CN106589254A - Anti-mud polycarboxylate water reducing agent masterbatch with monoalkyl phosphate and di-alkyl phosphate branches - Google Patents
Anti-mud polycarboxylate water reducing agent masterbatch with monoalkyl phosphate and di-alkyl phosphate branches Download PDFInfo
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- CN106589254A CN106589254A CN201611116054.XA CN201611116054A CN106589254A CN 106589254 A CN106589254 A CN 106589254A CN 201611116054 A CN201611116054 A CN 201611116054A CN 106589254 A CN106589254 A CN 106589254A
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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
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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
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/24—Macromolecular compounds
- C04B24/243—Phosphorus-containing polymers
- C04B24/246—Phosphorus-containing polymers containing polyether side chains
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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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
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Abstract
The invention discloses anti-mud polycarboxylate water reducing agent masterbatch with mono-di-alkyl phosphate branches. The masterbatch is used for higher-content clay minerals in gravel materials. The masterbatch shows characteristics of not low initial water reduction rate, good slump retaining property in the medium and late stages and good overall stability. In terms of 1000 parts of the total mass of the synthesis raw materials, 40% in percentage by mass, as the limit, of the masterbatch comprises the raw materials as follows: 350-360 parts of polyether macromonomers, 32.0-38.0 parts of acrylic acid, 2.0-6.0 parts of mono-di-alkyl phosphate, 1.0-5.0 parts of a phosphate chain transfer agent, 0.5-1.0 part of mercaptoacetic acid, 3.0-6.0 parts of hydrogen peroxide, 0.5-0.8 parts of vitamin C, 7-15 parts of liquid alkali and the balance of water. A synthesized polycarboxylate water reducing agent has large molecular weight and longer main chain, comprises long and short staggered branches, and is high in density, high in slump retaining property and wide in adaptability.
Description
Technical field
The present invention relates to a kind of anti-chamotte mould polycarboxylate water-reducer masterbatch of single bisalkyl phosphate side chain, is adapted to sandstone ground material
The higher situation of CLAY MINERALS AND THEIR SIGNIFICANCE content, belongs to cement additire field.
Background technology
The features such as polycarboxylate water-reducer is strengthened with high diminishing, high-thin arch dam, height, in high-speed railway, water conservancy and hydropower, nuclear power, height
The heavy constructions such as fast highway, bay harbour are widely applied；But with the high efficiency water reducing agent ratio such as naphthalene system, sulfamate system
Compared with the water-reducing rate of polycarboxylate water-reducer, slump retaining are more sensitive to sandstone clay content.It is negatively charged clay to trace it to its cause
Grain interacts with PCE molecules and positively charged cement granules, reduces absorbability of the cement granules to PCE, reduces
Active adsorption amounts of the PCE in cement particle surface.
Now PEG classes sacrifice agent, cationic polymer are limited to the adaptability of shale mechanism sandstone in architectural engineering, it is impossible to
Unification solves the problems, such as water-reducing rate and slump retaining, and contains admittedly or volume increase, and cost is significantly improved.Inventor project team early stage finds
A kind of multi-hydroxy complex and polymer acted on based on clay flocculating is glued to Hunan, Guizhou province nearly 20% clay content
Native mineral (based on calcite, dolomite and Anhydrite) have obvious inhibitory action, and consumption is less, but Chongqing, Hebei etc. its
His region action effect needs this multi-hydroxy complex and polymer volume to show certain effect compared with Gao Shicai.
CN 105542091A disclose a kind of slow release cation have anti-mud effect polycarboxylate high performance water-reducing agent and
Its preparation method.The present invention with unsaturated carboxylic acid, polyether macromonomer, cation unsaturated monomer, unsaturated esters, cross-linking agent,
Chain-transferring agent, oxidant and reducing agent are raw material, at normal temperatures, without thermal source the anti-mud polycarboxylic acids of slow release cationic are successfully synthesized
High-performance water reducing agent.Long-chain esters cross-linking agent and cation unsaturated monomer are introduced in molecular structure, the polycarboxylic acids diminishing is made
Agent has good slow release and anti-mud effect.
The A of CN 105271885 disclose a kind of anti-mud collapse protective poly-carboxylic acid high-performance water reducing agent and preparation method thereof, diminishing
Agent includes isopentene group polyoxyethylene ether, initiator, A liquid and B liquid；Wherein, A liquid is by acrylic acid, 2-(Acryloyloxy)ethanol, acrylic acid
Hydroxypropyl acrylate, methylpropene sodium sulfonate, 2- acrylamide-2-methylpro panesulfonic acids, vinyl acetate, VTES
With water composition；B liquid includes chain-transferring agent, reducing agent and water.
