CN113716889A - Fluorine-free antifreezing liquid alkali-free setting accelerator and preparation method thereof - Google Patents
Fluorine-free antifreezing liquid alkali-free setting accelerator and preparation method thereof Download PDFInfo
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- CN113716889A CN113716889A CN202110956293.0A CN202110956293A CN113716889A CN 113716889 A CN113716889 A CN 113716889A CN 202110956293 A CN202110956293 A CN 202110956293A CN 113716889 A CN113716889 A CN 113716889A
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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
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- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
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Abstract
The invention discloses a fluorine-free antifreezing liquid alkali-free setting accelerator and a preparation method thereof, belonging to the technical field of building materials. The accelerator is prepared from the following raw materials in parts by weight: 20-40 parts of high-molecular coagulant, 25-45 parts of aluminum sulfate, 2-7 parts of magnesium hydroxide, 2-6 parts of alcohol amine, 0.3-1.0 part of complexing agent, 1-4 parts of antifreezing agent and 25-45 parts of water. The synthetic polymer coagulant aid is used, so that the overall performance of the accelerator can be greatly improved, the strength is improved, the setting time is reduced, hydrofluoric acid, fluosilicate and other fluorine-containing raw materials are not used, and the accelerator has no toxic or harmful effect on the ecological environment in the production and use processes. The obtained accelerator has excellent stability and can be normally applied in construction at a low temperature of more than 15 ℃ below zero.
Description
Technical Field
The invention belongs to the technical field of building materials, and particularly relates to a fluorine-free anti-freezing liquid alkali-free accelerator and a preparation method thereof.
Background
The sprayed concrete wet spraying process has the characteristics of low rebound rate, high construction efficiency and environmental friendliness, and is becoming the mainstream of actual construction operation. With the increasing of the awareness of the environmental protection of human beings and the improvement of the requirement of underground engineering in China on the quality of sprayed concrete, the demand of high-quality accelerating agents in the engineering of tunnel construction, coal mine reinforcement, urban road and waterproof facility repair and the like is increasing. The traditional alkaline accelerator has the defects of strong corrosivity, great harm to constructors, large construction resilience, easy alkali aggregate reaction, serious later strength loss, deteriorated concrete durability and the like, and the liquid alkali-free accelerator has the characteristics of low alkali content (the alkali content is less than or equal to 1.0%), difficulty in causing alkali aggregate reaction, good durability of sprayed concrete and the like, and the demand is continuously expanded, so that the liquid alkali-free accelerator becomes a mainstream product for market development.
However, the liquid alkali-free accelerator on the market still has a series of problems of poor stability, high mixing amount, low compressive strength, excessive alkali content, large use of toxic raw materials and the like. Liquid alkali-free accelerator prepared by taking single aluminum sulfate as accelerating component and containing ionic Al in solution3+The concentration is insufficient, and the problem of poor coagulation promoting effect or poor stability exists; at present, a large amount of accelerator products containing hydrofluoric acid and fluorosilicate as main components exist in the market, aluminum sulfate dissolution and liquid phase system stabilization can be promoted, but the problem of insufficient concrete strength exists in practical application, and the accelerator products have great potential safety hazards in high-harm and high-toxicity characteristic production, and can cause serious physical injury to long-term contact production personnel and constructors to a certain extent. During construction in winter in northern China or in high-altitude areas in mountainous areas, the environmental temperature is kept below 0 ℃ for a long time, and the liquid alkali-free setting accelerator generally has the problems of crystallization and precipitation, so that the construction application cannot be realized.
Disclosure of Invention
The invention provides a fluorine-free antifreezing liquid alkali-free setting accelerator and a preparation method thereof, which can meet the construction environment under the low temperature condition of more than 15 ℃ below zero while ensuring no fluorine and alkali, have good stability, short setting time and high 28d compressive strength, meet the use requirements of various occasions, and are environment-friendly.
In order to achieve the technical purpose, the technical scheme adopted by the invention is as follows:
the fluorine-free antifreezing liquid alkali-free setting accelerator is prepared from the following raw materials in parts by weight: 20-40 parts of high-molecular coagulant, 25-45 parts of aluminum sulfate, 2-7 parts of magnesium hydroxide, 2-6 parts of alcohol amine, 0.3-1.0 part of complexing agent, 1-4 parts of antifreezing agent and 25-45 parts of water.
Further, the preparation method of the high-molecular accelerating agent comprises the following steps:
(1) synthesizing an auxiliary agent: putting 430 and 460 parts of acrylic acid into a container, adding 1-3 parts of hydroquinone and 0.5-1.5 parts of thiamine, and uniformly stirring; gradually adding 510-535 parts of diethanolamine according to the mol ratio of acrylic acid to diethanolamine of 1.25:1, heating to 65 ℃ after the addition, adding 9-11 parts of p-toluenesulfonic acid, continuously heating to 105-110 ℃, and carrying out heat preservation reaction for 5 hours for later use;
(2) preparing a dripping material: 8-14 parts of water, 35-45 parts of the auxiliary obtained in the step (1), 5-10 parts of 2-methacrylamide and 0.2-0.9 part of sodium methacylate are uniformly mixed to obtain a dropwise added material;
(3) synthetic high molecular coagulant: adding 35-40 parts of water and 4-10 parts of the auxiliary agent obtained in the step (1) into a container, adding 0.3-0.6 part of ammonium persulfate, stirring for 5-10min, starting to add dropwise addition, wherein the dropwise addition time is 2h, the heat preservation time is 2h, the process temperature is controlled to be 60-75 ℃, and discharging after the heat preservation is finished.
