CN104448286B - A kind of high-effective concrete air entraining agent, its preparation method and application thereof - Google Patents
A kind of high-effective concrete air entraining agent, its preparation method and application thereof Download PDFInfo
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- CN104448286B CN104448286B CN201410745638.8A CN201410745638A CN104448286B CN 104448286 B CN104448286 B CN 104448286B CN 201410745638 A CN201410745638 A CN 201410745638A CN 104448286 B CN104448286 B CN 104448286B
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- entraining agent
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Abstract
The present invention relates to a kind of high-effective concrete air entraining agent, its preparation method and application thereof.High-effective concrete air entraining agent of the present invention is under the effect of catalyst, with polyethylene polyamine compounds as initiator, adds oxirane and expoxy propane, occurs opening to prepare described high-effective concrete air entraining agent.The high-effective concrete air entraining agent that the present invention is developed has good bleed and the effect of steady bubble, and the amido functional structure in its molecular structure serves effect that is the strongest and that strengthen simultaneously, and the concrete strength that compensate for bringing because bubble introduces declines.
Description
Technical field
The present invention relates to a kind of high-effective concrete air entraining agent, its preparation method and application thereof.
Background technology
In concrete, introduce tiny, uniform, airtight bubble contribute to promoting the endurance quality of concrete, especially
Its lifting in terms of freezing and thawing performance and anti-medium osmosis performance is the most obvious.Draw in fresh concrete simultaneously
Entering bubble, bubble serves ball and the effect of floating torr during mixing and stirring, and mixes and stirs promoting fresh concrete
Performance has obvious beneficial effect, can reduce the generation of the problems such as fresh concrete isolation, bleeding simultaneously.
In general, during concrete mixes and stirs, add content that air entraining agent steep, greatly with optimised coagulation air in soil
Little and distribution etc..The air entraining agent type being generally used at present mainly includes modified rosin air entraining agent, modified saponin
Air entraining agent, alkylbenzenesulfonate air entraining agent, alkyl polyoxyethylene ether sulfonate air entraining agent etc..But these bleeds
It is poor, to shortcomings such as concrete hardening intensity effect are big, therefore the most all to there is bubble stability in agent
How to find a kind of research work of air entrained type compound to introduce in concrete and stablize controlled bubble, again can be to concrete
Hardening strength impact less, become concrete air-entrainer exploitation a great problem！
In existing document, mostly using the way of composite fortifier to develop affects less answering to concrete strength
Mould assembly air entraining agent.But the introducing of reinforcing agent often destroys introducing and the stable process of bubble, to bleed with steady
Bubble effect brings impact.Solving the maximally effective approach of this problem is exactly to strengthen having and the function knot of bleed
Structure unit is combined in a molecular structure by chemical bond, but the research of this respect is limited by subject crossing
System, few people relate to.
Summary of the invention
For in prior art, use the exploitation of compound reinforcing agent that less compound of concrete strength impact is drawn
Gas agent, and the introducing of reinforcing agent often destroys introducing and the stable process of bubble, to bleed and foam stabilizing effect band
The problem having carried out impact.The invention provides a kind of high-effective concrete introducing enhancement component in chemical constitution to draw
Gas agent.
By numerous studies, researcher of the present invention finds that concrete is had certain by the compound with many amine structures
Early strong and potentiation, and the block segments structure with suitable hydrophilic/oleophylic ratio have preferable bleed and
Foam stabilizing effect.Therefore both can be combined by the most suitably synthetic raw material, the most both may be used
To play good bleed and foam stabilizing effect at concrete during newly mixing, it is also possible in course of hardening
Play the effect promoting hydrated cementitious, stablizing air hole structure.
The structure of high-effective concrete air entraining agent of the present invention meets following formula
Wherein s is the integer of 1～8, and m is the integer of 1～5, and n is the integer of 2～10, and
N:m=1:(0.6～3).
