CN106699985A - Super-long super slow release type polycarboxylic acid slump-retaining agent master batch - Google Patents
Super-long super slow release type polycarboxylic acid slump-retaining agent master batch Download PDFInfo
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- CN106699985A CN106699985A CN201611003276.0A CN201611003276A CN106699985A CN 106699985 A CN106699985 A CN 106699985A CN 201611003276 A CN201611003276 A CN 201611003276A CN 106699985 A CN106699985 A CN 106699985A
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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
- C04B24/26—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
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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
Abstract
The invention discloses a super-long super slow release type polycarboxylic acid slump-retaining agent master batch suitable for projects such as hydraulic tunnels, railway tunnels, metros and underground oil and gas delivery adopting concrete having the capability of retaining slump for 4-6 hours under the conditions of hot weather and long distance. Limited by 40% of the mass percent of mother liquid, the total mass of synthesized raw materials is 1000 parts, the usage amount proportion is that the usage amount of polyether macromonomer accounts for 325-335 parts, the usage amount of unsaturated carboxylic acid micro-monomer accounts for 10.0-18.0 parts, the usage amount of acrylic hydroxyalkanoate accounts for 35.0-45.0 parts, the usage amount of crosslinking monomer accounts for 5.0-10.0 parts, the usage amount of sulfonic acid type chain transfer agent accounts for 2.0-5.0 parts, the usage amount of hydrogen peroxide accounts for 2.0-3.5 parts, the usage amount of vitamin C accounts for 0.60-0.90 part, the usage amount of caustic soda liquid accounts for 7-10 parts, and the balance is water. The polycarboxylic acid slump-retaining agent is moderate in molecular weight, can be independently used or compounded with other polycarboxylic acid water reducing agents for usage, can remarkably improve the indexes such as slump-retaining property, cohesiveness and flowing retention ability of newly mixed concrete in 6 hours.
Description
Technical field
The present invention relates to a kind of technical field of cement-based gelling material additive, and in particular to a kind of super sustained release of overlength
Type polycarboxylic acid slump retaining agent masterbatch, the excessive hydraulic tunnel of concrete slump loss, iron can be caused suitable for prolonged transport
Road tunnel, subway, the defeated reservoir hydrocarbon engineering in underground.
Background technology
With the raising of the fast-developing and building level of China's economy, the slump-loss problem of fresh concrete is always
It is the problem for perplexing engineering construction, particularly prolonged transport can cause concrete slump loss excessive, influence concrete
Workability.Excavation and construction especially as Super-long tunnel, engineering circles are to tunnel the wet shotcreting slump and mobility
Holding capacity requirement more and more higher.Hydraulic tunnel, railway tunnel, subway, the defeated reservoir hydrocarbon engineering in underground will have a large amount of tunnels need
Excavate, length is more than the hydraulic tunnel of 20km, railway tunnel, subway, underground is defeated, reservoir hydrocarbon engineering will be more and more, tunnel
Communications and transportation complex circuit in hole, surface gathered water, hollow are serious, condition of road surface extreme difference, and average speed is less than 10km/h.Additionally,
During long-distance transportation along with extreme scorching temperature weather appearance and wet shotcreting because sand coarse aggregate ratio it is high caused by it is sticky, exacerbate
The loss of the wet shotcreting slump and mobility, this is accomplished by concrete and is collapsed ability with more excellent guarantor.Therefore, coagulation
Soil must possess the slump holding capacity of 4 ~ 6h, certainly will otherwise influence being smoothed out for construction, seriously then influence concrete works
Quality.
It is to compound to change by the retarder such as polycarboxylic acids dehydragent and Portugal's sodium and slump retaining agent that the country solves to protect the method collapsed
The guarantor of kind water reducer is collapsed ability.Retarder can not be effectively improved the slump holding capacity of poly carboxylic acid series water reducer, be easily caused
Setting time excessively extends and reduces early strength；Excellent slump retaining agent, the coagulation under tropical conditions are showed for ordinary skill
The guarantor of soil is still difficult to more than 2h time of collapsing.To find out its cause, existing retarder or slump retaining agent cannot disposably show in concrete
The consumption of lifting slow-release type polycarboxylate water reducer is write, once consumption is too high, it is easy to and cause concrete original operating state to occur
Isolation, bleeding, or because the strong slow releasing function of a certain particular point in time causes isolation, bleeding occur in concrete application, so that
So that concrete state is uncontrollable to be difficult to construct.Secondly, wet shotcreting seems that viscosity is higher because itself sand coarse aggregate ratio is high, and viscous
Property it is bigger loss it is bigger.
