CN108794699A - A kind of preparation method of sustained release high collapse protection type polycarboxylate water-reducer - Google Patents
A kind of preparation method of sustained release high collapse protection type polycarboxylate water-reducer Download PDFInfo
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- CN108794699A CN108794699A CN201810722013.8A CN201810722013A CN108794699A CN 108794699 A CN108794699 A CN 108794699A CN 201810722013 A CN201810722013 A CN 201810722013A CN 108794699 A CN108794699 A CN 108794699A
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- CN
- China
- Prior art keywords
- protection type
- polycarboxylate water
- water
- reducer
- type polycarboxylate
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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
- C04B2103/30—Water reducers, plasticisers, air-entrainers, flow improvers
- C04B2103/302—Water reducers
Abstract
The present invention relates to a kind of sustained release high collapse protection type polycarboxylate water-reducers and preparation method thereof, this method is under normal temperature condition, after allyl polyethenoxy ether (HPEG) is mixed with water, stirring is to being completely dissolved, oxidant/hydroxy-ethyl acrylate and hydroxypropyl acrylate is added, the mixed solution of pre- solvent acrylic acid solution and reducing agent and chain-transferring agent is added dropwise successively, after being added dropwise completely, after reaction solution is fully cured, aqueous slkali is added into reaction solution again, it is 6~6.5 to neutralize pH, you can slow-release high collapse protection type polycarboxylate water-reducer is made.Compared with prior art, the sustained release high collapse protection type polycarboxylate water-reducer of the present invention is chemical slow release high collapse protection type polycarboxylate water-reducer, pass through the fracture of chemical bond, slow release, the concentration of polycarboxylate water-reducer is set to obtain lasting growth to achieve the purpose that keep high-thin arch dam effect, the sustained release high collapse protection type polycarboxylate water-reducer of the present invention is strong in various source cement material compatibilities, can effectively shield the interference effect of soil in sandstone.
Description
Technical field
The invention belongs to chemical building material technical fields, are related to a kind of preparation side of sustained release high collapse protection type polycarboxylate water-reducer
Method.
Background technology
For ready-mixed concrete industry, when fresh concrete long-distance transportation and hot weather transport, the slump
Lose excessive, high degree influences the quality and performance of concrete, is to perplex normal construction and problem in the urgent need to address.
In order to solve problem above, existing solution is typically that the slightly more water-reducing agent of more normal volume is added or will subtract
Aqua is used in combination with retarder and water-retaining agent.But there are certain drawbacks for these schemes, for example concrete slump is full sometimes
Sufficient construction requirement but early strength of concrete is too low and unacceptable, go wrong there is also concrete and cement compatibility and
The too fast and abnormal condensation phenomenon of slump-loss occurs, can occur the slump of rapid condensation suddenly using part retarder sometimes
Degree loss.
In addition, with the development of polycarboxylate water-reducer synthetic technology, also about chemical slow release type polycarboxylate water-reducer side
The report in face.Wherein, the 1 (patent No. of documents：201610402278.0) propose through polyethylene glycol, thioglycolic acid, three
Chloromethanes and hydroquinone etc. synthesize sustained-release polycarboxylic water reducer.But this synthesis technology is more complex, and reaction raw materials have
There is poisonous and harmful substance.2 (the patent No. of documents：201611119375.5) propose to pass through itaconic acid, itaconic anhydride and horse
Dimethyl phthalate etc. synthesizes sustained-release polycarboxylic water reducer, but in this synthesis technology is related to that monomeric species are more and all kinds of lists more
The reactivity ratio difference of body is larger, and synthetic system certainly will be caused unstable.
Invention content
In view of the drawbacks of the prior art, the present invention is based on polycarboxylate water-reducer molecule structure designability is strong, absorption-point
Internal relation is dissipated, a kind of slow-release high collapse protection type polycarboxylate water-reducer is provided, by controlling polycarboxylate water-reducer in cement
Initial adsorption amount and the rate of adsorption on grain surface, can effectively control the slump-loss degree of fresh concrete, have good
Application effect and market prospects.
