CN106800622A - A kind of slow release slump retaining polycarboxylate water reducer and preparation method thereof - Google Patents
A kind of slow release slump retaining polycarboxylate water reducer and preparation method thereof Download PDFInfo
- Publication number
- CN106800622A CN106800622A CN201710057876.3A CN201710057876A CN106800622A CN 106800622 A CN106800622 A CN 106800622A CN 201710057876 A CN201710057876 A CN 201710057876A CN 106800622 A CN106800622 A CN 106800622A
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- CN
- China
- Prior art keywords
- acid
- slow release
- preparation
- polycarboxylate water
- slump retaining
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Classifications
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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
- C04B24/24—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
- 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
- C04B2103/0045—Polymers chosen for their physico-chemical characteristics
- C04B2103/0059—Graft (co-)polymers
-
- 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 kind of slow release slump retaining polycarboxylate water reducer and preparation method thereof, by in water, unsaturated APEO, organic carboxyl acid, oxidant input reactor, stirring is extremely dissolved, after input oxidant, it is heated to 30 60 DEG C, the A liquid and B liquid of oneself configuration is added dropwise simultaneously thereto, A drops add 34 hours, and B drops add 3.5 5h, after being incubated 1 2h, plus it is 6 one 7 that alkali lye is neutralized to pH, moisturizing to solid content is 40 45%, obtains collapse protective poly-carboxylic acid water reducing agent.The invention has the advantages that：Basic hydrolysis group is introduced on polycarboxylic acids high polymer main chain, after concrete mixing, cement hydration process is constantly hydrolyzed in alkalescence, the basic hydrolysis group on polycarboxylic acids macromolecular chain, discharges carboxyl, the water-reducing property of polycarboxylic acids molecule is constantly discharged therewith.Overcome existing polycarboxylate water-reducer and the incompatible problem for causing slump-loss big of cement.
Description
Technical field
The present invention relates to technical field of concrete additives, and in particular to a kind of slow release slump retaining polycarboxylate water reducer and
Its preparation method.This water reducer can significantly improve concrete slump retaining performance on the premise of retarder is not compounded.
Background technology
Polycarboxylate water-reducer is third generation high performance concrete admixture, with volume is low, on good dispersion, molecular structure
The advantages of free degree is big, oneself achieves good effect through being widely used in various concrete workses.But in practical application mistake
Cheng Zhong, there is also some problems, the problems such as such as slump-loss is too fast, adaptability is bad, amount of water is sensitive, to a certain extent
The application of polycarboxylate water-reducer is constrained, while also influenceing construction quality.
For the fast problem of concrete slump loss, previous patent discloses some improved methods:Such as adjust sour ether
Ratio, changes the length and density of hydrophilic side-chains in diminishing agent molecule, and lipid polymeric monomer and ethers polymeric monomer carry out copolymerization, lead to
Cross compounding and add retarder etc., but in current complex working condition, cement type more and in the case of the deterioration of sand material quality, problem is still
Cannot solve well.
There is presently no a kind of adaptability extensively, the collapse protective poly-carboxylic acid diminishing of strong adaptability, process is simple, excellent performance
Agent.
The content of the invention
It is existing to overcome it is an object of the invention to provide a kind of slow release slump retaining polycarboxylate water reducer and preparation method thereof
Polycarboxylate water-reducer and the incompatible problem for causing slump-loss big of cement.
To achieve the above object, the present invention provides following technical scheme：
A kind of preparation method of slow release slump retaining polycarboxylate water reducer, it is characterised in that：Comprise the following steps：
By in water, unsaturated APEO, organic carboxyl acid, oxidant input reactor, stirring is extremely dissolved, input oxidation
After agent, 30-60 DEG C is heated to, the A liquid and B liquid of oneself configuration is added dropwise simultaneously thereto, A drops add 3-4 hours, and B drops add 3.5-
5h, after insulation 1-2h, plus it is 6 one 7 that alkali lye is neutralized to pH, and moisturizing to solid content is 40-45%, obtains collapse protective poly-carboxylic acid diminishing
Agent；
Described A liquid is organic carboxyl acid, acrylic acid alkyl lipid monomer, acrylamide monomers and water；
Described B liquid is reproducibility catalyst, chain-transferring agent and water.
Preferably：Described unsaturated APEO is methylallyl alcohol APEO (HPEG), prenol gathers
It is any in oxygen vinethene (TPEG), methoxy polyoxyethylene ether metacrylic acid ester, methoxy polyoxyethylene ether acrylate
One or more.
Preferably：Described organic carboxyl acid is one kind in acrylic acid, methacrylic acid, maleic anhydride, fumaric acid, itaconic acid
Or it is various.
Preferably：Described acrylic acid first vinegar, ethyl acrylate, propyl acrylate, acrylic acid hydroxyl second fat, acrylic acid hydroxypropyl
One or more in ester.