The A of patent CN 104230203 disclose a kind of super sustained-release polycarboxylic slump retaining agent and preparation method thereof, the polycarboxylic acids
Slump retaining agent is by monomer A：Modified APEO (TPEG), monomer B：Maleic anhydride or PEGMa polyethylene glycol maleate class, monomer C：
Acrylic acid, monomer D：Acrylic acid hydroxy alkyl ester or vinyl acetate, initiator, chain-transferring agent, water, by free-radical polymerized anti-
Should, plus in alkaline solution and be prepared from.
The A of patent CN 103724560 disclose a kind of superpower slump retaining agent, are made up of following raw materials：A. prenol polyoxy
The mixture of vinethene, b. acrylic acid or methacrylic acid or both, c. ethyl acrylates or propyl acrylate or
Both mixture, d. allyl methacrylates, e. ammonium persulfates or potassium peroxydisulfate, f. methylpropene sodium sulfonates；This hair
Not only initial water-reducing rate is not affected by influence to bright slump retaining agent, and concrete slump rheological parameters' change with time amount is obviously improved, 3h interior energies
Enough ensure without slump-loss.
The A of patent CN 104292396 provide a kind of preparation method of the polycarboxylic acid slump retaining agent of dual regulation and control, preparation process
It is as follows：Monomer A and deionized water are added in bed material, reaction temperature is warming up to, add oxidant to stir, at the same be added dropwise by
The first solution of monomer B, monomer C, monomer D and deionized water composition and the second being made up of chain-transferring agent, reducing agent and deionized water
Solution, after reaction certain hour, is adjusted to 6.5 ~ 7 the pH value of above-mentioned copolymerization product with liquid caustic soda.
6h protects the concrete tailored version poly carboxylic acid series water reducer that collapses under a kind of tropical conditions of present invention exploitation, and the spacetabs type gathers
Carboxylic acid high efficiency water reducing agent can be used alone or with other poly carboxylic acid series water reducer compound uses, fresh concrete can be substantially improved
Workability, cohesiveness, slump retaining etc., have no adverse effects to properties of hardened concrete, and the use that can meet ready-mixed concrete will
Ask.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of super sustained-release polycarboxylic slump retaining agent masterbatch of overlength.
The present invention can occur hydrolysis based on different Esters in cement alkaline environment, and increasingly generate carboxylic acid group
Group, the speed of ester-type hydrolysis with and esters be connected electron donating group, electron withdraw group and steric hindrance it is relevant.From molecular structure
Set about, introducing has slow-release function group, substitute the carboxyl of part acrylic acid containing ester group, sulfonic alkenyl monomer with part
Group's synthesis has sustained-release polycarboxylic high efficiency water reducing agent, using the hydrolysis point difference of different ester groups and senior ester, cross-linked structure water
The characteristics of solving delayed, while controlling ratio of the anion of sulfonic acid, carboxylic acid in water reducer product, makes the water-reducing rate of product and guarantor
Ability of collapsing is matched rationally in a long time, to reach the purpose that overlength surpasses sustained release.
The super sustained release polycarboxylic acid slump retaining agent of overlength of the invention, is a kind of dispersion collapsed with plasticising function with superpower guarantor,
Time and the function of slump protection of concrete opening can greatly be extended.The super slow releasing function mechanism of overlength is not to go to adjust by slow setting composition
Section concrete slump, this polymer combines " time release " technology and collapses the time extending guarantor, do not influence setting time with
Strength development, later strength is higher.The MOLECULE DESIGN for progressively hydrolyzing imparts the slump-retaining energy of concrete overlength, without
Extension setting time or influence strength development.Super guarantor collapse technology basis be by specially designed polymer, can be used for carry
The slump for ultra-long time keeps, without extension setting time or influence strength development.
A kind of super sustained-release polycarboxylic slump retaining agent masterbatch of overlength, is polymerized by following each components, and gross mass is 1000 parts,
Comprise the following steps that：
1) 325 ~ 335 parts of polyether macromonomers and 200 ~ 250 parts of water are added in reactor, lasting stirring, until solution is without bright
Aobvious block or sheet material；
2) control temperature in the kettle disposably puts into 2.0 ~ 3.5 parts of hydrogen peroxide at 5 ~ 25 DEG C；Add in 10min, drop is started successively
Plus initiator, minor comonomer solution, initiator time for adding is 0.5 hour more than minor comonomer solution time for adding；Initiator by 2.0 ~
5.0 parts of sulphonic acids chain-transferring agents, 0.60 ~ 0.90 part of Vc and 100 ~ 120 parts of water compositions；Minor comonomer solution by 10.0 ~ 18.0 parts not
Saturated carboxylic acid class minor comonomer, 35.0 ~ 45.0 parts of acrylic acid hydroxy alkyl esters, 5.0 ~ 10.0 parts of cross-linking monomers and 60 ~ 90 parts of water compositions；
3) after completion of dropwise addition, 1 ~ 2h is cured, when question response solution temperature is less than 30 DEG C, adds 7 ~ 10 parts of liquid caustic soda, moisturizing stirring is equal
10 ~ 15h is stood after even, the liquid caustic soda is the technical grade NaOH of mass ratio 30 ~ 32%.
