CN112707675B - Efficient concrete defoaming agent composition and preparation method thereof - Google Patents
Efficient concrete defoaming agent composition and preparation method thereof Download PDFInfo
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- CN112707675B CN112707675B CN202011150230.8A CN202011150230A CN112707675B CN 112707675 B CN112707675 B CN 112707675B CN 202011150230 A CN202011150230 A CN 202011150230A CN 112707675 B CN112707675 B CN 112707675B
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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
- C04B2103/50—Defoamers, air detrainers
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- Ceramic Engineering (AREA)
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Abstract
The invention relates to the technical field of building additives, in particular to a high-efficiency concrete defoamer composition and a preparation method thereof, wherein the high-efficiency concrete defoamer composition comprises a defoaming component with a defoaming function, a defoaming assistant component and a foam inhibiting component consisting of alkynol polyether and alkynol. According to the high-efficiency concrete defoamer composition provided by the invention, through polyether graft modification of polysiloxane, a hydrophilic polyether chain segment can improve the dispersibility in water, so that the polysiloxane chain segment is water-soluble, a hydrophobic polysiloxane chain segment is endowed with low surface tension, and meanwhile, different surface activities can be achieved by adjusting the arrangement, the number and the like of a polyoxyethylene chain segment and a polyoxypropylene chain segment in the polyether chain segment. And the acetylene glycol and the ethoxylate thereof which are used in a composite way have a synergistic effect, so that the balance and dynamic surface tension is remarkably lower, and the acetylene glycol and the ethoxylate thereof have the functions of defoaming, foam inhibition and the like.
Description
Technical Field
The invention relates to the technical field of building additives, in particular to a high-efficiency concrete defoamer composition and a preparation method thereof.
Background
The concrete is accompanied by a large amount of harmful bubbles in stirring and the work progress and produces, and the production of harmful bubbles not only can influence the quality and the outward appearance of product, causes the concrete defect for the honeycomb pitted skin appears in the concrete outward appearance, and inside can form a large amount of holes, has reduced the void ratio of concrete inner structure, causes concrete mechanical properties, durability's degradation etc. has shortened the life of concrete. Modern concrete puts high demands on strength and durability, so that the air content of the concrete, the stability and the quality of air bubbles need to be controlled, wherein the control and the elimination of harmful foams have great technical and economic significance.
The defoaming agent can reduce the surface tension of a liquid phase, is easy to spread on the surface of the solution, reduces the strength of the liquid film, enables the liquid film to be locally thinned, and can inhibit the generation of foam within a period of time, namely, has a defoaming function. For example, patent documents with publication number of CN106336138B, publication date of 2018, 10 and 19 and name of 'a foam control agent and an air-entraining and water-reducing compound agent and concrete prepared from the foam control agent' disclose a foam control agent which is mainly compounded by three alkynol wetting agents; and the concrete defoamer disclosed by the patent document CN107955173A, with the publication date of 24.4.2018 and the name of 'a novel concrete defoamer and a synthetic method thereof' is polyether, acrylate containing glycosyl and siloxane block polymer with low hydrogen content; the defoaming agent has a certain defoaming function, harmful large bubbles can be eliminated, the stability of excellent bubbles is reduced, and a part of micro bubbles beneficial to concrete are eliminated, so that the mechanical property and the durability of the concrete are reduced, and the concrete is required to be further improved.
Disclosure of Invention
In order to solve the problem that the prior defoaming agent mentioned in the background art can destroy the stability of excellent bubbles while eliminating the harmful bubbles to concrete, the invention provides a high-efficiency concrete defoaming agent composition, which comprises a silane defoaming component and a defoaming auxiliary component with defoaming function, and a foam inhibiting component consisting of alkynol polyether and alkynol;
wherein the silane defoaming component has a general formula shown in a structure of a formula (I):
wherein: r 1 is-CH 2 CH 2 -，-CH 2 CH 2 CH 2 -，-CH 2 CH 2 CH 2 CH 2 -one of the above; r is 2 is-H, -CH 3 One of (1); a. b, c, d, e and f are integers of 2-10.