High-effective concrete air entraining agent of the present invention is under the effect of catalyst, with polyethylene polyamine compounds
Prepare for initiator, open loop addition of ethylene oxide and expoxy propane.
The mass ratio of polyethylene polyamine compounds of the present invention and catalyst is 1000:(1～5).
Catalyst of the present invention is the one in sodium hydroxide, potassium hydroxide, Feldalat NM, Sodium ethylate.
The invention still further relates to the preparation method of a kind of high-effective concrete air entraining agent, as described below: by polyethylene polyamine
Compounds and catalyst are according to 1000:(1～5) mass ratio put in reactor, be warming up to 90～110
DEG C dehydration 10～30 minutes, then heat to 110～130 DEG C, toward reactor in addition oxirane, its matter
Amount is than for polyethylene polyamine compounds quality 1.2～8.0 times；After reacting 1～3 hour, it is warming up to 130～160
DEG C, in reactor, adding expoxy propane, its mass ratio is polyethylene polyamine compounds quality 4.5～20.5
Times；After continuing reaction 1～3 hour, it is cooled to less than 100 DEG C, in system, adds dilution water, its quality
Added 0.65～7.90 times of material total amount for system, regulation product solid content is to 10～60%.
Polyethylene polyamine of the present invention is diethylenetriamine, triethylene tetramine, TEPA, five ethylene
One in hexamine, six ethylene seven amine, seven ethylene eight amine, eight ethylene nine amine and nine ethylene ten amine.
High-effective concrete air entraining agent of the present invention has the synergism effect of bleed and enhancing, and this is mainly
Wherein research work of air entrained type side chain brings preferable bleed and foam stabilizing effect, and the main chain of polyethylene polyamine has preferably
Potentiation, can partly make up because the concrete strength that air content increase causes declines, and to system
Bleed and foam stability can affect less.
Either being used alone or compound use, the suggestion folding of high-effective concrete air entraining agent of the present invention is solid
Volume is 0.1/10000th～0.5 of cement consumption in concrete.Mix bleed less effective less, mix more and then can cause
Unnecessary waste.
Accompanying drawing explanation
Fig. 1 is structure and the nuclear magnetic spectrogram of the high-effective concrete air entraining agent prepared in embodiment 1；
Fig. 2 is structure and the nuclear magnetic spectrogram of the high-effective concrete air entraining agent prepared in embodiment 2；
Fig. 3 is structure and the nuclear magnetic spectrogram of the high-effective concrete air entraining agent prepared in embodiment 2；
Fig. 4 is structure and the nuclear magnetic spectrogram of the high-effective concrete air entraining agent prepared in embodiment 4.
Detailed description of the invention
Following example have described in more detail the method according to the invention and have prepared high-effective concrete air entraining agent, and
These embodiments are given by way of illustration, its object is to allow person skilled in the art will appreciate that this
Bright content is also implemented according to this, but these embodiments are in no way intended to limit the scope of the present invention.All according to present invention spirit
The equivalence that essence is made changes or modifies, and all should contain within protection scope of the present invention.
In Application Example of the present invention, the cement used is little wild field 52.5R.P. II cement, and sand is fineness
Modulus is the medium sand of Mx=2.6, stone be particle diameter be the rubble of 5-20mm continuous grading.Concrete strength,
Air content and bubble parameter testing are with reference to standard GB/T 8076-2008 " concrete admixture " relevant regulations
Perform.
Synthetic example 1
Diethylenetriamine 103g and Feldalat NM 0.28g is put in reactor, is warming up to 90 DEG C of dehydrations 30
Minute, then heat to 110 DEG C, in reactor, be slowly introducing the oxirane of 440g, react 1 hour
After, it is warming up to 150 DEG C, in reactor, is slowly introducing the expoxy propane of 580g, after continuing reaction 2 hours,
It is cooled to less than 100 DEG C, the dilution water 1120g added in system.Products obtained therefrom code name is N1E2P2,
Solid content is 50.2%, shown in structure and nuclear magnetic spectrogram 1.