The polyether macromonomer is methyl allyl polyoxyethylene ether, isopentenol polyoxyethylene ether, isobutene alcohol polyoxy
One or more of vinethene；It is 1 that the polyether macromonomer is preferably mass ratio：The isobutene alcohol polyoxy of 2 3000 molecular weight
The composition of the isopentenol polyoxyethylene ether of vinethene and 2400 molecular weight.
The hydrogen peroxide is that mass percent is 27.5% industrial grade hydrogen peroxide.
The sulphonic acids chain-transferring agent is sodium vinyl sulfonate, acrylic sodium sulfonate, methylpropene sodium sulfonate, styrene sulphur
One or more compositions of sour sodium, 2- acrylamide-2-methyl propane sulfonics；The sulphonic acids chain-transferring agent is preferably reactivity
Larger sulphonic acids chain-transferring agent, i.e. sodium vinyl sulfonate, acrylic sodium sulfonate, one or more groups of methylpropene sodium sulfonate
Into.
The unsaturated carboxylic acid class minor comonomer includes unsaturated monocarboxylic acid minor comonomer, i.e. acrylic acid；Undersaturated binary
One or more compositions of carboxylic acid minor comonomer, i.e. itaconic acid, fumaric acid, maleic acid；Unsaturated tricarboxylic acid minor comonomer, the i.e. rhizome of Chinese monkshood
Acid；The unsaturated carboxylic acid class minor comonomer is preferably unsaturated dicarboxylic acid class minor comonomer and the unsaturated tricarboxylic acid small list of class
One or more compositions of body, i.e. itaconic acid, fumaric acid, maleic acid, aconitic acid.
The acrylic acid hydroxy alkyl ester is one or two compositions of hydroxy-ethyl acrylate and hydroxypropyl acrylate；Described
Acrylic acid hydroxy alkyl ester is preferably the composition of hydroxy-ethyl acrylate and hydroxypropyl acrylate；Described acrylic acid hydroxy alkyl ester is excellent
It is 4 to elect mass ratio as：6 hydroxy-ethyl acrylate and the composition of hydroxypropyl acrylate.
The cross-linking monomer be polyethylene glycol acrylate, methoxy polyethylene glycol acrylate, allyl polyglycol,
One or more compositions of the double maleic mono-esters of polyethylene glycol；Described cross-linking monomer is preferably the larger friendship of space steric effect
One or two compositions of receipts or other documents in duplicate body, i.e. methoxy polyethylene glycol acrylate, the double maleic mono-esters of polyethylene glycol.
The minor comonomer solution time for adding is 2.5 ~ 4.5 h, preferably 3.5 h.
The beneficial effects of the invention are as follows：
1. the sulfydryl class chain-transferring agent that general polycarboxylic acid slump retaining agent is used, the super sustained release polycarboxylic acid slump retaining agent system of overlength are different from
In single use sulphonic acids chain-transferring agent, its object is in anchoring group introduce q.s sulfonic acid group；-COOH-Tool
Back-up dissipates, slow setting effect ,-SO3 -Electronegativity is compared with-COOH-Stronger, anchoring ability is stronger, and without slow setting effect, prevents overlength super slow
Release-the COOH of excess in polycarboxylic acid slump retaining agent component-The side effect for causing cementitious material system Slow setting time long.
2. under equal anchoring adsorption capacity, unsaturated two/tricarboxylic acid minor comonomer quality compares insatiable hunger in synthetic ratio design
Quality with monocarboxylic acid minor comonomer is small, therefore enough component design acrylic acid hydroxy alkyl esters and crosslinking list can be designed in synthetic ratio
The consumption of body, using different ester groups hydrolysis point difference and the delayed senior ester hydrolysis of cross-linked structure the characteristics of, matched design propylene
Sour hydroxy alkyl ester and cross-linking monomer, with the alkaline environment that hydrated cementitious are provided can in 6h progressively hydrolysis into parents such as carboxyls
Water base group is slowly adsorbed, and plays its slow release peptizaiton.
