CN110713357A - Liquid alkali-free accelerator and preparation method thereof - Google Patents

Liquid alkali-free accelerator and preparation method thereof Download PDF

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Publication number
CN110713357A
CN110713357A CN201911164847.2A CN201911164847A CN110713357A CN 110713357 A CN110713357 A CN 110713357A CN 201911164847 A CN201911164847 A CN 201911164847A CN 110713357 A CN110713357 A CN 110713357A
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China
Prior art keywords
liquid alkali
free
accelerator
free accelerator
alkali
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CN201911164847.2A
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Chinese (zh)
Inventor
陈世学
刘允伟
邹锋
廖思淘
陈华君
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Sichuan Yu Concrete Building Materials Co Ltd
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Sichuan Yu Concrete Building Materials Co Ltd
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Priority to CN201911164847.2A priority Critical patent/CN110713357A/en
Publication of CN110713357A publication Critical patent/CN110713357A/en
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B40/00Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
    • C04B40/0028Aspects relating to the mixing step of the mortar preparation
    • C04B40/0039Premixtures of ingredients
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2103/00Function or property of ingredients for mortars, concrete or artificial stone
    • C04B2103/10Accelerators; Activators
    • C04B2103/12Set accelerators

Abstract

The application relates to the field of concrete admixtures, in particular to a liquid alkali-free accelerator and a preparation method thereof. The liquid alkali-free accelerator is prepared by passing high-concentration Al3+The concentration forms a complex, the setting speed of the concrete is obviously improved, and in addition, F passes throughAnd increasing high concentration of Al3+The solution is stable and the early strength of the concrete is enhanced by other additives. The liquid alkali-free accelerator can greatly improve the workability of concrete under the condition of low doping amount meeting the detection standard, and has the advantages of easily obtained raw materials, convenient production, small doping amount and no pollution in production, thereby having good economic value and environmental protection value.