To achieve the above object, the present invention is achieved through the following technical solutions：
A kind of preparation method of sustained release high collapse protection type polycarboxylate water-reducer, this method is under normal temperature condition, by allyl
After polyoxyethylene ether (HPEG) is mixed with water, oxidant, hydroxy-ethyl acrylate and acrylic acid hydroxypropyl is added to being completely dissolved in stirring
Ester, is stirred well to uniformly mixed, then pre- solvent unsaturated acrylic acid solution and reducing agent and chain-transferring agent is added dropwise successively
Mixed solution after fully curing reaction solution, then aqueous slkali is added into reaction solution after being added dropwise completely, and it is 6 to neutralize pH
~6.5, you can slow-release high collapse protection type polycarboxylate water-reducer is made.
A kind of preparation method of sustained release high collapse protection type polycarboxylate water-reducer, this method specifically include following steps：
(1) it is 100 by the mass ratio of allyl polyethenoxy ether (HPEG) and water under normal temperature condition：(100~140),
By in allyl polyethenoxy ether (HPEG) and water input reaction vessel, it is stirred well to HPEG and is completely dissolved；
(2) into the reaction vessel of step (1), it is added at one time oxidant, hydroxy-ethyl acrylate and hydroxypropyl acrylate,
It is stirred well to and is completely dispersed uniformly；
(3) acrylic acid is added to the water, it is 1~5% to be pre-dissolved acrylic acid solution to be configured to mass concentration, waits for step (2)
After stirring evenly, dropwise addition is pre-dissolved acrylic acid solution, and control time for adding is 2~3h；
(4) reducing agent and chain-transferring agent are added to the water, are configured to reducing agent and chain tra nsfer that mass concentration is 2~5%
The mixed solution of agent waits for that step (2) stirring to after mixing, is added dropwise the mixed solution for being pre-dissolved reducing agent and chain-transferring agent, controls
System is pre-dissolved reducing agent and the mixed solution time for adding of chain-transferring agent is longer 0.5~1h than the time for adding of acrylic acid solution；
(5) after reducing agent in step (4) and chain-transferring agent mixed solution are added dropwise completely, continue to be stirred to react solution 0.5
A certain amount of aqueous slkali, neutralization reaction pH value of solution to 6~6.5 is added after reaction solution temperature is down to 30 DEG C in~1h, you can system
Obtain slow-release high collapse protection type polycarboxylate water-reducer.
In a preferred embodiment of the present invention, the matter of the allyl polyethenoxy ether (HPEG) and hydroxy-ethyl acrylate
Amount is than being 100：(5.0~7.5).
In a preferred embodiment of the present invention, the matter of the allyl polyethenoxy ether (HPEG) and hydroxypropyl acrylate
Amount is than being 100：(2.0~4.0).
In a preferred embodiment of the present invention, the allyl polyethenoxy ether (HPEG) and the mass ratio of acrylic acid are
100:(0.5~2.0).
In a preferred embodiment of the present invention, the oxidant quality is allyl polyethenoxy ether (HPEG) quality
1.5%.
In a preferred embodiment of the present invention, the reducing agent quality is allyl polyethenoxy ether (HPEG) quality
0.3%.
In a preferred embodiment of the present invention, the chain-transferring agent quality is allyl polyethenoxy ether (HPEG) quality
0.5%.
In a preferred embodiment of the present invention, the allyl polyethenoxy ether (HPEG) average molecular mass is
2100, the oxidant is one or both of ammonium persulfate, hydrogen peroxide, and the reducing agent is L-AA, institute
The chain-transferring agent stated is one kind in mercaptopropionic acid or thioacetic acid, and the aqueous slkali is that the NaOH of 30% mass concentration is molten
Liquid, KOH solution or Ca (OH)2In one kind, the water be tap water.
In a preferred embodiment of the present invention, the oxidant is ammonium persulfate, and the chain-transferring agent is sulfydryl second
Acid, the aqueous slkali are the NaOH solution of 30%30% mass concentration.
Formulation manipulation application is optimized by preferred radical polymerization initiator, and to initiator, thus the present invention closes
The mother liquor solid content of the polycarboxylate water-reducer of gained is prepared as 35-45% without heating and temperature control at whole in technique, is colourless
Transparent milk liquid thick liquid, with short production cycle, only 3h or so, energy consumption is low, not only energy saving, but also greatly reduces production
Cost, and can widely apply in the industrial production.