The A of CN 105236806 disclose a kind of phosphate modified polycarboxylic acid water reducer with high-adaptability and its preparation
Method, the water reducer is made up of following raw materials：Isopentenol polyoxyethylene ether, hydrogen peroxide, acrylic acid, unsaturated mono phosphoric acid ester
Body, deionized water, reducing agent, chain-transferring agent；Chain-transferring agent is the one kind in mercaptoethanol, TGA, mercaptopropionic acid.Insatiable hunger
It is made up of 2- phosphate -1,2,4- butane tricarboxylates, p-methyl benzenesulfonic acid and hydroquinone with phosphorus acid monomer.
The content of the invention
The technical problem to be solved is to provide a kind of anti-chamotte mould polycarboxylic acids diminishing of single bisalkyl phosphate side chain
Masterbatch, is adapted to the higher situation of sandstone ground material CLAY MINERALS AND THEIR SIGNIFICANCE content.
The present invention increases as far as possible polycarboxylic acids molecular backbone length, to be unfavorable in slight extent in hydrated alkali solution
Trail as standard, to buffer the initial adsorption amount of polycarboxylate water-reducer molecule, the introducing of single bisalkyl phosphate short-chain branch, with
Polyether macromonomer long-chain branch is interlaced, increases the adaptability of water reducer；Additionally, the initial anchoring ability of list bisalkyl phosphate is strong
In carboxylate radical, sulfonate radical, sulfate radical, nitrate anion, and alcohol acid phosphate and hydroxy-acid group are hydrolyzed in alkaline solution, increase concrete
Workability and guarantor are collapsed effect.
A kind of anti-chamotte mould polycarboxylate water-reducer masterbatch of single bisalkyl phosphate side chain, is polymerized by following each components, former
Material gross mass is 1000 parts, and each component includes：
Polyether macromonomer：350～360；
Acrylic acid：32.0～38.0；
Single bisalkyl phosphate：2.0～6.0；
Phosphate chain-transferring agent：1.0～5.0；
TGA：0.5～1.0；
Hydrogen peroxide：3.0～6.0；
Vc：0.5～0.8；
Liquid caustic soda：7～15；
Water：Remaining；
The polyether macromonomer is methyl allyl polyoxyethylene ether, isopentenol polyoxyethylene ether, isobutene alcohol polyoxy
One or more compositions of vinyl Ether；The polyether macromonomer is preferably the isopentenol polyoxyethylene ether of 3500 molecular weight；
Described hydrogen peroxide is industrial grade hydrogen peroxide that mass percent is 27.5%；
Described liquid caustic soda is technical grade NaOH solution that mass percent is 30～32%.
Described phosphate chain-transferring agent is in sodium hypophosphite, hydrogen phosphite disodium, sodium dihydrogen phosphate, sodium tripolyphosphate
One or more compositions；Described phosphate chain-transferring agent be preferably sodium hypophosphite, hydrogen phosphite disodium, in one or two
Composition；
Described single bisalkyl phosphate is the mixture of monoalkyl phosphoric acid esters and bisalkyl phosphate.
Described single bisalkyl phosphate is monoalkyl phosphoric acid esters ROPO (OH)2With bisalkyl phosphate (RO)2PO's (OH)
Mixture, wherein R are one of having structure：
Described single bisalkyl phosphate is preferably monoalkyl phosphoric acid esters ROPO (OH)2With bisalkyl phosphate (RO)2PO
(OH) mass ratio is 2：1 compositionss；
R molecular structural formulas are preferably one of having structure：
The synthetic method of the anti-chamotte mould polycarboxylate water-reducer masterbatch of single bisalkyl phosphate side chain of the present invention, process is as follows：
Polyether macromonomer is placed in reaction vessel, is persistently stirred, until agitating solution is without obvious bulk or sheet material；
After adding dissolving completely in polyether macromonomer solution hydrogen peroxide, again property add phosphate chain-transferring agent and
The acrylic acid of 1/3rd amounts；Initiator and minor comonomer solution are sequentially added in 10min, described initiator is TGA
With the water solution mixture of Vc, described minor comonomer solution is that 2/3rds amount acrylic acid are water-soluble with single bisalkyl phosphate
Liquid；Minor comonomer solution time for adding is 1.5～2.5h, and initiator is lagged behind and dripped after minor comonomer 10～20min of solution；
Do not open cooling water circulation, be placed in reactor 1～2h of reaction automatically, then Temperature fall to 30 DEG C, add liquid caustic soda,
And moisturizing, stir.
