 40 parts of acrylic acid, 2.0 parts of acrylamides and 60 parts of water；Minor comonomer solution time for adding is 3
Hour, when initiator time for adding is 3.5 small；
3rd, alkyl acrylate is added：After when minor comonomer dropwise addition 1 is small, 2.5 parts of tridecyl acrylate are disposably put into；Small list
Before liquid solution 1.5 it is small when, be added dropwise minor comonomer solution 2/3rds mass number；After minor comonomer solution 1.5 it is small when, small list is added dropwise
/ 3rd mass number of liquid solution；
4th, prepared by finished product：After completion of dropwise addition, when curing 0.5 is small, question response material temperature in kettle is less than 40 DEG C, is slowly added to 23 parts
Industrial lye, and moisturizing to gross mass is 1000 parts, stands, gets product after stirring evenly.
Embodiment 2
The ester modified high-adaptability polycarboxylate water-reducer of alkyl acrylic, is polymerized by following each components, and gross mass part is 1000,
Preparation method is specific as follows：
1st, feed for the first time：By the isoamyl alcohol polyoxyethylene ether of 342 part of 2400 molecular weight, 5.0 parts of sodium hypophosphites and 220 parts
Water is added in reaction kettle, lasting stirring, until solution is without obvious bulk or sheet material；Temperature in the kettle is measured, controls temperature
At 15 DEG C, 2.8 part of 27.5% industrial grade hydrogen peroxide and 1.5 parts of ammonium persulfates are disposably put into；
2nd, feed for second：In charging 2-5 minutes, start that initiator, minor comonomer solution is added dropwise successively；Initiator is by 3.5 parts of matter
Measure ratio 1：5 ascorbic acid and maltodextrin and 110 parts of water compositions；Initiator after adding starts that small list is added dropwise in 6-10 minutes
Liquid solution, minor comonomer solution are made of 36 parts of acrylic acid, 1.0 parts of acrylamides and 80 parts of water；Minor comonomer solution time for adding is 2
Hour, when initiator time for adding is 2.5 small；
3rd, alkyl acrylate is added：After when minor comonomer dropwise addition 2/3 is small, 3.5 parts of octadecyl polyoxyethylene first are disposably put into
Base acrylate；Before minor comonomer solution 1 it is small when, be added dropwise minor comonomer solution 2/3rds mass number；1 is small after minor comonomer solution
When, 1/3rd mass number of dropwise addition minor comonomer solution；
4th, prepared by finished product：After completion of dropwise addition, when curing 0.7 is small, question response material temperature in kettle is less than 40 DEG C, is slowly added to 20 parts
Industrial lye, and moisturizing to gross mass is 1000 parts, stands, gets product after stirring evenly.
Embodiment 3
The ester modified high-adaptability polycarboxylate water-reducer of alkyl acrylic, is polymerized by following each components, and gross mass part is 1000,
Preparation method is specific as follows：
1st, feed for the first time：By the vinyl butyl ether polyoxyethylene ether of 345 part of 2400 molecular weight, 3.0 parts of sodium hypophosphites and
240 parts of water are added in reaction kettle, lasting stirring, until solution is without obvious bulk or sheet material；Measure temperature in the kettle, control
Temperature disposably puts into 1.5 part of 27.5% industrial grade hydrogen peroxide and 2.0 parts of ammonium persulfates at 18 DEG C；
2nd, feed for second：In charging 2-5 minutes, start that initiator, minor comonomer solution is added dropwise successively；Initiator is by 2.0 parts of matter
Measure ratio 1：5 ascorbic acid and maltodextrin and 120 parts of water compositions；Initiator after adding starts that small list is added dropwise in 6-10 minutes
Liquid solution, minor comonomer solution are made of 35 parts of acrylic acid, 1.5 parts of acrylamides and 90 parts of water；Minor comonomer solution time for adding is
2.5 it is small when, initiator time for adding for 3.0 it is small when；
3rd, alkyl acrylate is added：After 2.5/3 lab scale is added dropwise in minor comonomer, 3.5 parts of perfluor alkyl ethide propylene are disposably put into
Acid esters；Before minor comonomer solution 1.25 it is small when, be added dropwise minor comonomer solution 2/3rds mass number；1.25 is small after minor comonomer solution
When, 1/3rd mass number of dropwise addition minor comonomer solution；
4th, prepared by finished product：After completion of dropwise addition, when curing 0.8 is small, question response material temperature in kettle is less than 40 DEG C, is slowly added to 19 parts
Industrial lye, and moisturizing to gross mass is 1000 parts, stands, gets product after stirring evenly.