The silane defoaming component is prepared by adopting a conventional preparation method through hydrosilylation reaction of Si-H group of a side chain in hydrogen-containing silicone oil and double bonds in unsaturated terminal enol polyether.
Further, it also includes having-CH 2 CH 2 O-structural unit and-CH 2 CH 2 CH 2 An emulsifying component of an O-structural unit, a cellulose derivative with foam stabilizing effect and an antiseptic component of isothiazolinone as an active component.
Further, the paint comprises the following components in percentage by mass:
5 to 40 percent of defoaming component, 2 to 10 percent of auxiliary defoaming component,
5-40% of foam inhibiting component composed of alkynol polyether and alkynol,
2% -10% of a compound having-CH 2 CH 2 O-structural unit and-CH 2 CH 2 CH 2 Emulsified component of O-structural units
0.2 to 2 percent of cellulose derivative with foam stabilizing effect, 0.1 to 1 percent of antiseptic component with isothiazolinone as active component and the balance of water.
Further, the absorption-aiding component consists of a component with a structure shown in the formula (II) and a component with a structure shown in the formula (III),
wherein: g is an integer of 4 to 10, h is an integer of 5 to 9; the auxiliary components can quickly permeate into the liquid and quickly diffuse away, and stubborn foams generated by the emulsified components are eliminated, so that a defoaming effect is achieved; and simultaneously overcomes the defect of residual silicon spots of the silicon defoamer.
Further, the mass ratio of the component with the structure of the formula (II) to the component with the structure of the formula (III) in the auxiliary digestion component is (1-16): 4.
Further, the mass ratio of the alkynol polyether to the alkynol in the foam inhibiting component is (1-10):1, and the alkynol defoaming agent is used as the foam inhibiting component for maintaining excellent bubble stability and keeping beneficial small bubbles.
Further, the alkynol polyether has a general formula shown as the following formula (IV):
wherein: i is an integer of 1 to 3, j is an integer of 2 to 10, and k is an integer of 2 to 10.
Further, the alkynol has a general formula shown in a structure of a formula (V):
wherein:
R 3 is-H, -CH 3 One of (1);
R 4 is-H, -CH 3 ，-CH 2 CH 3 ，-CH(CH 2 ) 2 ，-CH 2 CH 2 CH 3 ，-CH 2 CH(CH 2 ) 2 ，-CH 2 CH 2 CH 2 CH 3 ，-CH 2 CH 2 CH(CH 2 ) 2 ，-CH 2 CH 2 CH 2 CH 2 CH 3 ，-CH 2 CH 2 CH 2 CH(CH 2 ) 2 One of (a) and (b);
R 5 is-H, -CH 3 ，-CH 2 CH 3 One kind of (1).
Further, the emulsifying component is formed by compounding an emulsifier A with a structure shown in the following formula (VI) and an emulsifier B with a structure shown in the following formula (VII):
C 13 H 27 O(CH 2 CH 2 O) p (CH 2 CH 2 CH 2 O) q H (Ⅵ)
C 18 H 37 O(CH 2 CH 2 O) s (CH 2 CH 2 CH 2 O) t H (Ⅶ)
wherein:
p and q are integers of 2-20, and p and q can be the same or different;
s and t are integers of 2-20, and s and t can be the same or different;
the emulsified component is easy to disperse, has excellent wettability, permeability and emulsibility, and is beneficial to eliminating intractable foams generated by the emulsified component.
Further, the mass ratio of the emulsifier A to the emulsifier B is (1-16): 4.
Further, the cellulose derivative is one of Hydroxypropyl Methylcellulose (HMPC), hydroxyethyl methylcellulose (HEMC), hydroxyethyl cellulose (HEC), and hydroxypropyl cellulose (HPC).