Synthetic example 2
TEPA 199g and Sodium ethylate 0.20g is put in reactor, is warming up to 110 DEG C of dehydrations 10
Minute, then heating to 120 DEG C, in reactor, be slowly introducing the oxirane of 1540g, reaction 2 is little
Shi Hou, is warming up to 160 DEG C, is slowly introducing the expoxy propane of 4060g in reactor, continues reaction 1 little
Shi Hou, is cooled to less than 100 DEG C, the dilution water 3900g added in system.Products obtained therefrom code name is
N3E5P10, solid content is 59.5%, and structure and nuclear magnetic spectrogram are as shown in Figure 2.
Synthetic example 3
Eight ethylene nine amine 365g and sodium hydroxide 0.37g are put in reactor, is warming up to 100 DEG C of dehydrations
20 minutes, then heat to 130 DEG C, in reactor, be slowly introducing the oxirane of 484g, react 3
After hour, it is warming up to 130 DEG C, in reactor, is slowly introducing the expoxy propane of 1915g, continue reaction 1
After hour, it is cooled to less than 100 DEG C, the dilution water 8280g added in system.Products obtained therefrom code name is
N7E1P3, solid content is 25.2%, and structure and nuclear magnetic spectrogram are as shown in Figure 3.
Synthetic example 4
Triethylene tetramine 146g and potassium hydroxide 0.71g is put in reactor, is warming up to 100 DEG C of dehydrations
15 minutes, then heat to 120 DEG C, in reactor, be slowly introducing the oxirane of 792g, react 1.5
After hour, it is warming up to 140 DEG C, in reactor, is slowly introducing the expoxy propane of 696g, continue reaction 2 little
Shi Hou, is cooled to less than 100 DEG C, the dilution water 12900g added in system.Products obtained therefrom code name is
N2E3P2, solid content is 11.2%, and structure and nuclear magnetic spectrogram are as shown in Figure 4.
Application Example
Concrete strength has been carried out with reference to standard GB/T 8076-2008 " concrete admixture " relevant regulations
With the mensuration of air content, and use the bubble structure of corresponding concrete test piece that Bubble Parameters analyzer measures
And parameter, experimental result is shown in Table 1.In table, embodiment volume solid from the folding in comparative example is different, and its reason is,
If used with volume, initial airbleed dosage difference is relatively big, and the bad air content that compares is stablized and the number of intensity effect
According to, therefore this application embodiment is to adjust volume so that the initial amount of air entrainment of every kind of air entraining agent is close,
Air content that can be follow-up is stable, intensity effect and bubble parametric results.Result shows: the most initially containing
Under conditions of tolerance, the air content gradual loss of the high-effective concrete air entraining agent that the present invention is developed is less, introduces
Bubble size less, bubble gap factor is the least.This shows that high-effective concrete air entraining agent as herein described has
There are outstanding bleed and the ability of steady bubble.Being found by strong concrete degrees of data, it is efficient that use is invented herein
The different larval instar intensity of the test block of concrete air-entrainer is generally than the test block using other types concrete air-entrainer
Intensity wants height, and this shows that the high-effective concrete air entraining agent developed herein is less on the impact of concrete strength, its
Amido functional structure in molecular structure serves effect that is the strongest and that strengthen, compensate for bringing because bubble introduces
Concrete strength decline.
Table 1 each embodiment sample and the performance comparison of commercially available air entraining agent sample
Claims (5)
1. a high-effective concrete air entraining agent, it is characterised in that the constructor of described high-effective concrete air entraining agent
Close following formula:
Wherein s is the integer of 1～8, and m is the integer of 1～5, and n is the integer of 2～10, and
N:m=1:(0.6～3).
2. the preparation method of the high-effective concrete air entraining agent described in claim 1, it is characterised in that: it is in catalysis
Under the effect of agent, with polyethylene polyamine compounds as initiator, add oxirane and expoxy propane, occur
Opening prepares described high-effective concrete air entraining agent；
The mass ratio of described polyethylene polyamine compounds and catalyst is 1000:(1～5)；
Described catalyst is any one in sodium hydroxide, potassium hydroxide, Feldalat NM, Sodium ethylate.
