CN113548826B - Antifreezing alkali-free liquid accelerator and preparation method thereof - Google Patents
Antifreezing alkali-free liquid accelerator and preparation method thereof Download PDFInfo
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- CN113548826B CN113548826B CN202110983194.1A CN202110983194A CN113548826B CN 113548826 B CN113548826 B CN 113548826B CN 202110983194 A CN202110983194 A CN 202110983194A CN 113548826 B CN113548826 B CN 113548826B
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- free liquid
- liquid accelerator
- aluminum sulfate
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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
- C04B2103/10—Accelerators; Activators
- C04B2103/12—Set accelerators
-
- 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
- C04B2103/60—Agents for protection against chemical, physical or biological attack
- C04B2103/601—Agents for increasing frost resistance
Abstract
The invention provides an antifreezing alkali-free liquid accelerator, which is prepared by the following method: taking hydrophilic fumed silica, uniformly dispersing the hydrophilic fumed silica in water, adding iminodisuccinic acid or salt thereof, aluminum sulfate and pseudo-boehmite, stirring for at least 30min, adding ethylene glycol, triisopropanolamine, alkylbenzene sulfonate and lignosulfonate after stirring, uniformly mixing the materials, and adjusting the pH value of the whole system to 6-8. The antifreezing alkali-free liquid accelerator can accelerate the initial setting and final setting of concrete and increase the 1d compressive strength and the retention rate of the later compressive strength of set cement.
Description
Technical Field
The invention belongs to the technical field of concrete auxiliaries, and particularly relates to an antifreezing alkali-free liquid accelerator and a method for preparing the antifreezing alkali-free liquid accelerator.
Background
In recent years, the sprayed concrete is widely applied to urban construction and road construction engineering in China, particularly railways and highways in western regions in China, because of mountains in western regions, a large number of tunnels can be built in the construction process, the sprayed concrete is required to have high initial setting and final setting speeds, meanwhile, the 1d compressive strength of the sprayed concrete is as high as possible, and the loss rate of the subsequent compressive strength is as low as possible.
The accelerator is an indispensable key material in sprayed concrete, the accelerators are alkali accelerators and alkali-free accelerators, and at present, the alkali-free liquid accelerator is the main development direction of the accelerator. The method has the advantages of friendly construction environment, little harm to construction workers and reduction of alkali aggregate reaction. The existing alkali-free liquid accelerator has the problem of reducing the later strength of the set cement, and meanwhile, the concrete doped with the existing alkali-free liquid accelerator still needs to improve the setting speed and the 1d strength at low temperature.
Disclosure of Invention
In order to solve the problems, the invention provides an anti-freezing alkali-free liquid accelerator which is short in initial setting time and final setting time and high in later strength.
The technical scheme of the invention is as follows: an anti-freezing alkali-free liquid accelerator comprises, by weight, 15-30 parts of aluminum sulfate, 5-15 parts of pseudo-boehmite, 1-5 parts of iminodisuccinic acid or a salt thereof, 0.5-1 part of triisopropanolamine, 4-10 parts of ethylene glycol, 2-5 parts of alkylbenzene sulfonate, 1-4 parts of hydrophilic fumed silica, 2-5 parts of lignosulfonate and 100 parts of water, wherein the aluminum sulfate is calculated as the anhydrous aluminum sulfate, namely the water in the hydrated aluminum sulfate is discharged, and the calculation is based on the anhydrous aluminum sulfate alone, for example, for the octadecahydrated aluminum sulfate, according to the calculation method of the invention: w ═ W (W/666.43) × 342.15, where W is the weight of aluminum sulfate calculated as anhydrous aluminum sulfate, W is the weight of aluminum sulfate octadecahydrate, 666.43 is the molar mass of aluminum sulfate octadecahydrate, and 342.15 is the molar mass of anhydrous aluminum sulfate.
In one embodiment of the present invention, the aluminum sulfate is one of polyaluminum sulfate, anhydrous aluminum sulfate, and aluminum sulfate octadecahydrate.
In one embodiment of the present invention, the iminodisuccinate is tetrasodium iminodisuccinate.