Embodiment 4
The ester modified high-adaptability polycarboxylate water-reducer of alkyl acrylic, is polymerized by following each components, and gross mass part is 1000,
Preparation method is specific as follows：
1st, feed for the first time：By the isoamyl alcohol polyoxyethylene ether of 347 part of 2400 molecular weight, 3.5 parts of sodium hypophosphites and 250 parts
Water is added in reaction kettle, lasting stirring, until solution is without obvious bulk or sheet material；Temperature in the kettle is measured, controls temperature
At 22 DEG C, 2.5 part of 27.5% industrial grade hydrogen peroxide and 1.0 parts of ammonium persulfates are disposably put into；
2nd, feed for second：In charging 2-5 minutes, start that initiator, minor comonomer solution is added dropwise successively；Initiator is by 2.0 parts of matter
Measure ratio 1：5 ascorbic acid and maltodextrin and 115 parts of water compositions；Initiator after adding starts that small list is added dropwise in 6-10 minutes
Liquid solution, minor comonomer solution are made of 36 parts of acrylic acid, 2.0 parts of acrylamides and 85 parts of water；Minor comonomer solution time for adding is 3
Hour, when initiator time for adding is 3.5 small；
3rd, alkyl acrylate is added：After a/3 lab scales are added dropwise in minor comonomer, 3.0 parts of perfluor alkyl ethide acrylic acid are disposably put into
Ester；Before minor comonomer solution 1.5 it is small when, be added dropwise minor comonomer solution 2/3rds mass number；After minor comonomer solution 1.5 it is small when,
/ 3rd mass number of minor comonomer solution is added dropwise；
4th, prepared by finished product：After completion of dropwise addition, when curing 1 is small, question response material temperature in kettle is less than 40 DEG C, is slowly added to 17 parts of works
Industry liquid caustic soda, and moisturizing to gross mass is 1000 parts, stands, gets product after stirring evenly.
Embodiment 5
The ester modified high-adaptability polycarboxylate water-reducer of alkyl acrylic, is polymerized by following each components, and gross mass part is 1000,
Preparation method is specific as follows：
1st, feed for the first time：By the isoamyl alcohol polyoxyethylene ether of 348 part of 2400 molecular weight, 4.5 parts of sodium hypophosphites and 245 parts
Water is added in reaction kettle, lasting stirring, until solution is without obvious bulk or sheet material；Temperature in the kettle is measured, controls temperature
At 25 DEG C, 1.5 part of 27.5% industrial grade hydrogen peroxide and 2.0 parts of ammonium persulfates are disposably put into；
2nd, feed for second：In charging 2-5 minutes, start that initiator, minor comonomer solution is added dropwise successively；Initiator is by 2.0 parts of matter
Measure ratio 1：5 ascorbic acid and maltodextrin and 110 parts of water compositions；Initiator after adding starts that small list is added dropwise in 6-10 minutes
Liquid solution, minor comonomer solution are made of 35 parts of acrylic acid, 1.0 parts of acrylamides and 90 parts of water；Minor comonomer solution time for adding is 3
Hour, when initiator time for adding is 3.5 small；
3rd, alkyl acrylate is added：After when minor comonomer dropwise addition 1 is small, 2.5 parts of acrylate alkyl methyl propylene are disposably put into
Acid esters；Before minor comonomer solution 1.5 it is small when, be added dropwise minor comonomer solution 2/3rds mass number；1.5 is small after minor comonomer solution
When, 1/3rd mass number of dropwise addition minor comonomer solution；
4th, prepared by finished product：After completion of dropwise addition, when curing 1 is small, question response material temperature in kettle is less than 40 DEG C, is slowly added to 15 parts of works
Industry liquid caustic soda, and moisturizing to gross mass is 1000 parts, stands, gets product after stirring evenly.
Example detection result：
Test the ester modified high-adaptability polycarboxylate water-reducer of examples detailed above alkyl acrylic respectively and common polycarboxylate water-reducer is same
Concrete initial slump/divergence under isoconcentration and through when the slump/divergence.Cement used in experiment is general for Three Gorges 42.5
Silicon cement, clay content is larger in sandstone, with reference to GB/8076-2008《Concrete admixture》Testing standard.