Preferably：Described amide-type monomer is acrylamide, N-N DMAAs or 2- acrylamide -2- first
One or more in base propane sulfonic acid methyl propane sulfonic acid.
Preferably：Described oxidative initiator is one or more in hydrogen peroxide, over cure acid compounds；Described
Chain-transferring agent is one or two in coloured glaze base propionic acid or coloured glaze guanidine-acetic acid；Described reproducibility initiator is sodium formaldehyde sulfoxylate, vitamin C
Or one or more in sodium hydrogensulfite.
Preferably：The molecular weight of the unsaturated APEO is 1000-3000.
A kind of slow release slump retaining polycarboxylate water reducer, it is characterised in that：Including
Compared with prior art, the invention has the advantages that：
Basic hydrolysis group is introduced on polycarboxylic acids high polymer main chain, after concrete mixing, cement hydration process is in alkalescence,
Basic hydrolysis group on polycarboxylic acids macromolecular chain is constantly hydrolyzed, and discharges carboxyl, make polycarboxylic acids molecule water-reducing property constantly with
Release.Overcome existing polycarboxylate water-reducer and the incompatible problem for causing slump-loss big of cement.The sustained release of synthesis
Collapse protective poly-carboxylic acid water reducing agent has excellent slump-retaining, and different well adapting to property of cement, to second-rate
Well adapting to property of sand material.
Specific embodiment
Below in conjunction with the embodiment in the present invention, the technical scheme in the embodiment of the present invention is carried out clearly and completely
Description, it is clear that described embodiment is only a part of embodiment of the invention, rather than whole embodiments.Based on this hair
Embodiment in bright, the every other implementation that those of ordinary skill in the art are obtained under the premise of creative work is not made
Example, belongs to the scope of protection of the invention.
Embodiment 1
210g water, 200g methylallyl alcohols APEO (HPEG2400) are added in 1000m1 flask with three necks,round bottom,
8.0g acrylamides and 2.0g hydrogen peroxide are used as reaction bottom liquid.
Prepare solution A:15.0g acrylic acid, 1.5 grams of mercaptopropionic acids and 40g water are mixed and are put in dropping funel.
Prepare B solution:0.5 gram of Vc and 60g water are mixed and is put in dropping funel.
Stirring to monomer in flask is dissolved, and is warming up to 60 DEG C, and dropwise addition A liquid and B liquid are started simultaneously at immediately, and solution A 3.0 is small
When drip off simultaneously, B solution is dripped off for 3.5 hours, continues insulation reaction after 0.5 hour, adds 7.5 gram 32% of NaOH molten
Liquid, regulation solution ph is 6-7, and moisturizing obtains 40% collapse protective poly-carboxylic acid water reducing agent mother liquor.
Embodiment 2
210g water, 200g methylallyl alcohols APEO (HPEG2400) are added in 1000m1 flask with three necks,round bottom,
12g maleic anhydrides and 6.0gAMPS are used as reaction bottom liquid, 2.0g Ammonium Persulfate 98.5s and 1.0g hydrogen peroxide.
Prepare solution A：20g methyl acrylates, 2.0 grams of coloured glaze base propionic acid and 30g water are mixed and is put in dropping funel.
Prepare B solution：0.5 gram of sodium formaldehyde sulfoxylate and 60g water are mixed and is put in dropwise addition bottle.
Stirring to monomer in flask is dissolved, and is warming up to 40 DEG C, and dropwise addition A liquid and B liquid, A liquid 2.0 hours are started simultaneously at immediately
Drip off, A liquid is dripped off for 2.5 hours, continue insulation reaction after 1 hour, add 8.0 gram 32% of sodium hydroxide solution, adjust solution
PH value is 6-7, and moisturizing obtains 40% collapse protective poly-carboxylic acid water reducing agent mother liquor.
Embodiment 3
210g water, 200 isopentenol polyoxyethylene ethers (TPEG2400), 12g are added in 1000m1 flask with three necks,round bottom
Itaconic acid, 10gN-N DMAAs, 3.0g Ammonium Persulfate 98.5s are used as reaction bottom liquid.
Prepare solution A：24g hydroxypropyl acrylates, 1.5 grams of coloured glaze base propionic acid and 40g water are mixed and are put in addition funnel.
Prepare B solution：0.2 gram of sodium formaldehyde sulfoxylate and 0.4 gram of Vc and 60g water are mixed and is put in dropwise addition bottle funnel.
Stirring to monomer in flask is dissolved, and is warming up to 50 DEG C, and dropwise addition A liquid and B liquid, A liquid 3.0 hours are started simultaneously at immediately
Drip off, A liquid is dripped off for 3.5 hours, continue insulation reaction after 0.5 hour, add 8.0 gram 32% of sodium hydroxide solution, adjust molten
Liquid pH value is 6-7, and moisturizing obtains 40% collapse protective poly-carboxylic acid water reducing agent mother liquor.