Specific embodiment
Embodiment 1：
A kind of super sustained-release polycarboxylic slump retaining agent masterbatch of overlength, it is characterised in that：The slump retaining agent is polymerized by following each components,
Raw material gross mass is 1000 parts, and each component and technological parameter are as follows：
Bed material：The methyl allyl polyoxyethylene ether of 2400 molecular weight：327, water：220；
Hydrogen peroxide solution：27.5% industrial grade hydrogen peroxide：3.0, water：10；
After hydrogen peroxide addition initiator, minor comonomer solution are sequentially added in 10min；
Initiator：Methylpropene sodium sulfonate：3.7, Vc：0.70, water：110；
Minor comonomer solution：Itaconic acid：15.5, hydroxy-ethyl acrylate：42.8, methoxy polyethylene glycol acrylate：5.5, water：
65；
Initiator time for adding：3.5h；
Minor comonomer solution time for adding 3.0h；
Soaking time：1.5h；
Liquid caustic soda：8；
Moisturizing：188.8.
10 ~ 15h is stood after stirring.
Embodiment 2：
Bed material：The isopentenol polyoxyethylene ether of 2400 molecular weight：332, water：235；
Hydrogen peroxide solution：27.5% industrial grade hydrogen peroxide：2.5, water：10；
After hydrogen peroxide addition initiator, minor comonomer solution are sequentially added in 10min；
Initiator：Sodium vinyl sulfonate：4.5, Vc：0.75, water：110；
Minor comonomer solution：Fumaric acid：8.5, aconitic acid：2.5, hydroxy-ethyl acrylate：15.8, hydroxypropyl acrylate：23.7, poly- second
The double maleic mono-esters of glycol：6.0, water：70；
Initiator time for adding：3.5h；
Minor comonomer solution time for adding 3.0h；
Soaking time：2.0h；
Liquid caustic soda：9；
Moisturizing：169.75.
10 ~ 15h is stood after stirring.
Embodiment 3：
Bed material：The isobutene alcohol APEO of 3000 molecular weight：The isopentenol polyoxyethylene ether of 109,2400 molecular weight：
218, water：250；
Hydrogen peroxide solution：27.5% industrial grade hydrogen peroxide：3.5, water：10；
After hydrogen peroxide addition initiator, minor comonomer solution are sequentially added in 10min；
Initiator：Acrylic sodium sulfonate：4.9, Vc：0.85, water：118；
Minor comonomer solution：Maleic acid：11.5, hydroxy-ethyl acrylate：16.2, hydroxypropyl acrylate：24.3, polyethylene glycol span comes
Acid monoester：8.5, water：80；
Initiator time for adding：4.0h；
Minor comonomer solution time for adding 3.5h；
Soaking time：2.0h；
Liquid caustic soda：7.5；
Moisturizing：137.75.
10 ~ 15h is stood after stirring.
In addition to the implementation, the present invention can also have other embodiment.What all use equivalents or equivalent transformation were formed
Technical scheme, all falls within the protection domain of application claims.
The test super sustained-release polycarboxylic slump retaining agent masterbatch of examples detailed above overlength is same with common polycarboxylic acid slump retaining agent mother liquor respectively
Fluidity in cement paste initial flow degree and 6h under isoconcentration.Experiment cement used is new 42.5 ordinary portland cement of China, reference
GB/8076-2008《Concrete admixture》Testing standard.
Different slump retaining agents influence on flowing degree of net paste of cement
| Slump retaining agent species | Initial flow degree mm | 1h fluidities mm | 2h fluidities mm | 3h fluidities mm | 4h fluidities mm | 5h fluidities mm | 6h fluidities mm |
| Common slump retaining agent | - | 260 | 250 | 170 | - | - | - |
| Embodiment 1 | - | 210 | 260 | 270 | 260 | 240 | 180 |
| Embodiment 2 | - | 225 | 280 | 280 | 250 | 220 | 175 |
| Embodiment 3 | - | 200 | 245 | 260 | 275 | 270 | 220 |
According to it is above-mentioned initial and through when paste flowing degree compare, after common slump retaining agent 2h paste flowing degree trend downwards, 3h flowings
Degree starts to weaken, and 4h fluidities are determined not out；And the 1h flowings of the super sustained-release polycarboxylic slump retaining agent masterbatch example 1,2,3 of overlength
The smaller of more common slump retaining agent is spent, but 3h fluidities substantially achieve peak, and 4h or 5h fluidities start to weaken, during 6h
Still possesses certain fluidity.From the above mentioned, the super sustained-release polycarboxylic slump retaining agent 1h fluidities of overlength are smaller, and rate of release is slow
Slowly, the super sustained release polycarboxylic acid slump retaining agent design concept of overlength under hot weather and long distance long is met.