Different water-reducing agents influence concrete flowability
| Water-reducing agent species | Initial slump/divergence mm | Through when the slump/divergence mm |
| Ordinary water-reducing agent | 180/540 | 160/480 |
| Embodiment 1 | 205/570 | 180/545 |
| Embodiment 2 | 210/580 | 190/555 |
| Embodiment 3 | 205/570 | 180/560 |
| Embodiment 4 | 210/580 | 190/565 |
| Embodiment 5 | 200/570 | 180/570 |
Compared according to above-mentioned concrete flowability, the ester modified high-adaptability polycarboxylate water-reducer example 1 of alkyl acrylic, 2,3,4,
5 initial fluidity is relatively a little bigger compared with ordinary water-reducing agent mother liquor, and protects more notable, the anti-mud excellent performance that collapses；Trace it to its cause
It is that alkyl acrylate increases anchoring ability, and can improves concrete workability again after the larger phosphatide ester hydrolysis of steric hindrance
And slump retaining, comprehensive performance are obviously improved.
All features disclosed in this specification, or disclosed all formulas and volume, except mutually exclusive feature and/
Or beyond formula, volume, it can combine in any way.This specification（Including claim, summary）Disclosed in any
Feature, unless specifically stated, can be replaced by other alternative features that are equivalent or have similar purpose.Remove and non-specifically chat
State, each feature is an example in a series of equivalent or similar characteristics.
Described above is only the non-limiting embodiment of invention, substantial amounts of embodiment can also be derived, for this area
Those of ordinary skill for, do not departing from the invention design and on the premise of not making creative work, can also do
Go out the embodiment of several modifications and improvements, these belong to protection scope of the present invention.
Claims (7)
- A kind of 1. ester modified high-adaptability polycarboxylate water-reducer of alkyl acrylic, it is characterised in that：The polycarboxylate water-reducer Include parts by weight of component as follows in addition to water：Polyether macromonomer：340 ~ 350 parts, sodium hypophosphite：3.0 ~ 6.0 parts,Hydrogen peroxide：0.5 ~ 3.5 part, ammonium persulfate：1.0 ~ 2.0 parts,Initiator：101 ~ 123.5 parts, minor comonomer solution：96 ~ 132 parts,Alkyl acrylate：2.5 ~ 3.5 parts, industrial lye：10 ~ 25 parts；Wherein：Initiator is made of 1.0 ~ 3.5 parts of reducing agents and 100 ~ 120 parts of water, minor comonomer solution by 35 ~ 40 parts of acrylic acid, 1.0 ~ 2.0 parts of acrylamides and 60 ~ 90 parts of water compositions.
- 2. the ester modified high-adaptability polycarboxylate water-reducer of alkyl acrylic according to claim 1, it is characterised in that：It is described Polyether macromonomer for allyl polyethenoxy ether, methyl allyl polyoxyethylene ether, isoamyl alcohol polyoxyethylene ether, vinyl One or more of compositions of butyl ether polyoxyethylene ether, the preferably isoamyl alcohol polyoxyethylene ether of 2400 molecular weight, vinyl fourth One or two kinds of compositions of base ether polyoxyethylene ether.
- 3. the ester modified high-adaptability polycarboxylate water-reducer of alkyl acrylic according to claim 1, it is characterised in that：It is described Hydrogen peroxide be that mass percent is 27.5% industrial grade hydrogen peroxide.
- 4. the ester modified high-adaptability polycarboxylate water-reducer of alkyl acrylic according to claim 1, it is characterised in that：It is described Reducing agent for sodium dithionite, sodium formaldehyde sulphoxylate, ascorbic acid, sodium hydrogensulfite, sodium pyrosulfite, secondary phosphorous Sour sodium, Dextrose Monohydrate, one or more of compositions of maltodextrin, preferably neutral and weak reductant combination, i.e. mass ratio 1：5 ascorbic acid and the two of maltodextrin kinds of compositions.
- 5. the ester modified high-adaptability polycarboxylate water-reducer of alkyl acrylic according to claim 1, it is characterised in that：It is described Alkyl acrylate for tridecyl acrylate, perfluor alkyl ethyl acrylate, acrylate alkyl methacrylate One or more of compositions of ester, octadecyl Polyoxyethylene Methyl acryate.