Furthermore, the antiseptic component is formed by compounding 2-methyl-4-isothiazoline-3-ketone and 2-methyl-5-chlorine-4-isothiazoline-3-ketone.
Further, the mass ratio of the 2-methyl-4-isothiazolin-3-ketone to the 2-methyl-5-chloro-4-isothiazolin-3-ketone is (1-16) to 4.
The invention also provides a preparation method of the high-efficiency concrete defoamer composition, which comprises the following steps:
firstly, adding 20-80% of a silane defoaming component, a defoaming-assisting component, a foam-inhibiting component and an emulsifying component into a reactor for premixing;
step two, heating to 65-70 ℃, controlling the stirring speed to be 500-;
step three, increasing the stirring speed of the stirrer to 3000-4000rpm, then adding the cellulose derivative, the water and the rest emulsified components into the reactor, and continuing stirring for 30-60 min; cooling to room temperature, and adding the antiseptic component to obtain the product;
the silane defoaming component, the defoaming assistant component and the foam inhibiting component all contain polyether chain segments, premixing is firstly carried out, the intersolubility is better, and the later added emulsifying component mainly aims at improving the water solubility and ensuring the defoaming effect.
Compared with the prior art, the high-efficiency concrete defoamer composition provided by the invention has the following technical principles and effects:
1. the polyether graft modified polysiloxane and the hydrophilic polyether chain segment can improve the dispersibility in water and endow the water-solubility with the hydrophilic polyether chain segment, the hydrophobic polysiloxane chain segment endows the low surface tension with the hydrophobic polysiloxane chain segment, and simultaneously, different surface activities can be achieved by adjusting the arrangement, the number and the like of the polyoxyethylene chain segment and the polyoxypropylene chain segment in the polyether chain segment.
2. The acetylene glycol and the ethoxylate thereof are used in a compounding way, the water solubility of the molecule is increased by adding the ethoxylate group into the acetylene glycol molecule, the effect of reducing the surface tension is not influenced, and the foam control performance of the product is improved.
3. By compounding the defoaming agent, the synergistic effect of each component can be fully exerted, the defoaming capability is obviously improved, the generation of foam is prevented, the excellent bubble stability is maintained, beneficial small bubbles are kept, and the defoaming agent has certain foam inhibition performance.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the following description will clearly and completely describe the technical solutions in the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides examples and comparative examples as shown in table 1:
TABLE 1
Comparative example 1 is a commercially available polyether modified silane defoamer, specifically a defoamer having a product model number of FAG470, manufactured by jiangsu four new interfacial agent technologies ltd.
Comparative example 2
The alkynol polyethers of the formula IV added in example 1 were replaced in full and in equal amounts by alkynols of the formula V, the remainder remaining unchanged.
Comparative example 3
The alkynol of the formula V added in example 2 was replaced in all equal amounts by the alkynol polyether of the formula IV, the remainder remaining unchanged.
The invention also provides a preparation method of the embodiment, which comprises the following steps:
firstly, adding a defoaming component, a defoaming aid component, a foam inhibiting component and 60% of an emulsifying component into a reactor for premixing;
step two, heating to 65 ℃, controlling the stirring speed to be 600rpm, and continuously stirring for 15 min;
step three, increasing the stirring speed of the stirrer to 3000rpm, then adding the cellulose derivative, water and the rest of the emulsified components into the reactor, and continuing stirring for 30 min; cooling to room temperature, and adding antiseptic to obtain the final product.