Description

Liquid alkali-free accelerator and preparation method thereof
Technical Field
The application relates to the field of concrete admixtures, in particular to a liquid alkali-free accelerator and a preparation method thereof.
Background
The liquid alkali-free accelerator is an additive used for sprayed concrete, and can obviously shorten the setting and hardening time of the concrete. Compared with the traditional alkaline powder and alkaline liquid accelerating agent, the alkaline content of the accelerating agent is almost zero and no Cl is generated-The pH value is 3.0-5.0, and the construction can be effectively reducedThe alkali-free liquid accelerator has the advantages of fully dispersing in the mixture, low dust concentration in air during construction, improving the strength of sprayed concrete and avoiding the large fluctuation of the quality of the sprayed concrete, and thus gradually replaces the traditional accelerator in the existing market.
The liquid alkali-free accelerator in the prior market is usually prepared by reacting and mixing sulphoaluminate and other additives, solvents and auxiliaries, wherein Al is3+The content of (a) substantially determines the performance of the liquid alkali-free accelerator. Therefore, the technical development direction in the market is: the stable high Al is prepared under the premise of low cost and low pollution3+The concentrated liquid alkali-free accelerator also has to have good adaptability with cement common in the market.
Disclosure of Invention
The invention provides a liquid alkali-free accelerator which is characterized by comprising the following components: fluoride, organic amine, silica sol, sulphoaluminate, amide and water; wherein the fluoride is AlF 3.
Further, the organic amine is (HOCH2CH2)2NH and/or (HOCH2CH2)3N, and the mass percent of the organic amine in the liquid alkali-free accelerator is 5-8%.
Further, the sulphoaluminate is Al2(SO4)3, and the mass percentage of the sulphoaluminate in the liquid alkali-free accelerator is 35-38%.
Further, the amide is polyacrylamide, and the mass percent of the amide in the liquid alkali-free accelerator is 0.01-0.03%; the molecular weight of the polyacrylamide is 150-250 ten thousand.
Further, the mass percent of the silica sol in the liquid alkali-free setting accelerator is 0.1-0.2%, and the mass percent of the fluoride in the liquid alkali-free setting accelerator is 6-8%.
The application also provides a preparation method of the liquid alkali-free accelerator, which comprises the following steps:
1) adding H2O into a reaction container, and adding fluoride while stirring;
2) adding organic amine and silica sol;
3) adding an amide;
4) adding sulphoaluminate.
Further, the reaction time of the step 1) is 25-35 min.
Further, the reaction time of the step 2) is 35-45 min.
Further, the reaction time of the step 3) is 15-25 min.
Further, the reaction time of the step 4) is 4-5 h; and 4) observing whether the product is clear and transparent without precipitates after the step 4) is finished, and if not, continuing to react for 30 min.
The liquid alkali-free accelerator contains high-concentration Al3+By means of high concentrations of Al in the case of low doping levels3+The setting speed of concrete can be obviously improved, the use of the liquid alkali-free accelerator can obviously increase the early strength and the hourly strength increasing rate of the concrete, and the concrete using the liquid alkali-free accelerator also has the advantages of low rebound and no strength loss after the rebound, and meets the standard requirement of GBT 35159-2017. The preparation method of the liquid alkali-free accelerator adopts common materials, the reaction heat release can make the reaction process spontaneously proceed under the action of organic amine, and external heating or pressurization is not needed, so that the preparation method has the advantages of low cost and simple process, and in addition, no waste gas and waste water are generated in the preparation process, so the preparation method also has the advantages of environmental protection and no pollution.
Detailed Description
In order that those skilled in the art will better understand the technical solutions of the present invention, the present invention will be further described in detail with reference to the following embodiments.
The invention provides a liquid alkali-free accelerator, which is an additive in concrete accelerators and is mainly divided into a split accelerator and a liquid accelerator according to the physical state of the accelerator, and the liquid alkali-free accelerator can be further divided into a basic accelerator, a low-alkali accelerator and an alkali-free accelerator according to the alkalinity of the accelerator. The liquid alkali-free accelerator is a concrete accelerator which is liquid at normal temperature and normal pressure and has the pH value less than or equal to 7. The liquid alkali-free accelerator is mainly used as an additive of concrete in general, can remarkably improve the setting speed of the concrete, reduce the early strength of the concrete during setting, increase the hourly strength increasing rate, and has the advantages of low rebound and no strength loss after the concrete uses the liquid alkali-free accelerator.
The liquid alkali-free accelerator comprises the following components: fluoride, organic amine, silica sol, sulphoaluminate, amide and water; wherein the fluoride is AlF3Wherein the fluoride is AlF3