Polycarboxylate water-reducer of the present invention is meeting GB8076-2008《Concrete admixture》On the basis of national standard,
Improving in terms of concrete slump retention property has unique advantage, especially suitable for strength grade is C50 and below mixed
In solidifying soil, price is relatively low, cost-effective, and high temperature sweltering heat weather and long-distance transport concrete slump retaining performance are good, and cement adaptability is wide
General, late strength of concrete is high.
Polycarboxylate water-reducer of the present invention be applied to armored concrete, light aggregate concrete, artificial aggregate concrete, bridge,
In the production of the works such as building, water conservancy project and road surface, there is higher water-reducing rate, concrete workability, pumpability can be effectively improved,
High temperature sweltering heat weather and long-distance transport concrete slump retaining performance are good, have excellent raw material adaptability.
Compared with prior art, the invention has the characteristics that：
1) sustained release high collapse protection type polycarboxylate water-reducer of the invention is chemical slow release high collapse protection type polycarboxylate water-reducer, is passed through
The fracture of chemical bond, slow release make the concentration of polycarboxylate water-reducer obtain lasting growth and keep high-thin arch dam effect to reach
Purpose.
2) sustained release high collapse protection type polycarboxylate water-reducer of the invention not only ensures that concrete production technology is simple, but also to mixed
The early strength for coagulating soil will not have an adverse effect.
3) sustained release high collapse protection type polycarboxylate water-reducer of the invention is strong in various source cement material compatibilities, can be effective
Shield the interference effect of soil in sandstone.
Specific implementation mode
With reference to specific embodiment, the present invention is described in detail.
Embodiment 1：
Allyl polyethenoxy ether (HPEG) 200g, water 200g is added under room temperature into the reactor equipped with agitating device,
Agitating device is opened, stirring to HPEG polymeric monomers is completely dissolved.Ammonium persulfate 3g, hydroxy-ethyl acrylate is added to reaction system
10g, hydroxypropyl acrylate 4g are stirred well to and are completely dissolved and are uniformly dispersed.4g acrylic acid is uniformly mixed preparation with 35g water
At acrylic acid solution (i.e. A material), by 1g thioacetic acid, 0.6gL- ascorbic acid is uniformly mixed with 40g water and is prepared into thioacetic acid
With the mixed solution (being B material) of L-AA.It is controlled by valving, A material and B material is gradually at the uniform velocity added dropwise to reaction
System, wherein A expects that time for adding is 2.5 hours, and B expects that time for adding is 3 hours.After A, B material are added dropwise to complete completely, continue
It is stirred to react solution 0.5 hour, after reaction solution temperature is down to 30 DEG C, the NaOH solution of 30% mass concentration is added, neutralizes
Reaction solution pH to 6.5, you can slow-release high collapse protection type polycarboxylate water-reducer is made.
Embodiment 2：
Allyl polyethenoxy ether (HPEG) 200g, water 280g is added under room temperature into the reactor equipped with agitating device,
Agitating device is opened, stirring to HPEG polymeric monomers is completely dissolved.Ammonium persulfate 3g, hydroxy-ethyl acrylate is added to reaction system
15g, hydroxypropyl acrylate 8g are stirred well to and are completely dissolved and are uniformly dispersed.1g acrylic acid is uniformly mixed preparation with 40g water
At acrylic acid solution (i.e. A material), by 1g thioacetic acid, 0.6gL- ascorbic acid is uniformly mixed with 50g water and is prepared into thioacetic acid
With the mixed solution (being B material) of L-AA.It is controlled by valving, A material and B material is gradually at the uniform velocity added dropwise to reaction
System, wherein A expects that time for adding is 3 hours, and B expects that time for adding is 4 hours.After A, B material are added dropwise to complete completely, continue to stir
It mixes reaction solution 0.5 hour, after reaction solution temperature is down to 30 DEG C, the NaOH solution of 30% mass concentration is added, neutralize anti-
Answer pH value of solution to 6, you can slow-release high collapse protection type polycarboxylate water-reducer is made.