The defoamer compositions prepared in the above examples and comparative examples were tested for concrete application performance by the following methods:
the cement is P.O42.5R cement (Longyan Fufu cement); the fine aggregate is river sand (Xiamen forward building material) with fineness modulus of 2.7; the coarse aggregate is continuous graded broken stone (Xiamen is a building material) with the particle size of 5-20 mm; the mineral powder is S95 grade (Quanzhou Lu new building material); the fly ash is level II (Zhangzhou gangue power plant); the water for the test meets the regulation of JGJ63-2006 Water for concrete Standard; compounding a mother solution of a Point-TS8 type polycarboxylate superplasticizer (produced by Jie New Material group Co., Ltd., Kejie) with a defoaming agent to form a concrete admixture, wherein the addition amount of the defoaming agent is 0.1 percent of the mass of Point-TS 8; the mixing amount of the concrete admixture is 0.18 percent of the cementing material. Concrete mix ratios are shown in table 2:
TABLE 2 concrete mix proportion
| Variety of material | Cement | River sand | Crushing stone | Fly ash | Mineral powder | Water (W) |
| The dosage is kg/m 3 | 330 | 640 | 1140 | 30 | 50 | 165 |
The concrete mixture performance test method and the hardened concrete performance test are carried out according to GB/T50080-2016 standard of common concrete mixture performance test method and GB/T50081-2019 standard of concrete physical and mechanical performance test method. The concrete test results are shown in table 3:
TABLE 3 results of testing the performance of the defoamer concrete
The present invention also performs a performance evaluation test on the above examples and comparative examples, the test method is as follows:
1. evaluation of stability:
adjusting the concentration of the prepared defoaming agent composition to 20%, placing the composition in a standard colorimetric tube, standing for 72 hours, and observing whether layering occurs or not so as to evaluate the stability of the defoaming agent;
2. defoaming and foam inhibition evaluation:
under normal pressure and temperature conditions, 5g of commercially available Point-TS8 type polycarboxylate superplasticizer mother liquor (produced by Kejie New materials group Co., Ltd.), 2g of sodium dodecylbenzene sulfonate and 98g of saturated calcium hydroxide solution are added into a 1000ml measuring cylinder, a cork is used for plugging the measuring cylinder, the measuring cylinder is vibrated up and down for 15 times, and the foam height (V) is recorded 0 ) And defoaming time (t) 0 )；
Under normal pressure and temperature conditions, 5g of Point-S polycarboxylic acid (produced by Corjie New materials group Co., Ltd.) sold on the market and 2g of sodium dodecylbenzenesulfonate are added into a 1000ml measuring cylinder, a cork is used to plug the measuring cylinder, the cylinder is shaken up and down for 15 times, 10ml of defoamer composition with the mass fraction of 0.05 percent is dripped in, and the defoaming time (t) is recorded 1 )；
Under normal pressure and temperature conditions, 5g of commercially available Point-S polycarboxylic acid (produced by Kojie New Material group Co., Ltd.), 2g of sodium dodecylbenzenesulfonate and 10ml of a defoaming agent composition having a mass fraction of 0.05% were charged into a 1000ml measuring cylinder, the measuring cylinder was stoppered with a cork, and shaken up and down 15 times to record the foam height (V) 1 )。
Will (t) 0 -t 1 )/t 0 Defined as the defoaming value, which reflects the defoaming capability of the defoamer: the larger the defoaming value is, the better the defoaming capability of the defoaming agent is;
will (V) 0 -V 1 )/V 0 Defined as the foam inhibition value, which reflects the foam inhibition capability of the defoamer: the larger the foam inhibition value, the better the foam inhibition ability of the defoaming agent. The results of the performance evaluation tests are shown in the table4, and (2) is as follows:
TABLE 4
| Sample (I) | Stability of | Defoaming value | Foam inhibition value |
| Blank space | / | 0 | 0 |
| Example 1 | Good taste | 0.90 | 0.65 |
| Example 2 | Good taste | 0.62 | 0.30 |
| Example 3 | Good taste | 0.25 | 0.42 |
| Comparative example 1 | In general | 0.11 | 0.19 |
| Comparative example 2 | Good taste | 0.95 | 0.21 |
| Comparative example 3 | Good taste | 0.18 | 0.38 |
As can be seen from the test results in Table 3 and Table 4, the defoamer composition provided by the invention has better overall performance than the comparative example in concrete application test and foam control performance;
example 1 and comparative example 2, and example 2 and comparative example 3 demonstrate that acetylenic diols have reduced surface tension in aqueous systems and exhibit better defoaming properties; the ethoxylation group is connected into the alkyne diol molecule, so that the water solubility of the molecule can be increased, the foam control capability is improved, the foam inhibition performance is good, but the efficiency of reducing the surface tension is reduced, and the defoaming performance is poor.