The invention has the beneficial effects as follows：
1., slightly to limit range of extension of the diminishing agent molecule in strong adsorbate hydrated environment, polycarboxylate water-reducer master is increased
Chain length, water reducer Molecular Adsorption amount is limited；And sour ether ratio and high side chain density design theory in use, molecular dimension becomes big,
Initial adsorption amount of the synchronous auxiliary water reducer molecular backbone length constraint diminishing agent molecule under strong adsorbate hydrated environment.
2. single alkyl phosphonic acid is introduced except the isopentenol polyoxyethylene ether using 3500 molecular weight is as long-chain branch in side chain
Ester ROPO (OH)2With bisalkyl phosphate (RO)2Used as short-chain branch, long short-chain branch is interspersed PO (OH), cooperates with peptizaiton,
Water reducer adaptability is good；Phosphate anchoring ability is better than sulfonic group, sulfate radical, nitrate anion, so that water reducer absorption dispersion energy
Power is not suppressed by salt.
Specific embodiment
Below by example, the present invention will be further elaborated, and the description below is not right only for explaining the present invention
Content is defined.
Embodiment 1
A kind of anti-chamotte mould polycarboxylate water-reducer masterbatch of single bisalkyl phosphate side chain, the water reducer is polymerized by following each components
Form, raw material gross mass is 1000, and each component and technological parameter are as follows：
Bed material：The methyl allyl polyoxyethylene ether of 2400 molecular weight：358, water：220；
Hydrogen peroxide solution：27.5% industrial grade hydrogen peroxide：3.5, water：10；
After hydrogen peroxide is added, the acrylic acid of disposable addition sodium hypophosphite and 1/3rd amounts；
Sodium hypophosphite：3.0, acrylic acid (is first thrown)：11.0
After disposably finishing the acrylic acid of above-mentioned phosphate chain-transferring agent and 1/3rd amounts, sequentially add in 10min and draw
Send out agent, minor comonomer solution；
Initiator：TGA：0.8, Vc：0.75, water：120；
Minor comonomer solution：Acrylic acid (Deca)：22,2-(Acryloyloxy)ethanol base phosphate ester：1, di(2-ethylhexyl)phosphate (acrylic acid hydroxyl second
Base) ester：1.5, water：50；
Initiator time for adding：3.0h；
Minor comonomer solution time for adding 2.5h；
Temperature retention time：2h；
Liquid caustic soda：8；
Moisturizing：190.45.
Embodiment 2
A kind of anti-chamotte mould polycarboxylate water-reducer masterbatch of single bisalkyl phosphate side chain, the water reducer is polymerized by following each components
Form, raw material gross mass is 1000, and each component and technological parameter are as follows：
Bed material：The isobutene alcohol polyoxyethylene ether of 3000 molecular weight：355, water：220；
Hydrogen peroxide solution：27.5% industrial grade hydrogen peroxide：4.5, water：10；
After hydrogen peroxide is added, the acrylic acid of disposable addition sodium hypophosphite and 1/3rd amounts；
Hydrogen phosphite disodium：1.5, acrylic acid (is first thrown)：12.0；
After disposably finishing the acrylic acid of above-mentioned phosphate chain-transferring agent and 1/3rd amounts, sequentially add in 10min and draw
Send out agent, minor comonomer solution；
Initiator：TGA：1.0, Vc：0.68, water：120；
Minor comonomer solution：Acrylic acid (Deca)：24, hydroxyethyl methylacrylate base phosphate ester：2.0, di(2-ethylhexyl)phosphate (methyl-prop
Olefin(e) acid hydroxypropyl) ester：2.0, water：50；
Initiator time for adding：2.5h；
Minor comonomer solution time for adding 2.0h；
Temperature retention time：1.5h；
Liquid caustic soda：10；
Moisturizing：187.32.