Liquid alkali-free accelerator as described herein vs. solvent H2O has no special requirement, common qualified tap water can be directly adopted in the actual use, the performance of the finished product of the liquid alkali-free accelerator can be met by adopting the common qualified tap water, and the production cost and the raw material acquisition difficulty of the liquid alkali-free accelerator can be obviously reduced by using the tap water. Specifically, the organic amine is (HOCH)2CH2)2NH and/or (HOCH)2CH2)3N, the sulphoaluminate is Al2(SO4)3The amide is polyacrylamide, the molecular weight of the polyacrylamide is 150-250 ten thousand, and polyacrylamide with the molecular weight of 200 ten thousand is preferably adopted. The fluoride, the organic amine, the sulphoaluminate and the amide all adopt common commodities on the market.
Specifically, the liquid alkali-free accelerator comprises the following substances in percentage by mass:
the invention also provides a preparation method of the liquid alkali-free accelerator, which comprises the following steps:
1) adding H2O into the reaction container, adding fluoride while stirring, and reacting for 25-35 min;
2) adding organic amine and silica sol, and reacting for 35-45 min;
3) adding amide, and stirring for 15-25 min;
4) adding sulphoaluminate and reacting for 4-5 h.
And 4) observing whether the product is clear and transparent without precipitates after the step 4), if so, obtaining a finished product of the liquid alkali-free accelerator, and if not, continuing to react for 30min to obtain the finished product of the liquid alkali-free accelerator.
Example 1
The specific formulation of this embodiment is as follows, and it should be noted that the values in the following table are mass percentages of the substance in the liquid alkali-free setting accelerator, and the balance in each embodiment is water:
examples Fluoride compounds Organic amine Silica sol Thioaluminate salts Amides of carboxylic acids
Examples 1 to 1 6 6.5 0.15 36.5 0.02
Examples 1 to 2 7 6.5 0.15 36.5 0.02
Examples 1 to 3 8 6.5 0.15 36.5 0.02
The liquid alkali-free setting accelerator in the embodiment is prepared by the preparation method of the liquid alkali-free setting accelerator.
The liquid alkali-free accelerator in the embodiment is added into conventional cement in an addition amount of 9%, the conventional cement is common cement which can be purchased in the market, the type of the cement adopted in the experiment is conch P.O42.5R, and the performance is obtained by testing as follows:
Figure BDA0002287165370000051
according to the data, when the mass percent of the fluoride is 6-8%, the fluoride is added into the conventional cement by adopting the mixing amount of 9%, the setting time of the cement paste can be obviously shortened and the compressive strength of the cement mortar can be obviously enhanced through the conventional process, and when the mass percent of the fluoride is 7%, the obtained liquid alkali-free accelerator has the best comprehensive performance.
Example 2
The specific formulation of this embodiment is as follows, and it should be noted that the values in the following table are mass percentages of the substance in the liquid alkali-free setting accelerator, and the balance in each embodiment is water:
examples Fluoride compounds Organic amine Silica sol Thioaluminate salts Amides of carboxylic acids
Example 2-1 7 5 0.15 36.5 0.02
Examples 2 to 2 7 8 0.15 36.5 0.02
The liquid alkali-free setting accelerator in the embodiment is prepared by the preparation method of the liquid alkali-free setting accelerator.
The liquid alkali-free accelerator in the embodiment is added into conventional cement in an addition amount of 9%, the conventional cement is common cement which can be purchased in the market, the type of the cement adopted in the experiment is conch P.O42.5R, and the performance is obtained by testing as follows:
according to the data, when the mass percent of the organic amine is 5-8%, the organic amine is added into the conventional cement by adopting the mixing amount of 9%, and the setting time of the cement paste can be obviously shortened and the compressive strength of the cement mortar can be enhanced by the conventional process.
Example 3
The specific formula of each embodiment of the invention is as follows, and it should be noted that the numerical values in the following table are the mass percentage of the substance in the liquid alkali-free accelerator, and the balance in each embodiment is water:
examples Fluoride compounds Organic amine Silica sol Thioaluminate salts Amides of carboxylic acids
Example 3-1 7 6.5 0.1 36.5 0.02
Examples 3 to 2 7 6.5 0.2 36.5 0.02
The liquid alkali-free setting accelerator in the embodiment is prepared by the preparation method of the liquid alkali-free setting accelerator.
The liquid alkali-free accelerator in the embodiment is added into conventional cement in an addition amount of 9%, the conventional cement is common cement which can be purchased in the market, the type of the cement adopted in the experiment is conch P.O42.5R, and the performance is obtained by testing as follows:
Figure BDA0002287165370000062
Figure BDA0002287165370000071
according to the data, when the mass percent of the silica sol is 0.1-0.2%, 9% of the silica sol is added into the conventional cement, the setting time of the cement paste can be obviously shortened and the compressive strength of the cement mortar can be obviously enhanced through the conventional process, and when the mass percent of the silica sol is 0.15%, the obtained liquid alkali-free accelerator has the best comprehensive performance.
Example 4
The specific formulation of this embodiment is as follows, and it should be noted that the values in the following table are mass percentages of the substance in the liquid alkali-free setting accelerator, and the balance in each embodiment is water:
examples Fluoride compounds Organic amine Silica sol Thioaluminate salts Amides of carboxylic acids
Example 4-1 7 6.5 0.15 35 0.02
Example 4 to 2 7 6.5 0.15 38 0.02
The liquid alkali-free setting accelerator in the embodiment is prepared by the preparation method of the liquid alkali-free setting accelerator.
The liquid alkali-free accelerator in the embodiment is added into conventional cement in an addition amount of 9%, the conventional cement is common cement which can be purchased in the market, the type of the cement adopted in the experiment is conch P.O42.5R, and the performance is obtained by testing as follows:
Figure BDA0002287165370000081
according to the data, when the mass percent of the sulphoaluminate is 5-8%, the sulphoaluminate is added into the conventional cement by adopting the mixing amount of 9%, and the setting time of the cement paste can be obviously shortened and the compressive strength of the cement mortar can be enhanced by the conventional process.
EXAMPLE five
The specific formulation of this embodiment is as follows, and it should be noted that the values in the following table are mass percentages of the substance in the liquid alkali-free setting accelerator, and the balance in each embodiment is water:
examples Fluoride compounds Organic amine Silica sol Thioaluminate salts Amides of carboxylic acids
Example 5-1 7 6.5 0.15 36.5 0.01
Examples 5 and 2 7 6.5 0.15 36.5 0.03
The liquid alkali-free setting accelerator in the embodiment is prepared by the preparation method of the liquid alkali-free setting accelerator.
The liquid alkali-free accelerator in the embodiment is added into conventional cement in an addition amount of 9%, the conventional cement is common cement which can be purchased in the market, the type of the cement adopted in the experiment is conch P.O42.5R, and the performance is obtained by testing as follows:
according to the data, when the mass percent of the amide is 5-8%, the amide is added into the conventional cement by adopting the mixing amount of 9%, and the setting time of the cement paste can be obviously shortened and the compressive strength of the cement mortar can be enhanced by the conventional process.
Through the embodiment, the liquid alkali-free accelerator with relatively excellent comprehensive performance can be obtained when the components of the liquid alkali-free accelerator take the intermediate values of the mass percentages, and the liquid alkali-free accelerator obtained when any component (except water) takes any numerical value in the mass percentage range can still meet the actual performance requirement when other components take the intermediate values of the mass percentages.
Example 6
The liquid alkali-free accelerator described in this embodiment comprises the following components in percentage by mass:
fluoride: 7 percent;
organic amine: 6.5 percent;
0.15% of silica sol;
sulphoaluminate salt: 36.5 percent;
amide: 0.02 percent;
the balance being water.
The liquid alkali-free setting accelerator in the embodiment is prepared by the preparation method of the liquid alkali-free setting accelerator. The liquid alkali-free accelerator in the embodiment is added into several kinds of common cement in the market according to different mixing amounts, and the detection data obtained by the same process and detection method are as follows:
Figure BDA0002287165370000091
the liquid alkali-free accelerator contains high-concentration Al3+By means of high concentrations of Al in the case of low doping levels3+The setting speed of concrete can be obviously improved, the use of the liquid alkali-free accelerator can obviously increase the early strength and the hourly strength increasing rate of the concrete, and the concrete using the liquid alkali-free accelerator also has the advantages of low rebound and no strength loss after the rebound, and meets the standard requirement of GBT 35159-2017. The preparation method of the liquid alkali-free accelerator adopts common materials, and under the action of organic amine, the reaction heat release enables the reaction process to be carried out spontaneously, and external heating or pressurization is not needed, so that the preparation method has the advantages of low cost and simple process, and in addition, no waste gas or waste water is generated in the preparation process, so the preparation method also has the advantages of environmental protection and no pollution.
The same and similar parts among the various embodiments in the specification of the present application may be referred to each other. Especially, for the system and terminal embodiments, since the method therein is basically similar to the method embodiments, the description is relatively simple, and the relevant points can be referred to the description in the method embodiments.
Of course, the above description is not limited to the above examples, and technical features that are not described in this application may be implemented by or using the prior art, and are not described herein again; the above examples are merely illustrative of the technical solutions of the present application and are not intended to limit the present application, and the present application is only described in detail with reference to the preferred embodiments, and those skilled in the art should understand that changes, additions or substitutions which are made by those skilled in the art within the spirit of the present application are also within the scope of the claims of the present application.