The efficient concrete defoamer composition provided by the invention can fully play the synergistic effect of each component through the compounding of the defoamer, remarkably improve the defoaming capability, prevent the generation of foam, maintain excellent bubble stability, keep beneficial small bubbles and have certain foam inhibition performance.
It is obvious to those skilled in the art that the technical solutions of the present invention can still be obtained the same as or similar to the above embodiments when the technical solutions of the present invention are changed within the following ranges, and still belong to the protection scope of the present invention.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and these modifications or substitutions do not depart from the spirit of the corresponding technical solutions of the embodiments of the present invention.
Claims (9)
1. The high-efficiency concrete defoaming agent composition is characterized in that: comprises defoaming component and auxiliary defoaming component of silanes with defoaming function, foam inhibiting component composed of alkynol polyether and alkynol, and has-CH 2 CH 2 O-structural unit and-CH 2 CH 2 CH 2 An emulsifying component of an O-structural unit, a cellulose derivative with a foam stabilizing effect and an antiseptic component of isothiazolinone as an active ingredient;
wherein, the silane defoaming component has a general formula shown in the structure of formula (I):
wherein: r 1 is-CH 2 CH 2 -，-CH 2 CH 2 CH 2 -，-CH 2 CH 2 CH 2 CH 2 -one of the above; r 2 is-H, -CH 3 One of (1); a. b, c, d, e and f are integers of 2-10;
the alkynol polyether has a general formula shown as the following formula (IV):
wherein: i is an integer of 1-3, j is an integer of 2-10, and k is an integer of 2-10;
the alkynol has a general formula shown in a structure of a formula (V):
wherein:
R 3 is-H, -CH 3 One of (1);
R 4 is-H, -CH 3 ，-CH 2 CH 3 ，-CH(CH 3 ) 2 ，-CH 2 CH 2 CH 3 ，-CH 2 CH(CH 3 ) 2 ，-CH 2 CH 2 CH 2 CH 3 ，-CH 2 CH 2 CH(CH 3 ) 2 ，-CH 2 CH 2 CH 2 CH 2 CH 3 ，-CH 2 CH 2 CH 2 CH(CH 3 ) 2 One of (1);
R 5 is-H, -CH 3 ，-CH 2 CH 3 One of (1);
the composite material comprises the following components in percentage by mass:
5 to 40 percent of defoaming component, 2 to 10 percent of auxiliary defoaming component and 5 to 40 percent of foam inhibiting component consisting of alkynol polyether and alkynol;
2% -10% of a compound having-CH 2 CH 2 O-structural unit and-CH 2 CH 2 CH 2 An emulsifying component of O-building blocks;
0.2 to 2 percent of cellulose derivative with foam stabilizing function, 0.1 to 1 percent of active component which is an antiseptic component of isothiazolinone, and the balance of water;
wherein the mass ratio of the alkynol polyether to the alkynol in the foam inhibiting component is (1-10): 1.
2. The high efficiency concrete defoamer composition of claim 1, wherein: the auxiliary elimination component consists of a component with the structure shown as the following formula (II) and a component with the structure shown as the formula (III),
wherein: g is an integer from 4 to 10 and h is an integer from 5 to 9.
3. The high efficiency concrete defoamer composition of claim 2, wherein: the mass ratio of the component with the structure of the formula (II) to the component with the structure of the formula (III) in the auxiliary digestion component is (1-16): 4.
