CN109279809A - A kind of modified air entraining agent and preparation method thereof - Google Patents
A kind of modified air entraining agent and preparation method thereof Download PDFInfo
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- CN109279809A CN109279809A CN201811171081.6A CN201811171081A CN109279809A CN 109279809 A CN109279809 A CN 109279809A CN 201811171081 A CN201811171081 A CN 201811171081A CN 109279809 A CN109279809 A CN 109279809A
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- air entraining
- entraining agent
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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
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
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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
- C04B2103/304—Air-entrainers
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to air entraining agent technical fields, specific a kind of modified air entraining agent and preparation method thereof, it in parts by weight include: 50-60 parts of allyl fatty alcohol-polyoxyethylene ether, 5-9 parts of laureth sodium sulfovinate, 15-20 parts of sulfamic acid, 0.6-1 parts of carbamide peroxide, 1-4 parts of anti-freeze components, 0.2-0.6 parts of catechol, 0.7-1.3 parts of hydroxypropyl methyl fiber, 0.1-0.4 parts of starch ether, 66-70 parts of water；Air entraining agent of the invention solves the problems, such as and poly carboxylic acid series water reducer, inferior suitability, it is good with simple process, rapid reaction, bubble and foam stabilizing effect, bubble compactness and foam stabilizing time good advantage, the stabilization bubble of fine uniform can be introduced in concrete, concrete strength, frost resistance are effectively improved when being used cooperatively with water-reducing agent, reduce slump loss.
Description
Technical field
The present invention relates to air entraining agent technical field, specific a kind of modified air entraining agent and preparation method thereof.
Background technique
Air entraining agent is that one kind can significantly improve workability of concrete and maturing internal pore structure, improves concrete
The most economical effective material of frost resistance and one kind can reduce alkali-aggregate reaction in concrete risk, increase substantially concrete
The additive of the Synthesis durabilities such as impervious and resist chemical energy.Currently, common concrete air-entrainer type has: 1) rosin
Class has and prepares the features such as simple, cheap, foaming characteristic is good, and bubble is big；2) alkyl benzene sulfonate, good with foaming characteristic,
The features such as bubble is big, stability is poor；3) saponins have good water solubility, easily deliquesce, the features such as bubble structure is good；4) fatty acid
And its esters, have the characteristics that foaming characteristic is bad, bubble is small；But poly carboxylic acid series water reducer and rosin thermopolymer or saponins
When concrete air-entrainer mixes, often there is incompatible appearance in the two, and air entraining agent or layering swim in solution surface, or in cotton-shaped heavy
It forms sediment in solution bottom, therefore, studies a kind of function admirable, the good air entraining agent of poly carboxylic acid series water reducer, cement adaptability is to closing weight
It wants.
Summary of the invention
The present invention is in order to solve the above technical problems, the present invention provides a kind of modified air entraining agents and preparation method thereof.
Specifically realized according to following technical scheme:
A kind of modified air entraining agent includes: that 50-60 parts of allyl fatty alcohol-polyoxyethylene ether, laruyl alcohol are poly- in parts by weight
5-9 parts of ether sodium sulfovinate, 15-20 parts of sulfamic acid, 0.6-1 parts of carbamide peroxide, 1-4 parts of anti-freeze components, catechol 0.2-0.6
Part, 0.7-1.3 parts of hydroxypropyl methyl fiber, 0.1-0.4 parts of starch ether, 66-70 parts of water.
The water, temperature are 45-50 DEG C.
The anti-freeze components are one or more of calcium nitrate, calcium formate, calcium acetate, calcium thiocyanate composition.