Embodiment 3：
Allyl polyethenoxy ether (HPEG) 200g, water 240g is added under room temperature into the reactor equipped with agitating device,
Agitating device is opened, stirring to HPEG polymeric monomers is completely dissolved.Ammonium persulfate 3g, hydroxy-ethyl acrylate is added to reaction system
12g, hydroxypropyl acrylate 5g are stirred well to and are completely dissolved and are uniformly dispersed.2g acrylic acid is uniformly mixed preparation with 40g water
At acrylic acid solution (i.e. A material), by 1g thioacetic acid, 0.6gL- ascorbic acid is uniformly mixed with 50g water and is prepared into thioacetic acid
With the mixed solution (being B material) of L-AA.It is controlled by valving, A material and B material is gradually at the uniform velocity added dropwise to reaction
System, wherein A expects that time for adding is 2 hours, and B expects that time for adding is 2.5 hours.After A, B material are added dropwise to complete completely, continue
It is stirred to react solution 0.5 hour, after reaction solution temperature is down to 30 DEG C, the NaOH solution of 30% mass concentration is added, neutralizes
Reaction solution pH to 6, you can slow-release high collapse protection type polycarboxylate water-reducer is made.
To C30 ready-mixed concrete (concrete each component match ratio is shown in Table 1), adds polycarboxylic acids made from 1-3 embodiments and subtract
The properties of aqua, concrete are shown in Table 2.
1 concrete mix of table
| Cement | Flyash | Water | Sand | Great Shi | Gravelstone | Glue material total amount | W/C | Sand coarse aggregate ratio |
| 307 | 45 | 172 | 789 | 413 | 619 | 352 | 0.49 | 43% |
Table 2 implements concrete performance data
Claims (10)
1. a kind of normal temperature preparation method of sustained release high collapse protection type polycarboxylate water-reducer, which is characterized in that this method is in room temperature item
Under part, after allyl polyethenoxy ether (HPEG) is mixed with water, oxidant, acrylic acid hydroxyl second is added to being completely dissolved in stirring
Ester and hydroxypropyl acrylate, be stirred well to it is uniformly mixed, then be added dropwise successively pre- solvent unsaturated acrylic acid solution and also
Former agent and chain-transferring agent mixed solution after fully curing reaction solution, then alkali are added into reaction solution after being added dropwise completely
Solution, it is 6~6.5 to neutralize pH, you can slow-release high collapse protection type polycarboxylate water-reducer is made.
2. a kind of normal temperature preparation method of slow-release high collapse protection type polycarboxylate water-reducer according to claim 1, feature
It is, this method specifically includes following steps：
(1) it is 100 by the mass ratio of allyl polyethenoxy ether (HPEG) and water under normal temperature condition：(100~140), by alkene
Propyl polyoxyethylene ether (HPEG) is stirred well to HPEG and is completely dissolved with water input reaction vessel；
(2) into the reaction vessel of step (1), it is added at one time oxidant, hydroxy-ethyl acrylate and hydroxypropyl acrylate, fully
Stirring is uniform to being completely dispersed；
(3) acrylic acid is added to the water, it is 1~5% to be pre-dissolved acrylic acid solution to be configured to mass concentration, waits for that step (2) stirs
After uniformly, dropwise addition is pre-dissolved acrylic acid solution, and control time for adding is 2~3h；
(4) reducing agent and chain-transferring agent are added to the water, are configured to reducing agent and chain-transferring agent that mass concentration is 2~5%
Mixed solution waits for step (2) stirring to the mixed solution for being pre-dissolved reducing agent and chain-transferring agent after mixing, is added dropwise, and control is pre-
The mixed solution time for adding of molten reducing agent and chain-transferring agent is longer 0.5~1h than the time for adding of acrylic acid solution；
(5) after reducing agent in step (4) and chain-transferring agent mixed solution are added dropwise completely, continue to be stirred to react 0.5~1h of solution,
After reaction solution temperature is down to 30 DEG C, a certain amount of aqueous slkali, neutralization reaction pH value of solution to 6~6.5 is added, you can sustained release is made
Type high collapse protection type polycarboxylate water-reducer.
3. a kind of normal temperature preparation method of sustained release high collapse protection type polycarboxylate water-reducer according to claim 2, feature exist
In the mass ratio of the allyl polyethenoxy ether (HPEG) and hydroxy-ethyl acrylate is 100：(5.0~7.5).