With our company universal polycarboxylic water reducer GTS-102 as comparative example, concrete performance (concrete mix reference
GB8076-2008) contrast test is as follows：
Can be seen that the Slump Time losing of Large of collapse protective poly-carboxylic acid water reducing agent of the invention is smaller by above-mentioned test result,
3 days and 28 days compression strength meet the requirements, and higher than universal polycarboxylic water reducer, illustrate to fill the coagulation of collapse protection type water reducer
Native aquation is more complete.
Although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
Understanding can carry out various changes, modification, replacement to these embodiments without departing from the principles and spirit of the present invention
And modification, the scope of the present invention be defined by the appended.
Claims (8)
1. a kind of preparation method of slow release slump retaining polycarboxylate water reducer, it is characterised in that：Comprise the following steps：
By in water, unsaturated APEO, organic carboxyl acid, oxidant input reactor, stirring puts into oxidant to dissolving
Afterwards, 30-60 DEG C is heated to, the A liquid and B liquid of oneself configuration is added dropwise simultaneously thereto, A drops add 3-4 hours, and B drops add 3.5-5h,
After insulation 1-2h, plus it is 6 one 7 that alkali lye is neutralized to pH, and moisturizing to solid content is 40-45%, obtains collapse protective poly-carboxylic acid water reducing agent；
Described A liquid is organic carboxyl acid, acrylic acid alkyl lipid monomer, acrylamide monomers and water；
Described B liquid is reproducibility catalyst, chain-transferring agent and water.
2. the preparation method of a kind of slow release slump retaining polycarboxylate water reducer according to claim 1, it is characterised in that：It is described
Unsaturated APEO be methylallyl alcohol APEO, isopentenol polyoxyethylene ether, methoxy polyoxyethylene ether
Any one or a few in methacrylate, methoxy polyoxyethylene ether acrylate.
3. the preparation method of a kind of slow release slump retaining polycarboxylate water reducer according to claim 1, it is characterised in that：It is described
Organic carboxyl acid for one or more in acrylic acid, methacrylic acid, maleic anhydride, fumaric acid, itaconic acid.
4. the preparation method of a kind of slow release slump retaining polycarboxylate water reducer according to claim 1, it is characterised in that：It is described
Acrylic acid first vinegar, ethyl acrylate, propyl acrylate, acrylic acid hydroxyl second fat, hydroxypropyl acrylate in one or more.
5. the preparation method of a kind of slow release slump retaining polycarboxylate water reducer according to claim 1, it is characterised in that：It is described
Amide-type monomer be acrylamide, in N-N DMAAs or 2- acrylamide-2-methyl propane sulfonic methyl propane sulfonic acids
One or more.
6. the preparation method of a kind of slow release slump retaining polycarboxylate water reducer according to claim 1, it is characterised in that：It is described
Oxidative initiator be one or more in hydrogen peroxide, over cure acid compounds；Described chain-transferring agent is coloured glaze base propionic acid
Or one or two in coloured glaze guanidine-acetic acid；Described reproducibility initiator is sodium formaldehyde sulfoxylate, in vitamin C or sodium hydrogensulfite one
Plant or various.
7. the preparation method of a kind of slow release slump retaining polycarboxylate water reducer according to claim 1, it is characterised in that：It is described
The molecular weight of unsaturated APEO is 1000-3000.