The preparation method of the modified air entraining agent, includes the following steps:
S1 takes allyl fatty alcohol-polyoxyethylene ether, sulfamic acid, carbamide peroxide to be placed in titanium alloy reactor and stirs
Uniformly, stage is warming up to 100 DEG C, and catechol is then added and stirs evenly, isothermal holding 1-1.5h；
S1 step gains are cooled to 82-87 DEG C by S2, and hydroxypropyl methyl cellulose, starch ether stirring is then added
It is even, isothermal holding 20-30min；
S2 step gains are cooled to 62-67 DEG C by S3, and antifreezing agent is then added and stirs evenly, isothermal holding 10-
15min。
S4 is into S3 step gains plus water, laureth sodium sulfovinate are uniformly mixed to get modified air entraining agent.
The interim heating, is divided into three step-up temperatures, the first stage is warming up to 80 DEG C, and second stage is warming up to 90 DEG C.
One step-up temperature is to be warming up to 80 DEG C with the rate of 0.2-0.5 DEG C/min, then isothermal holding 10min.
The two-stage heating, is to be warming up to 90 DEG C with the rate of 0.8-1.2 DEG C/min, then isothermal holding 20min.
The phase III heating, is to be warming up to 100 DEG C with the rate of 0.2-0.5 DEG C/min, then isothermal holding 8min.
Compared with prior art, the beneficial effects of the present invention are:
Air entraining agent of the invention solves the problems, such as and poly carboxylic acid series water reducer, inferior suitability, has technique
Simply, rapid reaction, bubble and foam stabilizing effect are good, and bubble compactness and foam stabilizing time good advantage can introduce in concrete
The stabilization bubble of fine uniform effectively improves concrete strength, frost resistance when being used cooperatively with water-reducing agent, reduce the coagulation earth fall
Degree of falling loss.
The present invention using catechol promote allyl fatty alcohol-polyoxyethylene ether, sulfamic acid, carbamide peroxide it is anti-
It answers, shortens the reaction time, using hydroxypropyl methyl fiber, starch ether, further improve the viscosity and elasticity of walls, into
And improve bubble stability；Using laureth sodium sulfovinate, the reactivity of air entraining agent, Jin Erti are further improved
High air entraining agent adaptability and dissolubility.
Specific embodiment
Specific embodiments of the present invention will be described in further detail below, but the invention is not limited to these realities
Mode is applied, it is claimed to still fall within the claims in the present invention for any improvement or replacement on the present embodiment essence spirit
Range.
Embodiment 1
A kind of modified air entraining agent includes: allyl fatty alcohol-polyoxyethylene ether 60g, laureth sodium sulfovinate 9g, ammonia
Base sulfonic acid 20g, carbamide peroxide 1g, anti-freeze components 4g, catechol 0.6g, hydroxypropyl methyl fiber 1.3g, starch ether 0.4g, temperature
The water 70g that degree is 50 DEG C；
The anti-freeze components are the composition of calcium nitrate, calcium formate, calcium acetate, calcium thiocyanate；
The preparation method of the modified air entraining agent, includes the following steps:
S1 takes allyl fatty alcohol-polyoxyethylene ether, sulfamic acid, carbamide peroxide to be placed in titanium alloy reactor and stirs
Uniformly, then three step-up temperatures are added catechol and stir evenly to 100 DEG C, isothermal holding 1.5h；
S1 step gains are cooled to 87 DEG C by S2, hydroxypropyl methyl cellulose then are added, starch ether stirs evenly, guarantor
Temperature processing 30min；
S2 step gains are cooled to 67 DEG C by S3, and antifreezing agent is then added and stirs evenly, isothermal holding 15min.
S4 is into S3 step gains plus water, laureth sodium sulfovinate are uniformly mixed to get modified air entraining agent；
One step-up temperature is to be warming up to 80 DEG C with the rate of 0.5 DEG C/min, then isothermal holding 10min；
The two-stage heating, is to be warming up to 90 DEG C with the rate of 1.2 DEG C/min, then isothermal holding 20min；
The phase III heating, is to be warming up to 100 DEG C with the rate of 0.5 DEG C/min, then isothermal holding 8min.