In one embodiment of the present invention, the lignosulfonate is sodium lignosulfonate.
In one embodiment of the present invention, the alkyl chain of the alkylbenzene sulfonate is a linear alkane having a chain length of 10 to 20, and alkylbenzene sulfonates in this range have a good effect of increasing the strength of concrete, and are preferably sodium dodecylbenzenesulfonate.
Preferably, the aluminum sulfate-based water treatment agent comprises, by weight, 18-25 parts of aluminum sulfate, 8-10 parts of pseudo-boehmite, 1-3 parts of iminodisuccinic acid or salts thereof, 0.6-0.8 part of triisopropanolamine, 5-8 parts of ethylene glycol, 3-3.5 parts of alkylbenzene sulfonate, 2-3 parts of hydrophilic fumed silica, 3.5-5 parts of lignosulfonate and 100 parts of water.
The invention also aims to provide a method for preparing the antifreezing alkali-free liquid accelerator, which comprises the following steps: taking hydrophilic fumed silica, uniformly dispersing the hydrophilic fumed silica in water, adding iminodisuccinic acid or salt thereof, aluminum sulfate and pseudo-boehmite, stirring for at least 30min, wherein the stirring speed is basically not required, but preferably 100-200r/min, adding ethylene glycol, triisopropanolamine, alkylbenzene sulfonate and lignosulfonate after stirring, uniformly mixing, and then adjusting the pH of the whole system to 6-8.
The antifreezing alkali-free liquid accelerator adopts aluminum sulfate and pseudo-boehmite as main agents of the accelerator, and has good accelerating effect; the selected iminodisuccinic acid or the salt thereof has a good complexing effect on aluminum ions, and meanwhile, the complexing degree of the iminodisuccinic acid or the salt thereof on calcium ions is greater than that of the iminodisuccinic acid on aluminum ions, so that after the antifreezing alkali-free liquid accelerator disclosed by the invention is contacted with cement, the iminodisuccinic acid aluminum can be quickly changed into iminodisuccinic acid calcium and aluminum ions are released, and the coagulation accelerating effect of the whole system is accelerated; triisopropanolamine can increase the stability of the accelerator, and after the concrete is added, the strength of the set cement can be enhanced; the glycol and the alkylbenzene sulfonate can improve the frost resistance of the whole system, so that the concrete can be still coagulated at a coagulation speed meeting the standard at the temperature of-20 ℃, and meanwhile, the later strength of the concrete is not influenced; the hydrophilic fumed silica and lignosulfonate can increase the strength of the whole system.
The invention has the beneficial effects that:
according to the antifreezing alkali-free liquid accelerator, the iminodisuccinic acid or the salt thereof is used as a stabilizer of aluminum ions, the stabilizer has good selectivity, the complexing degree of calcium ions is greater than that of aluminum ions, and after the antifreezing alkali-free liquid accelerator is added into concrete, aluminum ions are released from the iminodisuccinic acid, so that the initial setting speed and the final setting speed of the concrete are accelerated; hydrophilic fumed silica and lignosulfonate are added at the same time, so that the later strength of the set cement can be improved; the freezing resistance of the whole system can be increased by adding glycol and alkylbenzene sulfonate.
Detailed Description
In order to make the technical solutions and technical advantages of the present invention clearer, the following will clearly and completely describe the technical solutions in the implementation process of the present invention with reference to the embodiments.
The present invention will be further illustrated by the following specific examples.
The reagents in the following examples are all commercially pure unless otherwise specified.
In the following examples, the parts are by weight.
Example 1
Taking 3 parts of hydrophilic fumed silica, uniformly dispersing the hydrophilic fumed silica in 100 parts of water by ultrasonic treatment for 5min, adding 3 parts of iminodisuccinic acid, 22 parts of anhydrous aluminum sulfate and 8 parts of pseudo-boehmite, continuously stirring for 30min at the speed of 100r/min, continuously adding 7 parts of ethylene glycol, 0.8 part of triisopropanolamine, 3 parts of sodium dodecyl benzene sulfonate and 4 parts of sodium lignin sulfonate after stirring is finished, uniformly mixing all materials by stirring, and adjusting the pH value of the system to 7 to obtain the anti-freezing alkali-free liquid accelerator F1.