4. a kind of normal temperature preparation method of sustained release high collapse protection type polycarboxylate water-reducer according to claim 2, feature exist
In the mass ratio of the allyl polyethenoxy ether (HPEG) and hydroxypropyl acrylate is 100：(2.0~4.0).
5. a kind of preparation method of sustained release high collapse protection type polycarboxylate water-reducer according to claim 2, which is characterized in that institute
The mass ratio of the allyl polyethenoxy ether (HPEG) stated and acrylic acid is 100:
(0.5~2.0).
6. a kind of preparation method of sustained release high collapse protection type polycarboxylate water-reducer according to claim 2, which is characterized in that institute
The oxidant quality stated is the 1.5% of allyl polyethenoxy ether (HPEG) quality.
7. a kind of preparation method of sustained release high collapse protection type polycarboxylate water-reducer according to claim 2, which is characterized in that institute
The reducing agent quality stated is the 0.3% of allyl polyethenoxy ether (HPEG) quality.
8. a kind of preparation method of slow-release high collapse protection type polycarboxylate water-reducer according to claim 2, which is characterized in that
The chain-transferring agent quality is the 0.5% of allyl polyethenoxy ether (HPEG) quality.
9. a kind of preparation method of slow-release high collapse protection type polycarboxylate water-reducer according to claim 2, which is characterized in that
Described allyl polyethenoxy ether (HPEG) average molecular mass is 2100, and the oxidant is ammonium persulfate, double
One or both of oxygen water, the reducing agent are L-AA, and the chain-transferring agent is mercaptopropionic acid or sulfydryl second
One kind in acid, the aqueous slkali are NaOH solution, KOH solution or the Ca (OH) of 30% mass concentration2In one kind, it is described
Water be tap water.
10. a kind of preparation method of slow-release high collapse protection type polycarboxylate water-reducer according to claim 2, feature exist
In the oxidant is ammonium persulfate, and the chain-transferring agent is thioacetic acid, and the aqueous slkali is 30% mass concentration
NaOH solution.
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Cited By (7)
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| CN109879628A (en) * | 2019-02-25 | 2019-06-14 | 谢新昇 | A kind of water-resistant type building mortar plasticizer and preparation method thereof |
| CN111116841A (en) * | 2019-12-31 | 2020-05-08 | 陕西友邦新材料科技有限公司 | Viscosity-reducing polycarboxylate superplasticizer mother liquor as well as preparation method and application thereof |
| CN111116840A (en) * | 2019-12-31 | 2020-05-08 | 陕西友邦新材料科技有限公司 | Compound polycarboxylate superplasticizer mother liquor as well as preparation method and application thereof |
| CN111793174A (en) * | 2020-07-31 | 2020-10-20 | 贵州石博士科技有限公司 | Normal-temperature synthesis method of multi-element-initiated slow-release slump-retaining polycarboxylic acid water reducer |
| CN113549182A (en) * | 2021-08-30 | 2021-10-26 | 科之杰新材料集团(广东)有限公司 | Slow-release water reducing agent and preparation method thereof |
| CN113956406A (en) * | 2021-10-09 | 2022-01-21 | 科之杰新材料集团有限公司 | Slump-retaining type polycarboxylate superplasticizer and preparation method thereof |
| CN115449024A (en) * | 2022-06-24 | 2022-12-09 | 江西迪特科技有限公司 | Preparation method of high-workability slump-retaining type polycarboxylate superplasticizer |
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| CN109879628A (en) * | 2019-02-25 | 2019-06-14 | 谢新昇 | A kind of water-resistant type building mortar plasticizer and preparation method thereof |
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| CN111116840A (en) * | 2019-12-31 | 2020-05-08 | 陕西友邦新材料科技有限公司 | Compound polycarboxylate superplasticizer mother liquor as well as preparation method and application thereof |
| CN111793174A (en) * | 2020-07-31 | 2020-10-20 | 贵州石博士科技有限公司 | Normal-temperature synthesis method of multi-element-initiated slow-release slump-retaining polycarboxylic acid water reducer |
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| CN115449024A (en) * | 2022-06-24 | 2022-12-09 | 江西迪特科技有限公司 | Preparation method of high-workability slump-retaining type polycarboxylate superplasticizer |
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Application publication date: 20181113 |