Embodiment 2
A kind of modified air entraining agent includes: allyl fatty alcohol-polyoxyethylene ether 50g, laureth sodium sulfovinate 5g, ammonia
Base sulfonic acid 15g, carbamide peroxide 0.6g, anti-freeze components 1-4g, catechol 0.2g, hydroxypropyl methyl fiber 0.7g, starch ether
0.1g, the water 66g that temperature is 45 DEG C；
The anti-freeze components are calcium formate；
The preparation method of the modified air entraining agent, includes the following steps:
S1 takes allyl fatty alcohol-polyoxyethylene ether, sulfamic acid, carbamide peroxide to be placed in titanium alloy reactor and stirs
Uniformly, then three step-up temperatures are added catechol and stir evenly to 100 DEG C, isothermal holding 1h；
S1 step gains are cooled to 82 DEG C by S2, hydroxypropyl methyl cellulose then are added, starch ether stirs evenly, guarantor
Temperature processing 20min；
S2 step gains are cooled to 62 DEG C by S3, and antifreezing agent is then added and stirs evenly, isothermal holding 10min.
S4 is into S3 step gains plus water, laureth sodium sulfovinate are uniformly mixed to get modified air entraining agent；
One step-up temperature is to be warming up to 80 DEG C with the rate of 0.2 DEG C/min, then isothermal holding 10min；
The two-stage heating, is to be warming up to 90 DEG C with the rate of 0.8 DEG C/min, then isothermal holding 20min；
The phase III heating, is to be warming up to 100 DEG C with the rate of 0.2 DEG C/min, then isothermal holding 8min.
Embodiment 3
A kind of modified air entraining agent includes: allyl fatty alcohol-polyoxyethylene ether 55g, laureth sodium sulfovinate 7g, ammonia
Base sulfonic acid 18g, carbamide peroxide 0.8g, anti-freeze components 1-4g, catechol 0.4g, hydroxypropyl methyl fiber 1g, starch ether 0.2g,
The water 68g that temperature is 50 DEG C；
The anti-freeze components are the composition of calcium nitrate, calcium formate；
The preparation method of the modified air entraining agent, includes the following steps:
S1 takes allyl fatty alcohol-polyoxyethylene ether, sulfamic acid, carbamide peroxide to be placed in titanium alloy reactor and stirs
Uniformly, then three step-up temperatures are added catechol and stir evenly to 100 DEG C, isothermal holding 1.2h；
S1 step gains are cooled to 85 DEG C by S2, hydroxypropyl methyl cellulose then are added, starch ether stirs evenly, guarantor
Temperature processing 25min；
S2 step gains are cooled to 65 DEG C by S3, and antifreezing agent is then added and stirs evenly, isothermal holding 12min.
S4 is into S3 step gains plus water, laureth sodium sulfovinate are uniformly mixed to get modified air entraining agent；
One step-up temperature is to be warming up to 80 DEG C with the rate of 0.4 DEG C/min, then isothermal holding 10min；
The two-stage heating, is to be warming up to 90 DEG C with the rate of 1 DEG C/min, then isothermal holding 20min；
The phase III heating, is to be warming up to 100 DEG C with the rate of 0.3 DEG C/min, then isothermal holding 8min.
Comparative example 1
The preparation of air entraining agent: fatty alcohol polyoxyethylene ether 50g, sulfamic acid 18g, urea 0.5g are put into flask, no
Stop stirring and is gradually warming up to 100 DEG C, constant temperature 4h；70 DEG C are cooled to, hot water 370g dilution is added, then be cooled to 40 DEG C once,
Modified silicone resin polyethers microemulsion 10g is added, stirs to get air entraining agent.
Comparative example 2
In 1000 milliliters of reaction kettles plus water 250g, sodium hydroxide 25g are slowly added to colophony powder when being warming up to 90 DEG C
25gOP-10 emulsifier is added after 90 DEG C of insulation reaction 2-3h in 250g, and water use regulation solid content 35% controls pH value
8.5-9.5 is to get air entraining agent.