Example 2
Taking 3 parts of hydrophilic fumed silica, uniformly dispersing the hydrophilic fumed silica in 100 parts of water by ultrasonic treatment for 5min, adding 2 parts of iminodisuccinic acid, 50 parts of aluminum sulfate octadecahydrate and 8 parts of pseudo-boehmite, continuously stirring for 30min under the condition of 100r/min, after stirring is finished, continuously adding 5 parts of ethylene glycol, 0.8 part of triisopropanolamine, 3 parts of sodium dodecyl benzene sulfonate and 5 parts of sodium lignin sulfonate, stirring to uniformly mix all the materials, and adjusting the pH value of the system to 7 to obtain the anti-freezing alkali-free liquid accelerator F2.
Example 3
Taking 3 parts of hydrophilic fumed silica, uniformly dispersing the hydrophilic fumed silica in 100 parts of water by ultrasonic treatment for 5min, adding 5 parts of iminodisuccinic acid, 18 parts of anhydrous aluminum sulfate and 8 parts of pseudo-boehmite, continuously stirring for 30min under the condition of 100r/min, after stirring is finished, continuously adding 5 parts of ethylene glycol, 0.8 part of triisopropanolamine, 3 parts of sodium dodecyl benzene sulfonate and 5 parts of sodium lignin sulfonate, stirring to uniformly mix all the materials, and adjusting the pH value of the system to 7 to obtain the anti-freezing alkali-free liquid accelerator F3.
Example 4
Taking 3 parts of hydrophilic fumed silica, uniformly dispersing the hydrophilic fumed silica in 100 parts of water by ultrasonic treatment for 5min, adding 3 parts of iminodisuccinic acid, 15 parts of anhydrous aluminum sulfate and 14 parts of pseudo-boehmite, continuously stirring for 30min under the condition of 100r/min, after stirring is finished, continuously adding 5 parts of ethylene glycol, 0.8 part of triisopropanolamine, 3 parts of sodium dodecyl benzene sulfonate and 5 parts of sodium lignin sulfonate, stirring to uniformly mix all the materials, and adjusting the pH value of the system to 7 to obtain the anti-freezing alkali-free liquid accelerator F4.
Example 5
Taking 1 part of hydrophilic fumed silica, uniformly dispersing the hydrophilic fumed silica in 100 parts of water by ultrasonic treatment for 5min, adding 3 parts of iminodisuccinic acid, 22 parts of anhydrous aluminum sulfate and 8 parts of pseudo-boehmite, continuously stirring for 30min under the condition of 100r/min, after stirring is finished, continuously adding 7 parts of ethylene glycol, 0.8 part of triisopropanolamine, 3 parts of sodium dodecyl benzene sulfonate and 2 parts of sodium lignin sulfonate, stirring to uniformly mix all the materials, and adjusting the pH value of the system to 7 to obtain the anti-freezing alkali-free liquid accelerator F5.
Comparative example 1
Taking 3 parts of hydrophilic fumed silica, uniformly dispersing the hydrophilic fumed silica in 100 parts of water by ultrasonic treatment for 5min, adding 3 parts of citric acid, 22 parts of anhydrous aluminum sulfate and 8 parts of pseudo-boehmite, continuously stirring for 30min under the condition of 100r/min, continuously adding 7 parts of ethylene glycol, 0.8 part of triisopropanolamine, 3 parts of sodium dodecyl benzene sulfonate and 4 parts of sodium lignin sulfonate after stirring is finished, stirring to uniformly mix all the materials, and adjusting the pH value of the system to 7 to obtain the antifreezing alkali-free liquid accelerator D1.
Comparative example 2
Taking 3 parts of hydrophilic fumed silica, performing ultrasonic treatment for 5min to uniformly disperse the hydrophilic fumed silica in 100 parts of water, adding 3 parts of iminodisuccinic acid, 22 parts of anhydrous aluminum sulfate and 8 parts of pseudo-boehmite, uniformly mixing, continuously adding 7 parts of ethylene glycol, 0.8 part of triisopropanolamine, 3 parts of sodium dodecyl benzene sulfonate and 4 parts of sodium lignin sulfonate, stirring to uniformly mix all the materials, and adjusting the pH value of the system to 7 to obtain the antifreezing alkali-free liquid accelerator D2. After successful preparation, a few flocs were found in the whole system and after some time, a small amount of precipitation occurred.