- A kind of 6. preparation method of the ester modified high-adaptability polycarboxylate water-reducer of alkyl acrylic, it is characterised in that：The method Carry out as follows：1) feed for the first time：340 ~ 350 parts of polyether macromonomers, 3.0 ~ 6.0 parts of sodium hypophosphites and 200 ~ 250 parts of water are added to In reaction kettle, lasting stirring, until solution measures temperature in the kettle, control temperature is 10 ~ 25 without obvious bulk or sheet material DEG C, disposably put into 0.5 ~ 3.5 part of hydrogen peroxide and 1.0 ~ 2.0 parts of ammonium persulfates；2) feed for second：In charging 2-5 minutes, it is molten to start 101 ~ 123.5 parts of initiators of dropwise addition, 96 ~ 132 parts of minor comonomers successively Liquid, initiator starts that minor comonomer solution is added dropwise after adding in 6-10 minutes, when minor comonomer solution time for adding is a small, initiator When time for adding is a+0.5 small；3) alkyl acrylate is added：After when minor comonomer dropwise addition a/3 is small, 2.5 ~ 3.5 parts of alkyl acrylates are disposably put into, it is small When a/2 is small before monomer solution, 2/3rds mass number of minor comonomer solution is added dropwise, when a/2 is small after minor comonomer solution, is added dropwise small / 3rd mass number of monomer solution；4) prepared by finished product：After completion of dropwise addition, when curing 0.5-1 is small, question response material temperature in kettle is less than 40 DEG C, is slowly added to 10 ~ 25 parts of industrial lyes, and moisturizing to gross mass is 1000 parts, stands, gets product after stirring evenly.
- 7. the preparation method of the ester modified high-adaptability polycarboxylate water-reducer of alkyl acrylic according to claim 6, it is special Sign is：When the minor comonomer solution time for adding a is 2.0-4.0 small.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711239109.0A CN107987223A (en) | 2017-11-30 | 2017-11-30 | A kind of ester modified high-adaptability polycarboxylate water-reducer of alkyl acrylic and preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711239109.0A CN107987223A (en) | 2017-11-30 | 2017-11-30 | A kind of ester modified high-adaptability polycarboxylate water-reducer of alkyl acrylic and preparation method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107987223A true CN107987223A (en) | 2018-05-04 |
Family
ID=62034609
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711239109.0A Pending CN107987223A (en) | 2017-11-30 | 2017-11-30 | A kind of ester modified high-adaptability polycarboxylate water-reducer of alkyl acrylic and preparation method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107987223A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109569240A (en) * | 2018-12-14 | 2019-04-05 | 山东汇之蓝环保科技有限公司 | NO_x Reduction by Effective ionic liquid and its application method |
| CN110240676A (en) * | 2019-04-10 | 2019-09-17 | 武汉理工大学 | A kind of preparation method of solid polycarboxylic acid water reducing agent |
| CN110540620A (en) * | 2019-01-09 | 2019-12-06 | 咸阳鸿鑫建材有限公司 | polycarboxylate superplasticizer and preparation method thereof |
| CN112062910A (en) * | 2020-09-09 | 2020-12-11 | 安徽海螺新材料科技有限公司 | Micro-crosslinking anti-mud polycarboxylate superplasticizer and preparation method thereof |
| CN116715815A (en) * | 2023-08-10 | 2023-09-08 | 北京慕湖外加剂有限公司 | Slump-retaining water reducer and preparation method and application thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20140031486A1 (en) * | 2012-07-26 | 2014-01-30 | The Sherwin-Williams Company | Waterborne coatings |
| CN105061690A (en) * | 2015-07-22 | 2015-11-18 | 江苏奥莱特新材料有限公司 | Preparation method for high performance water reducer made from high water reducing solid polycarboxylic acid |
| CN105110687A (en) * | 2015-07-30 | 2015-12-02 | 厦门路桥翔通建材科技有限公司 | Mud resisting and slump retaining type polycarboxylic acids water reducer and preparation method thereof |
| CN106632885A (en) * | 2016-10-27 | 2017-05-10 | 湖北工业大学 | Short-haul-distance high-flowability low-slump-retaining polycarboxylate water reducer master batch |
| CN106977129A (en) * | 2017-04-10 | 2017-07-25 | 河北润砼新材料科技有限公司 | Anti- mud collapse protective poly-carboxylic acid high efficiency water reducing agent and preparation method thereof |
-
2017
- 2017-11-30 CN CN201711239109.0A patent/CN107987223A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20140031486A1 (en) * | 2012-07-26 | 2014-01-30 | The Sherwin-Williams Company | Waterborne coatings |
| CN105061690A (en) * | 2015-07-22 | 2015-11-18 | 江苏奥莱特新材料有限公司 | Preparation method for high performance water reducer made from high water reducing solid polycarboxylic acid |
| CN105110687A (en) * | 2015-07-30 | 2015-12-02 | 厦门路桥翔通建材科技有限公司 | Mud resisting and slump retaining type polycarboxylic acids water reducer and preparation method thereof |