8. a kind of slow release slump retaining polycarboxylate water reducer, it is characterised in that：Including
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| CN201710057876.3A CN106800622A (en) | 2017-01-23 | 2017-01-23 | A kind of slow release slump retaining polycarboxylate water reducer and preparation method thereof |
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| CN201710057876.3A CN106800622A (en) | 2017-01-23 | 2017-01-23 | A kind of slow release slump retaining polycarboxylate water reducer and preparation method thereof |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106947028A (en) * | 2017-03-20 | 2017-07-14 | 上海钢球厂有限公司 | A kind of fluid film gloves and preparation method thereof |
| CN107459599A (en) * | 2017-09-07 | 2017-12-12 | 上海高铁化学建材有限公司 | A kind of anti-chamotte mould polycarboxylate water-reducer and preparation method thereof |
| CN107686539A (en) * | 2017-09-07 | 2018-02-13 | 上海高铁化学建材有限公司 | A kind of polycarboxylate water-reducer of ether-ether copolymerization and preparation method thereof |
| 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 |
| CN108659177A (en) * | 2018-06-11 | 2018-10-16 | 四川同舟化工科技有限公司 | A kind of overlength sustained release slump retaining agent of high-adaptability and its normal low temperature preparation method |
| CN108676131A (en) * | 2018-06-06 | 2018-10-19 | 淮北旭日建材有限公司 | A kind of high-performance polycarboxylic acids water reducing agent and preparation method thereof |
| CN109053967A (en) * | 2018-05-25 | 2018-12-21 | 湖北工业大学 | A kind of stepwise hydrolysis release type polycarboxylic acid slump retaining agent and preparation method |
| CN109626859A (en) * | 2018-12-24 | 2019-04-16 | 山西黄河新型化工有限公司 | A kind of anti-mud slow release slump retaining polycarboxylate water reducer and preparation method thereof |
| CN110041004A (en) * | 2019-03-20 | 2019-07-23 | 昆明巴赛科技有限公司 | A kind of cement water reducing agent and preparation method thereof |
| CN110698612A (en) * | 2019-10-28 | 2020-01-17 | 四川鑫统领新材料有限公司 | Viscosity-reducing polycarboxylate-type water reducer mother liquor, water reducer and preparation method |
| CN112897929A (en) * | 2021-01-26 | 2021-06-04 | 山东同盛建材有限公司 | Slow-release polycarboxylate superplasticizer microsphere and preparation method thereof |
| CN113336466A (en) * | 2021-06-30 | 2021-09-03 | 苏州弗克技术股份有限公司 | Slump-retaining and mud-resisting stabilizing agent for concrete and mortar and preparation method thereof |
| CN113980204A (en) * | 2021-11-29 | 2022-01-28 | 眉山海螺新材料科技有限公司 | Slump-retaining type polycarboxylate superplasticizer and preparation method thereof |
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| CN102503226A (en) * | 2011-10-19 | 2012-06-20 | 中建商品混凝土有限公司 | High slump retaining type polycarboxylic acid water reducing agent with sustained-release effect and preparation method thereof |
| CN103881029A (en) * | 2014-04-17 | 2014-06-25 | 山东卓星化工有限公司 | Heat source-free short-time preparation method of controlled-release type polycarboxylic acid high-performance slump retaining agent |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106947028A (en) * | 2017-03-20 | 2017-07-14 | 上海钢球厂有限公司 | A kind of fluid film gloves and preparation method thereof |
| CN107459599A (en) * | 2017-09-07 | 2017-12-12 | 上海高铁化学建材有限公司 | A kind of anti-chamotte mould polycarboxylate water-reducer and preparation method thereof |
| CN107686539A (en) * | 2017-09-07 | 2018-02-13 | 上海高铁化学建材有限公司 | A kind of polycarboxylate water-reducer of ether-ether copolymerization and preparation method thereof |
| 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 |
| CN109053967A (en) * | 2018-05-25 | 2018-12-21 | 湖北工业大学 | A kind of stepwise hydrolysis release type polycarboxylic acid slump retaining agent and preparation method |
| CN108676131A (en) * | 2018-06-06 | 2018-10-19 | 淮北旭日建材有限公司 | A kind of high-performance polycarboxylic acids water reducing agent and preparation method thereof |
| CN108659177A (en) * | 2018-06-11 | 2018-10-16 | 四川同舟化工科技有限公司 | A kind of overlength sustained release slump retaining agent of high-adaptability and its normal low temperature preparation method |
| CN108659177B (en) * | 2018-06-11 | 2021-02-02 | 四川同舟化工科技有限公司 | High-adaptability ultra-long slow-release slump retaining agent and preparation method thereof at normal and low temperature |
| CN109626859A (en) * | 2018-12-24 | 2019-04-16 | 山西黄河新型化工有限公司 | A kind of anti-mud slow release slump retaining polycarboxylate water reducer and preparation method thereof |
| CN110041004A (en) * | 2019-03-20 | 2019-07-23 | 昆明巴赛科技有限公司 | A kind of cement water reducing agent and preparation method thereof |
| CN110698612A (en) * | 2019-10-28 | 2020-01-17 | 四川鑫统领新材料有限公司 | Viscosity-reducing polycarboxylate-type water reducer mother liquor, water reducer and preparation method |
| CN112897929A (en) * | 2021-01-26 | 2021-06-04 | 山东同盛建材有限公司 | Slow-release polycarboxylate superplasticizer microsphere and preparation method thereof |
| CN112897929B (en) * | 2021-01-26 | 2022-04-26 | 山东同盛建材有限公司 | Slow-release polycarboxylate superplasticizer microsphere and preparation method thereof |
| CN113336466A (en) * | 2021-06-30 | 2021-09-03 | 苏州弗克技术股份有限公司 | Slump-retaining and mud-resisting stabilizing agent for concrete and mortar and preparation method thereof |
| CN113980204A (en) * | 2021-11-29 | 2022-01-28 | 眉山海螺新材料科技有限公司 | Slump-retaining type polycarboxylate superplasticizer and preparation method thereof |
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Application publication date: 20170606 |