Comparative example 3
Taking 3 parts of hydrophilic fumed silica, uniformly dispersing the hydrophilic fumed silica in 100 parts of water by ultrasonic treatment for 5min, adding 3 parts of iminodisuccinic acid, 22 parts of anhydrous aluminum sulfate and 8 parts of pseudo-boehmite, continuously stirring for 30min under the condition of 100r/min, continuously adding 0.8 part of triisopropanolamine and 4 parts of sodium lignosulfonate after stirring is finished, uniformly mixing all the materials by stirring, and adjusting the pH value of the system to 7 to obtain the antifreezing alkali-free liquid accelerator D3.
In order to further explain the effects of the present invention, various experiments are used to explain the performance of the present invention.
1. Setting time and compressive strength
The test is carried out by adopting reference cement according to GB/T35159 and 2017 accelerator for concrete for spraying. In the measuring process, the cement is used as reference cement, and the sand is used as standard sand.
TABLE 1 test results at a test temperature of 20. + -. 1 ℃ C
TABLE 2 test results at-20. + -. 1 ℃ test temperature
In Table 2, "__" indicates that the value is far beyond the specification of GB/T35159 and 2017 for the accelerator.
As can be seen from tables 1 and 2, as for the antifreezing alkali-free liquid accelerator F1-F2, the proportion of each component is relatively excellent, so that the initial setting time and the final setting time are far better than the specification of GB/T35159-2017 on the setting time of concrete added with the antifreezing alkali-free liquid accelerator, and at the same time, the antifreezing alkali-free liquid accelerator can still meet the specification of GB/T35159-2017 at the temperature of-20 ℃; meanwhile, the 1d compressive strength is higher, the compressive strength retention rate in the subsequent process still exceeds the specification of GB/T35159-2017, and F1 and F2 still have higher strength even under the condition of-20 ℃; the comprehensive performance of the anti-freezing alkali-free liquid accelerator is far superior to that of the existing anti-freezing alkali-free liquid accelerator. Even for the antifreezing alkali-free liquid accelerator J3-J5 which is not in the preferred range of the invention, the effect still meets the regulation of GB/T35159-2017 and is superior to most of the antifreezing alkali-free liquid accelerators at present.
Compared with F1, D1 is obtained by replacing iminodisuccinic acid with citric acid which is commonly used in the market at present, and the citric acid also has certain complexing and stabilizing effects on aluminum ions, so that the D1 is also a stabilizer which is commonly used in the accelerator at present. However, as can be seen from the results in Table 1, both the setting rate and the compressive strength are significantly lower than D1, indicating that citric acid is far less effective than iminodisuccinic acid.
Compared with F1, D2 has the advantages that after raw materials such as anhydrous aluminum sulfate are added, the raw materials are not fully stirred, so that the complexing effect of the iminodisuccinic acid on aluminum ions is not obvious, the added iminodisuccinic acid does not exert the complexing effect, and the coagulation speed and the compression resistance are obviously lower than those of D1.
For D3, compared with F1, no ethylene glycol or sodium dodecylbenzenesulfonate was added to D3, which resulted in poor freezing resistance.
In conclusion, the mixing amount of the antifreezing alkali-free liquid accelerator of examples 1-5 is 4%, the requirement of GB/T35159-; when the anti-freezing alkali-free liquid accelerator faces a severe temperature environment of-20 ℃, the doping amount is only required to be increased to 7 percent, and the effect of the accelerator meets the regulation of GB/T35159 and 2017 and is far superior to the prior anti-freezing alkali-free liquid accelerator.
Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (6)
1. An anti-freezing alkali-free liquid accelerator is characterized by comprising, by weight, 15-30 parts of aluminum sulfate, 5-15 parts of pseudo-boehmite, 1-5 parts of iminodisuccinic acid or a salt thereof, 0.5-1 part of triisopropanolamine, 4-10 parts of ethylene glycol, 2-5 parts of alkylbenzene sulfonate, 1-4 parts of hydrophilic fumed silica, 2-5 parts of lignosulfonate and 100 parts of water, wherein the aluminum sulfate is calculated by the anhydrous aluminum sulfate; the preparation method of the antifreezing alkali-free liquid accelerator comprises the following steps:
taking hydrophilic fumed silica, uniformly dispersing the hydrophilic fumed silica in water, adding iminodisuccinic acid or salt thereof, aluminum sulfate and pseudo-boehmite, stirring for at least 30min, adding ethylene glycol, triisopropanolamine, alkylbenzene sulfonate and lignosulfonate after stirring is finished, stirring to uniformly mix, and adjusting the pH value of the whole system to 6-8.
2. The antifreeze alkali-free liquid accelerator as set forth in claim 1, wherein the aluminum sulfate is one of polyaluminum sulfate, anhydrous aluminum sulfate, aluminum sulfate octadecahydrate.
3. The antifreeze alkali-free liquid accelerator according to claim 1, wherein the iminodisuccinate is tetrasodium iminodisuccinate.
4. The antifreeze alkali-free liquid accelerator according to claim 1, wherein the lignosulfonate is sodium lignosulfonate.
5. The antifreeze alkali-free liquid accelerator according to claim 1, wherein the alkyl chain of the alkylbenzene sulfonate is a linear alkane having a chain length of 10 to 20.
6. The antifreeze alkali-free liquid accelerator as set forth in any one of claims 1 to 5, which comprises, in parts by weight, 18 to 25 parts of aluminum sulfate, 8 to 10 parts of pseudo boehmite, 1 to 3 parts of iminodisuccinic acid or a salt thereof, 0.6 to 0.8 part of triisopropanolamine, 5 to 8 parts of ethylene glycol, 3 to 3.5 parts of an alkylbenzene sulfonate, 2 to 3 parts of hydrophilic fumed silica, 3.5 to 5 parts of a lignin sulfonate, and 100 parts of water.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| ES2327924T3 (en) * | 2003-02-25 | 2009-11-05 | CONSTRUCTION RESEARCH & TECHNOLOGY GMBH | ACCELERATING MIX |
| CN103553406A (en) * | 2013-09-27 | 2014-02-05 | 中国建筑材料科学研究总院 | Alkali and chlorine-free liquid setting accelerator based on industrial polyaluminium sulfate and its preparation method |
| CN109678388A (en) * | 2019-01-29 | 2019-04-26 | 新疆中材精细化工有限责任公司 | A kind of antifreeze alkali-free liquid accelerating agent and preparation method thereof |
| CN111265993A (en) * | 2020-01-15 | 2020-06-12 | 四川西油致诚石油技术有限公司 | Complex iron desulfurizer |
| CN113121146A (en) * | 2021-04-16 | 2021-07-16 | 厦门欣润岩新材料有限公司 | Alkali-free accelerator and preparation method thereof |
-
2021
- 2021-08-25 CN CN202110983194.1A patent/CN113548826B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| ES2327924T3 (en) * | 2003-02-25 | 2009-11-05 | CONSTRUCTION RESEARCH & TECHNOLOGY GMBH | ACCELERATING MIX |
| CN103553406A (en) * | 2013-09-27 | 2014-02-05 | 中国建筑材料科学研究总院 | Alkali and chlorine-free liquid setting accelerator based on industrial polyaluminium sulfate and its preparation method |
| CN109678388A (en) * | 2019-01-29 | 2019-04-26 | 新疆中材精细化工有限责任公司 | A kind of antifreeze alkali-free liquid accelerating agent and preparation method thereof |
| CN111265993A (en) * | 2020-01-15 | 2020-06-12 | 四川西油致诚石油技术有限公司 | Complex iron desulfurizer |
| CN113121146A (en) * | 2021-04-16 | 2021-07-16 | 厦门欣润岩新材料有限公司 | Alkali-free accelerator and preparation method thereof |
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