| CN106632885A (en) * | 2016-10-27 | 2017-05-10 | 湖北工业大学 | Short-haul-distance high-flowability low-slump-retaining polycarboxylate water reducer master batch |
| CN106977129A (en) * | 2017-04-10 | 2017-07-25 | 河北润砼新材料科技有限公司 | Anti- mud collapse protective poly-carboxylic acid high efficiency water reducing agent and preparation method thereof |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109569240A (en) * | 2018-12-14 | 2019-04-05 | 山东汇之蓝环保科技有限公司 | NO_x Reduction by Effective ionic liquid and its application method |
| CN109569240B (en) * | 2018-12-14 | 2021-08-13 | 山东汇之蓝环保科技有限公司 | Efficient denitration ionic liquid and use method thereof |
| CN110540620A (en) * | 2019-01-09 | 2019-12-06 | 咸阳鸿鑫建材有限公司 | polycarboxylate superplasticizer and preparation method thereof |
| CN110240676A (en) * | 2019-04-10 | 2019-09-17 | 武汉理工大学 | A kind of preparation method of solid polycarboxylic acid water reducing agent |
| CN112062910A (en) * | 2020-09-09 | 2020-12-11 | 安徽海螺新材料科技有限公司 | Micro-crosslinking anti-mud polycarboxylate superplasticizer and preparation method thereof |
| CN116715815A (en) * | 2023-08-10 | 2023-09-08 | 北京慕湖外加剂有限公司 | Slump-retaining water reducer and preparation method and application thereof |
| CN116715815B (en) * | 2023-08-10 | 2023-11-07 | 北京慕湖外加剂有限公司 | Slump-retaining water reducer and preparation method and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107987223A (en) | A kind of ester modified high-adaptability polycarboxylate water-reducer of alkyl acrylic and preparation method | |
| CN107987224A (en) | A kind of short-chain branch crosslinking water conservation solvent layer control release type polycarboxylic acid slump retaining agent and preparation method | |
| CN105110687B (en) | A kind of anti-mud collapse protective poly-carboxylic acid water reducing agent and preparation method thereof | |
| CN106008853B (en) | A kind of preparation method of anti-mud collapse protection type phosphate ester-containing based polycarboxylic acid water-reducing agent | |
| CN105754047B (en) | A kind of phosphate ester-containing high-adaptability polycarboxylate water-reducer and preparation method thereof | |
| CN104231182B (en) | A kind of esters collapse protective poly-carboxylic acid water reducing agent and preparation method thereof | |
| CN109021181A (en) | A kind of poly carboxylic acid series water reducer and preparation method thereof for having both viscosity reduction and protecting function of collapsing | |
| CN102976655B (en) | Slump retaining polycarboxylic acid superplasticizer | |
| CN102515618A (en) | Slow release slump retaining polycarboxylate water reducer and preparation thereof | |
| CN110642993B (en) | Preparation method of retarding ether polycarboxylate superplasticizer | |
| CN106749972B (en) | A kind of prefabricated components low slump Early-strength polycarboxylate superplasticizer masterbatch | |
| CN106046269B (en) | A kind of cross-linking type muting sensitive sense ester ether copoly type polycarboxylate water-reducer and preparation method thereof | |
| CN106432628B (en) | A kind of muting sensitive induction reactance mud ether-ether copoly type polycarboxylate water-reducer and preparation method thereof | |
| CN105294953B (en) | A kind of preparation method of polycarboxylic acid slump retaining agent | |
| CN109467632B (en) | Long-acting slow-release polycarboxylic slump retaining agent and preparation method thereof | |
| CN107987225A (en) | A kind of anti-negative electricity adsorbate phosphate polycarboxylate water-reducer and low temperature preparation method | |
| CN108864374A (en) | A kind of preparation method of the high water-retaining type polycarboxylate water-reducer of ethers | |
| CN108047396A (en) | A kind of anti-chamotte mould polycarboxylate water-reducer of polycation and preparation method thereof | |
| CN109111551A (en) | A kind of anti-chamotte mould polycarboxylate water-reducer preparation method of 3000 molecular weight polyethers | |
| CN114014999A (en) | Method for preparing polycarboxylate superplasticizer from six-carbon polyether and polycarboxylate superplasticizer | |
| CN108276533A (en) | A kind of high ecad polycarboxylate water-reducer and preparation method thereof | |
| CN112708041B (en) | Esterification product for preparing water reducing agent and preparation method thereof, and reduction type ether polycarboxylic acid water reducing agent and preparation method thereof | |
| CN111378076A (en) | Polycarboxylate superplasticizer with high temperature adaptability and preparation method thereof | |
| CN109400825A (en) | A kind of low responsive type polycarboxylate water-reducer and preparation method thereof with anti-mud effect | |
| CN111533862A (en) | High-water-retention type lipid polycarboxylate superplasticizer and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180504 |