Claims (10)

1. A liquid alkali-free accelerator which is characterized by comprising the following components: fluoride, organic amine, silica sol, sulphoaluminate, amide and water; wherein the fluoride is AlF3
2. The liquid alkali-free accelerator according to claim 1, wherein the organic amine is (HOCH)2CH2)2NH and/or (HOCH)2CH2)3And N accounts for 5-8% of the liquid alkali-free accelerator.
3. The liquid alkali-free accelerator according to claim 1, wherein the thioaluminate is Al2(SO4)3The mass percentage of the alkali-free accelerator in the liquid alkali-free accelerator is 35-38%.
4. The liquid alkali-free accelerator according to claim 1, wherein the amide is polyacrylamide, and the mass percent of the amide in the liquid alkali-free accelerator is 0.01-0.03%; the molecular weight of the polyacrylamide is 150-250 ten thousand.
5. The liquid alkali-free setting accelerator according to claim 1, wherein the silica sol is present in the liquid alkali-free setting accelerator in an amount of 0.1 to 0.2% by mass, and the fluoride is present in the liquid alkali-free setting accelerator in an amount of 6 to 8% by mass.
6. A method for preparing a liquid alkali-free accelerator, which is the liquid alkali-free accelerator described in any one of claims 1 to 5, comprises the following steps:
1) adding H into a reaction vessel2O, adding fluoride while stirring;
2) adding organic amine and silica sol;
3) adding an amide;
4) adding sulphoaluminate.
7. The method for producing a liquid alkali-free accelerator according to claim 6, characterized in that: the reaction time of the step 1) is 25-35 min.
8. The method for producing a liquid alkali-free accelerator according to claim 6, characterized in that: the reaction time of the step 2) is 35-45 min.
9. The method for producing a liquid alkali-free accelerator according to claim 6, characterized in that: the reaction time of the step 3) is 15-25 min.
10. The method for producing a liquid alkali-free accelerator according to claim 6, characterized in that: the reaction time of the step 4) is 4-5 h; and 4) observing whether the product is clear and transparent without precipitates after the step 4) is finished, and if not, continuing to react for 30 min.
CN201911164847.2A 2019-11-25 2019-11-25 Liquid alkali-free accelerator and preparation method thereof Pending CN110713357A (en)

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Publication number Priority date Publication date Assignee Title
CN102219425A (en) * 2011-04-15 2011-10-19 中铁隧道集团有限公司 Alkali-free liquid accelerating agent and preparation method thereof
CN105174790A (en) * 2015-08-31 2015-12-23 仇鹏 Alkaline-free liquid cement accelerator and using method therefor
CN107337374A (en) * 2017-07-15 2017-11-10 王宇青 Fluorine-containing alkali-free liquid accelerator
CN110128044A (en) * 2019-04-09 2019-08-16 湖北工业大学 A kind of alkali-free liquid accelerator preparation method

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102219425A (en) * 2011-04-15 2011-10-19 中铁隧道集团有限公司 Alkali-free liquid accelerating agent and preparation method thereof
CN105174790A (en) * 2015-08-31 2015-12-23 仇鹏 Alkaline-free liquid cement accelerator and using method therefor
CN107337374A (en) * 2017-07-15 2017-11-10 王宇青 Fluorine-containing alkali-free liquid accelerator
CN110128044A (en) * 2019-04-09 2019-08-16 湖北工业大学 A kind of alkali-free liquid accelerator preparation method

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Application publication date: 20200121