Embodiment 3
A kind of anti-chamotte mould polycarboxylate water-reducer masterbatch of single bisalkyl phosphate side chain, the water reducer is polymerized by following each components
Form, raw material gross mass is 1000, and each component and technological parameter are as follows：
Bed material：The isopentenol polyoxyethylene ether of 3500 molecular weight：352, water：220；
Hydrogen peroxide solution：27.5% industrial grade hydrogen peroxide：4.5, water：10；
After hydrogen peroxide is added, the acrylic acid of disposable addition sodium hypophosphite and 1/3rd amounts；
Sodium hypophosphite：3.5, sodium dihydrogen phosphate：1.5, acrylic acid (is first thrown)：12.5；
After disposably finishing the acrylic acid of above-mentioned phosphate chain-transferring agent and 1/3rd amounts, sequentially add in 10min and draw
Send out agent, minor comonomer solution；
Initiator：TGA：0.65, Vc：0.57, water：120；
Minor comonomer solution：Acrylic acid (Deca)：25, Hydroxypropyl methacrylate base phosphate ester：3.0, di(2-ethylhexyl)phosphate (methyl-prop
Olefin(e) acid ethoxy) ester：1.5, water：50；
Initiator time for adding：2.0h；
Minor comonomer solution time for adding 1.5h；
Temperature retention time：2.0h；
Liquid caustic soda：13.5；
Moisturizing：181.78.
Anti- chamotte mould polycarboxylate water-reducer of the above-described embodiment using the chain modified preparation of single bisalkyl phosphate is tested respectively
The slump/expansion during concrete initial slump/divergence and Jing under masterbatch and common polycarboxylate superplasticizer mother liquor comparable sodium
The latitude of emulsion.Experiment cement used is the ordinary portland cement of Yadong 42.5, and clay content is 8.5% in sandstone, with reference to GB/8076-2008《Coagulation
Native additive》Testing standard.
Different water reducers affect on concrete flowability
According to above-mentioned concrete is initial and mobility compares during Jing, the anti-chamotte mould of the chain modified preparation of single bisalkyl phosphate
The initial fluidity of polycarboxylate water-reducer masterbatch embodiment 1,2,3 is slightly not good enough compared with ordinary water-reducing agent mother solution, but its encapsulation compared with
Good, index is embodied in common smaller in the slump, but divergence is bigger, and it is that ordinary water-reducing agent is initial a little to trace it to its cause
Isolation bleeding；The guarantor of embodiment 1,2,3 collapses more notable, anti-mud excellent performance；It is single bisalkyl phosphate anchor to trace it to its cause
Gu discharge carboxylic acid and alcohol after ability and hydrolysis.
Claims (4)
1. a kind of anti-chamotte mould polycarboxylate water-reducer masterbatch of single bisalkyl phosphate side chain, is polymerized by following each components, raw material
Gross mass is 1000 parts, and each component includes：
Polyether macromonomer：350～360；
Acrylic acid：32.0～38.0；
Single bisalkyl phosphate：2.0～6.0；
Phosphate chain-transferring agent：1.0～5.0；
TGA：0.5～1.0；
Hydrogen peroxide：3.0～6.0；
Vc：0.5～0.8；
Liquid caustic soda：7～15；
Water：Remaining；
The polyether macromonomer is methyl allyl polyoxyethylene ether, isopentenol polyoxyethylene ether, isobutene alcohol Polyethylene oxide
One or more compositions of ether；
Described single bisalkyl phosphate is the mixture of monoalkyl phosphoric acid esters and bisalkyl phosphate；
Described hydrogen peroxide is industrial grade hydrogen peroxide that mass percent is 27.5%；
Described liquid caustic soda is technical grade NaOH solution that mass percent is 30～32%.
2. anti-chamotte mould polycarboxylate water-reducer masterbatch according to claim 1, it is characterised in that described phosphate chain tra nsfer
Agent is one or more compositions in sodium hypophosphite, hydrogen phosphite disodium, sodium dihydrogen phosphate, sodium tripolyphosphate.