Test example 1
5% aqueous solution is made into air entraining agent prepared by embodiment 1-3 and air entraining agent prepared by comparative example 1, comparative example 2,
Its stability is as shown in table 1:
Table 1
Test example 2
Air entraining agent and poly carboxylic acid series water reducer, silicate prepared by the embodiment 1-3 air entraining agent prepared and comparative example 1-2
Cement carries out the test of air content, the slump, and selection cement is portland cement, and rolling over solid volume is the 0.08% of cement quality,
Acquired results are as shown in table 2:
Table 2
| The slump (cm) | Air content (%) | |
| Embodiment 1 | 19.8 | 3.5 |
| Embodiment 2 | 19.3 | 3.6 |
| Embodiment 3 | 20.5 | 3.4 |
| Comparative example 1 | 12.3 | 5.5 |
| Comparative example 2 | 18.5 | 3.4 |
Claims (8)
1. a kind of modified air entraining agent, which is characterized in that include: in parts by weight 50-60 parts of allyl fatty alcohol-polyoxyethylene ether,
5-9 parts of laureth sodium sulfovinate, 15-20 parts of sulfamic acid, 0.6-1 parts of carbamide peroxide, 1-4 parts of anti-freeze components, catechu
0.2-0.6 parts of phenol, 0.7-1.3 parts of hydroxypropyl methyl fiber, 0.1-0.4 parts of starch ether, 66-70 parts of water.
2. modified air entraining agent as described in claim 1, which is characterized in that the water, temperature are 45-50 DEG C.
3. modified air entraining agent as described in claim 1, which is characterized in that the anti-freeze components are calcium nitrate, calcium formate, acetic acid
One or more of calcium, calcium thiocyanate composition.
4. the preparation method of modified air entraining agent as described in claim 1, which comprises the steps of:
S1 takes allyl fatty alcohol-polyoxyethylene ether, sulfamic acid, carbamide peroxide to be placed in titanium alloy reactor and stirs evenly,
Stage is warming up to 100 DEG C, and catechol is then added and stirs evenly, isothermal holding 1-1.5h；
S1 step gains are cooled to 82-87 DEG C by S2, hydroxypropyl methyl cellulose then are added, starch ether stirs evenly, guarantor
Temperature processing 20-30min；
S2 step gains are cooled to 62-67 DEG C by S3, and antifreezing agent is then added and stirs evenly, isothermal holding 10-15min.
S4 is into S3 step gains plus water, laureth sodium sulfovinate are uniformly mixed to get modified air entraining agent.
5. the preparation method of modified air entraining agent as claimed in claim 4, which is characterized in that the interim heating is divided into three ranks
Duan Shengwen, first stage are warming up to 80 DEG C, and second stage is warming up to 90 DEG C.
6. the preparation method of modified air entraining agent as claimed in claim 4, which is characterized in that a step-up temperature, is with 0.2-
The rate of 0.5 DEG C/min is warming up to 80 DEG C, then isothermal holding 10min.
7. the preparation method of modified air entraining agent as claimed in claim 4, which is characterized in that the two-stage heating, is with 0.8-
The rate of 1.2 DEG C/min is warming up to 90 DEG C, then isothermal holding 20min.
8. the preparation method of modified air entraining agent as claimed in claim 4, which is characterized in that the phase III heating, be with
The rate of 0.2-0.5 DEG C/min is warming up to 100 DEG C, then isothermal holding 8min.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111217970A (en) * | 2020-02-25 | 2020-06-02 | 陕西科技大学 | Modified starch concrete air entraining agent and preparation method thereof |
| CN115947563A (en) * | 2022-10-27 | 2023-04-11 | 贵州大学 | Polyether air entraining agent and preparation method and application thereof |
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| CN102276290A (en) * | 2011-07-18 | 2011-12-14 | 马清浩 | Concrete foaming agent and composite additive containing same |
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| CN115947563A (en) * | 2022-10-27 | 2023-04-11 | 贵州大学 | Polyether air entraining agent and preparation method and application thereof |
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