Claims (6)
1. the super sustained-release polycarboxylic slump retaining agent masterbatch of a kind of overlength, it is characterised in that be polymerized by following each components, gross mass
It is 1000 parts, comprises the following steps that：
1) 325 ~ 335 parts of polyether macromonomers and 200 ~ 250 parts of water are added in reactor, lasting stirring, until solution is without bright
Aobvious block or sheet material；
2) control temperature in the kettle disposably puts into 2.0 ~ 3.5 parts of hydrogen peroxide at 5 ~ 25 DEG C；Add in 10min, drop is started successively
Plus initiator, minor comonomer solution, initiator time for adding is 0.5 hour more than minor comonomer solution time for adding；Initiator by 2.0 ~
5.0 parts of sulphonic acids chain-transferring agents, 0.60 ~ 0.90 part of Vc and 100 ~ 120 parts of water compositions；Minor comonomer solution by 10.0 ~ 18.0 parts not
Saturated carboxylic acid class minor comonomer, 35.0 ~ 45.0 parts of acrylic acid hydroxy alkyl esters, 5.0 ~ 10.0 parts of cross-linking monomers and 60 ~ 90 parts of water compositions；
3) after completion of dropwise addition, 1 ~ 2h is cured, when question response solution temperature is less than 30 DEG C, adds 7 ~ 10 parts of liquid caustic soda, moisturizing stirring is equal
10 ~ 15h is stood after even, the liquid caustic soda is the technical grade NaOH of mass ratio 30 ~ 32%；
The polyether macromonomer is methyl allyl polyoxyethylene ether, isopentenol polyoxyethylene ether, isobutene alcohol polyoxyethylene
One or more of ether；The hydrogen peroxide is that mass percent is 27.5% industrial grade hydrogen peroxide.
2. the super sustained-release polycarboxylic slump retaining agent masterbatch of overlength according to claim 1, it is characterised in that the sulphonic acids chain
Transfer agent is sodium vinyl sulfonate, acrylic sodium sulfonate, methylpropene sodium sulfonate, SSS, 2- acrylamide -2- first
One or more compositions of base propane sulfonic acid.
3. the super sustained-release polycarboxylic slump retaining agent masterbatch of overlength according to claim 1, it is characterised in that the unsaturated carboxylic
Acids minor comonomer includes one or more compositions in acrylic acid, itaconic acid, fumaric acid, maleic acid, aconitic acid.
4. the super sustained-release polycarboxylic slump retaining agent masterbatch of overlength according to claim 1, it is characterised in that the acrylic acid hydroxyl
Arrcostab is one or two compositions of hydroxy-ethyl acrylate and hydroxypropyl acrylate.
5. the super sustained-release polycarboxylic slump retaining agent masterbatch of overlength according to claim 1, it is characterised in that the cross-linking monomer
It is polyethylene glycol acrylate, methoxy polyethylene glycol acrylate, allyl polyglycol, the double maleic mono-esters of polyethylene glycol
One or more composition.
6. the super sustained-release polycarboxylic slump retaining agent masterbatch of overlength according to claim 1, it is characterised in that the minor comonomer is molten
Liquid time for adding is 2.5 ~ 4.5 h.
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| CN107352838A (en) * | 2017-08-24 | 2017-11-17 | 重庆三圣实业股份有限公司 | A kind of super carboxylic acid slump retaining agent and its preparation and application |
| CN108129056A (en) * | 2018-01-11 | 2018-06-08 | 贵州天威建材科技有限责任公司 | A kind of special water-reducing agent of railway tunnel construction gunite concrete |
| CN109265622A (en) * | 2018-08-02 | 2019-01-25 | 四川恒泽建材有限公司 | A kind of no heat source high-performance controlled-release polycarboxylic acid water reducing agent and preparation method thereof |
| CN109970385A (en) * | 2019-04-23 | 2019-07-05 | 刘翠芬 | One kind is super to protect the concrete water-reducing agent that collapses |
| CN110590219A (en) * | 2019-09-12 | 2019-12-20 | 衡水积土科技有限公司 | Preparation method of concrete curing agent |
| CN110938176A (en) * | 2018-09-25 | 2020-03-31 | 中建材中岩科技有限公司 | Super-long slump loss resistant cement-based polycarboxylate superplasticizer mother liquor and application thereof |
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| CN114380957A (en) * | 2022-01-21 | 2022-04-22 | 太原市天鼎恒砼外加剂科技发展有限公司 | High-performance ultra-slow release slump retaining agent and preparation method thereof |
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