4. The high efficiency concrete defoamer composition of claim 1, wherein: the emulsifying component is formed by compounding an emulsifier A with a structure shown in the following formula (VI) and an emulsifier B with a structure shown in the following formula (VII):
C 13 H 27 O(CH 2 CH 2 O) p (CH 2 CH 2 CH 2 O) q H (Ⅵ)
C 18 H 37 O(CH 2 CH 2 O) s (CH 2 CH 2 CH 2 O) t H (Ⅶ)
wherein:
p and q are integers of 2-20, and p and q can be the same or different;
s and t are integers of 2 to 20, and s and t may be the same or different.
5. The high efficiency concrete defoamer composition of claim 4, wherein: the mass ratio of the emulsifier A to the emulsifier B is (1-16) to 4.
6. The high efficiency concrete defoamer composition of claim 1, wherein: the cellulose derivative is one of hydroxypropyl methyl cellulose, hydroxyethyl cellulose and hydroxypropyl cellulose.
7. The high efficiency concrete defoamer composition of claim 1, wherein: the anticorrosive component is formed by compounding 2-methyl-4-isothiazoline-3-ketone and 2-methyl-5-chlorine-4-isothiazoline-3-ketone.
8. The high efficiency concrete defoamer composition of claim 7, wherein: the mass ratio of the 2-methyl-4-isothiazoline-3-ketone to the 2-methyl-5-chloro-4-isothiazoline-3-ketone is (1-16) to 4.
9. A method for preparing a high efficiency concrete defoamer composition according to any one of claims 2-8, comprising the steps of:
firstly, adding 20-80% of silane defoaming component, defoaming assistant component, foam inhibiting component and emulsifying component into a reactor for premixing;
step two, raising the temperature to 65-70 ℃, controlling the stirring speed to be 500-1000rpm, and continuously stirring for 15-30 min;
step three, increasing the stirring speed of the stirrer to 3000-4000rpm, then adding the cellulose derivative, the water and the rest emulsified components into the reactor, and continuing stirring for 30-60 min; cooling to room temperature, and adding antiseptic to obtain the final product.
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| CN101780383A (en) * | 2009-12-07 | 2010-07-21 | 江苏赛欧信越消泡剂有限公司 | Aqueous emulsion non-silicon defoamer and preparation method thereof |
| CN102160939A (en) * | 2011-03-02 | 2011-08-24 | 江苏斯德瑞克化工有限公司 | Self-emulsifying molecular antifoaming agent and preparation method thereof |
| CN103897628A (en) * | 2012-12-28 | 2014-07-02 | 南通市晗泰化工有限公司 | Polyether modified organic silicon defoaming agent and its preparation method |
-
2020
- 2020-10-23 CN CN202011150230.8A patent/CN112707675B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4626559A (en) * | 1985-04-22 | 1986-12-02 | Pep Rally Paint, Inc. | Non-permanent ornamental paint mixture |
| CN101780383A (en) * | 2009-12-07 | 2010-07-21 | 江苏赛欧信越消泡剂有限公司 | Aqueous emulsion non-silicon defoamer and preparation method thereof |
| CN102160939A (en) * | 2011-03-02 | 2011-08-24 | 江苏斯德瑞克化工有限公司 | Self-emulsifying molecular antifoaming agent and preparation method thereof |
| CN103897628A (en) * | 2012-12-28 | 2014-07-02 | 南通市晗泰化工有限公司 | Polyether modified organic silicon defoaming agent and its preparation method |
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Address after: 571900 the north side of the south 2nd Ring Road of Laocheng Economic Development Zone, Chengmai County, Hainan Province Applicant after: Kezhijie new material group (Hainan) Co.,Ltd. Applicant after: KZJ NEW MATERIALS GROUP Co.,Ltd. Address before: 571900 north of the South Second Ring Road, Laocheng Economic Development Zone, Chengmai County, Sanya City, Hainan Province Applicant before: Kezhijie new material group (Hainan) Co.,Ltd. Applicant before: KZJ NEW MATERIALS GROUP Co.,Ltd. |
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