The preparation method of high-effective concrete air entraining agent the most according to claim 2, it is characterised in that concrete
Comprise the steps:
(1) polyethylene polyamine compounds and catalyst are put in reactor, be warming up to 90～110 DEG C
It is dehydrated 10～30 minutes；
(2) then heating to 110～130 DEG C, add oxirane in reactor, its mass ratio is many second
Alkene polyamine compounds quality 1.2～8.0 times；
(3) after reacting 1～3 hour, it is warming up to 130～160 DEG C, in reactor, adds expoxy propane,
Its mass ratio is polyethylene polyamine compounds quality 4.5～20.5 times；
(4) after continuing reaction 1～3 hour, it is cooled to less than 100 DEG C, in system, adds dilution water, its
Quality is 0.65～7.90 times that system has added material total amount, and regulation product solid content is extremely
10～60%.
4. according to the preparation method of the high-effective concrete air entraining agent described in Claims 2 or 3, it is characterised in that
Described polyethylene polyamine is diethylenetriamine, triethylene tetramine, TEPA, five hexamine, six second
Any one in alkene seven amine, seven ethylene eight amine, eight ethylene nine amine and nine ethylene ten amine.
5. the application process of the high-effective concrete air entraining agent described in claim 1, it is characterised in that described is mixed
The solid volume of folding of solidifying soil air entraining agent is 0.1/10000th～0.5 of cement consumption in concrete.
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| CN105646871A (en) * | 2015-12-31 | 2016-06-08 | 江苏苏博特新材料股份有限公司 | Preparation method of polymer and application thereof |
| CN105727827B (en) * | 2016-01-27 | 2017-10-10 | 江苏苏博特新材料股份有限公司 | Surfactant, its preparation method and application |
| CN110964193B (en) * | 2018-09-30 | 2022-05-31 | 镇江苏博特新材料有限公司 | Concrete foam stabilizer and preparation method thereof |
| CN110885218B (en) * | 2019-12-20 | 2022-03-11 | 中国长江三峡集团有限公司 | Low-temperature-rise, low-shrinkage, high-crack-resistance and high-durability roller compacted concrete and preparation method thereof |
| CN114644478B (en) * | 2020-12-18 | 2023-04-14 | 博特新材料泰州有限公司 | Multi-arm concrete defoamer and preparation method and application thereof |
| CN113087437B (en) * | 2021-04-20 | 2022-03-25 | 北京博润佳科技有限公司 | Composite air entraining agent, preparation method thereof and cement-based material |
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| US4230824A (en) * | 1978-06-12 | 1980-10-28 | Mobay Chemical Corporation | Sucrose based polyether polyols |
| CN102492460A (en) * | 2011-12-21 | 2012-06-13 | 孙安顺 | Preparation method and application of crude oil low-temperature demulsifier |
| CN102558539A (en) * | 2011-12-19 | 2012-07-11 | 上海东大聚氨酯有限公司 | Method for preparing rigid foam polyether polyol by using multi-amine as initiator |
| CN102731769A (en) * | 2011-04-12 | 2012-10-17 | 大连广汇科技有限公司 | Preparation method of high molecular polyethylene polyamine polyether used for preparing water-based functional liquids |
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| US4230824A (en) * | 1978-06-12 | 1980-10-28 | Mobay Chemical Corporation | Sucrose based polyether polyols |
| CN102731769A (en) * | 2011-04-12 | 2012-10-17 | 大连广汇科技有限公司 | Preparation method of high molecular polyethylene polyamine polyether used for preparing water-based functional liquids |
| CN102558539A (en) * | 2011-12-19 | 2012-07-11 | 上海东大聚氨酯有限公司 | Method for preparing rigid foam polyether polyol by using multi-amine as initiator |
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