3. anti-chamotte mould polycarboxylate water-reducer masterbatch according to claim 1, it is characterised in that described single double alkyl phosphoric acids
Ester is monoalkyl phosphoric acid esters ROPO (OH)2With bisalkyl phosphate (RO)2The mixture of PO (OH), wherein R is following structural：
4. the synthetic method of the anti-chamotte mould polycarboxylate water-reducer masterbatch described in claim 1, it is characterised in that：
Polyether macromonomer is placed in reaction vessel, is persistently stirred, until agitating solution is without obvious bulk or sheet material；
Hydrogen peroxide is added after dissolving in completely polyether macromonomer solution, again property adds phosphate chain-transferring agent and three points
One of amount acrylic acid；Initiator and minor comonomer solution are sequentially added in 10min, described initiator is TGA and dimension
The water solution mixture of C, described minor comonomer solution is the aqueous solution of 2/3rds amount acrylic acid and single bisalkyl phosphate；It is little
Monomer solution time for adding is 1.5～2.5h, and initiator is lagged behind and dripped after minor comonomer 10～20min of solution；
Do not open cooling water circulation, be placed in reactor 1～2h of reaction automatically, then Temperature fall to 30 DEG C, add liquid caustic soda, and mend
Water, stirs.
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Cited By (8)
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|---|---|---|---|---|
| CN107698716A (en) * | 2017-07-06 | 2018-02-16 | 徐州巨龙新材料科技有限公司 | A kind of polycarboxylate water-reducer and preparation method thereof |
| CN107698715A (en) * | 2017-07-06 | 2018-02-16 | 徐州巨龙新材料科技有限公司 | A kind of anti-mud polycarboxylate water-reducer |
| CN107698717A (en) * | 2017-07-06 | 2018-02-16 | 徐州巨龙新材料科技有限公司 | A kind of preparation method of anti-mud polycarboxylate water-reducer |
| CN107987225A (en) * | 2017-11-30 | 2018-05-04 | 湖北工业大学 | A kind of anti-negative electricity adsorbate phosphate polycarboxylate water-reducer and low temperature preparation method |
| CN108218282A (en) * | 2017-12-28 | 2018-06-29 | 科之杰新材料集团有限公司 | A kind of preparation method of anti-mud viscosity reduction type polycarboxylic acids plasticiser |
| CN109293849A (en) * | 2018-09-27 | 2019-02-01 | 武汉奥克化学有限公司 | A kind of anti-chamotte mould polycarboxylate water-reducer and preparation method thereof |
| CN111303405A (en) * | 2018-12-11 | 2020-06-19 | 江苏苏博特新材料股份有限公司 | Phosphate water reducing agent suitable for high-temperature construction environment in summer and preparation method thereof |
| CN112778467A (en) * | 2021-01-13 | 2021-05-11 | 科之杰新材料集团(贵州)有限公司 | Polycarboxylate superplasticizer for concrete and preparation method thereof |
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Cited By (10)
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| CN107698716A (en) * | 2017-07-06 | 2018-02-16 | 徐州巨龙新材料科技有限公司 | A kind of polycarboxylate water-reducer and preparation method thereof |
| CN107698715A (en) * | 2017-07-06 | 2018-02-16 | 徐州巨龙新材料科技有限公司 | A kind of anti-mud polycarboxylate water-reducer |
| CN107698717A (en) * | 2017-07-06 | 2018-02-16 | 徐州巨龙新材料科技有限公司 | A kind of preparation method of anti-mud polycarboxylate water-reducer |
| CN107987225A (en) * | 2017-11-30 | 2018-05-04 | 湖北工业大学 | A kind of anti-negative electricity adsorbate phosphate polycarboxylate water-reducer and low temperature preparation method |
| CN108218282A (en) * | 2017-12-28 | 2018-06-29 | 科之杰新材料集团有限公司 | A kind of preparation method of anti-mud viscosity reduction type polycarboxylic acids plasticiser |
| CN108218282B (en) * | 2017-12-28 | 2020-03-06 | 科之杰新材料集团有限公司 | Preparation method of anti-mud viscosity-reducing polycarboxylic acid plasticizer |
| CN109293849A (en) * | 2018-09-27 | 2019-02-01 | 武汉奥克化学有限公司 | A kind of anti-chamotte mould polycarboxylate water-reducer and preparation method thereof |
| CN111303405A (en) * | 2018-12-11 | 2020-06-19 | 江苏苏博特新材料股份有限公司 | Phosphate water reducing agent suitable for high-temperature construction environment in summer and preparation method thereof |
| CN111303405B (en) * | 2018-12-11 | 2022-07-08 | 江苏苏博特新材料股份有限公司 | Phosphate water reducing agent suitable for high-temperature construction environment in summer and preparation method thereof |
| CN112778467A (en) * | 2021-01-13 | 2021-05-11 | 科之杰新材料集团(贵州)有限公司 | Polycarboxylate superplasticizer for concrete and preparation method thereof |
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Application publication date: 20170426 |