Further, the alcohol amine is one or more of diethanolamine, triethanolamine, triisopropanolamine and diethylisopropanolamine.
Further, the complexing agent is one or more of ethylenediamine tetraacetic acid and sodium salt thereof.
Further, the antifreezing agent is one or more of diethylene glycol, triethylene glycol, urea, isopropanol and ethylene glycol.
A preparation method of a fluorine-free antifreezing liquid alkali-free setting accelerator comprises the following steps:
(1) preparing a high-molecular accelerating agent;
(2) adding water into a container according to the weight part, starting stirring and heating, adding a high-molecular coagulant into the stirring container, stirring for 30min, and controlling the reaction temperature to be 25-40 ℃;
(3) adding aluminum sulfate into a reaction container, then adding an antifreezing agent, alcohol amine and magnesium hydroxide, and finally adding a complexing agent, wherein the reaction temperature is controlled to be 40-75 ℃;
(4) and (4) preserving the temperature, continuously stirring for 3-4 hours, and naturally cooling to obtain the fluorine-free antifreezing liquid alkali-free accelerator.
The alkali-free liquid accelerator product obtained by adopting conventional raw materials and a production mode has poor stability, is easy to generate the phenomena of product layering, effective component precipitation and the like, and influences the use effect; on the other hand, the introduction of the fluorine-containing substance can effectively improve the coagulation promoting effect of the product, but has great potential safety hazard to the health of human bodies and the safety of ecological environment, and is not beneficial to sustainable development.
The high-molecular coagulant is prepared by organic synthesis esterification to obtain a functional small monomer with coagulation accelerating performance; the synthesized functional small monomer is copolymerized with 2-methacrylamide and sodium methallylsulfonate to synthesize a straight-chain type high polymer which takes C-C double bonds as a main chain and is assisted by a functional group with an alcohol amine group and an amide short side chain by virtue of a high molecular structure design and a free radical copolymerization principle.
The side chain molecules of the high-molecular coagulant have smaller steric hindrance, and are easier to contact with cement particles in mixed concrete or mortar, so that the hydramine groups and the amide groups promote the rapid hydration and solidification of tricalcium aluminate in the cement particles, and a large amount of Al is introduced3+The reaction system is promoted to generate a large amount of ettringite needle crystals in a short time, and then the crystals grow to form a net structure, so that the cement paste is promoted to be rapidly solidified.
Advantageous effects
(1) According to the invention, the self-synthesized high-molecular coagulant is used, and the design of the short side chain molecular structure can greatly improve the overall performance of the coagulant, improve the strength and reduce the coagulation time;
(2) the accelerator does not use any fluorine-containing raw materials such as hydrofluoric acid, fluosilicate and the like, and has no toxic or harmful effect on the ecological environment in the production and use processes;
(3) the stability is excellent, and the construction method can be normally applied under the low temperature condition of more than 15 ℃ below zero.
Detailed Description
The technical solution of the present invention is further described below with reference to specific embodiments, but is not limited thereto.
Example 1
The fluorine-free antifreezing liquid alkali-free setting accelerator is prepared from the following raw materials in parts by weight: 20 parts of high-molecular coagulant, 38 parts of aluminum sulfate, 4 parts of magnesium hydroxide, 4.5 parts of alcohol amine, 0.6 part of complexing agent, 2 parts of antifreezing agent and 30.9 parts of water.
The preparation method of the high-molecular coagulant comprises the following steps:
(1) synthesizing an auxiliary agent: putting 430 parts of acrylic acid into a container, adding 1 part of hydroquinone and 0.5 part of thiamine, and uniformly stirring; gradually adding 510 parts of diethanolamine according to the mol ratio of acrylic acid to diethanolamine of 1.25:1, heating to 65 ℃ after the addition, adding 9 parts of p-toluenesulfonic acid, continuously heating to 105 ℃ and 110 ℃, and carrying out heat preservation reaction for 5 hours for later use;
(2) preparing a dripping material: uniformly mixing 13 parts of water, 40 parts of the auxiliary obtained in the step (1), 6 parts of 2-methacrylamide and 0.6 part of sodium methallylsulfonate to obtain a dropwise added material;
(3) synthetic high molecular coagulant: adding 36 parts of water and 4 parts of the auxiliary agent obtained in the step (1) into a container, adding 0.4 part of ammonium persulfate, stirring for 5min, starting to add dropwise addition for 2h, keeping the temperature for 2h, controlling the process temperature to be 60-75 ℃, and discharging after the temperature is kept.
The alcohol amine is triethanolamine.
The complexing agent is disodium ethylene diamine tetraacetate.
The antifreezing agent is prepared from isopropanol and urea according to a mass ratio of 1: 1.5 mixing.
A preparation method of a fluorine-free antifreezing liquid alkali-free setting accelerator comprises the following steps:
(1) preparing a high-molecular coagulant;
(2) adding water into a container according to the weight part, starting stirring and heating, adding a high-molecular coagulant into the stirring container, stirring for 30min, and controlling the reaction temperature at 30 ℃;
(3) sequentially adding aluminum sulfate, an antifreezing agent, alcohol amine, magnesium hydroxide and a complexing agent into a reaction container, and controlling the reaction temperature to be 60-75 ℃;
(4) keeping the temperature, continuously stirring for 3h, and naturally cooling to obtain the fluorine-free anti-freezing liquid alkali-free accelerator.
Example 2
The fluorine-free antifreezing liquid alkali-free setting accelerator is prepared from the following raw materials in parts by weight: 25 parts of high-molecular coagulant, 35 parts of aluminum sulfate, 3.5 parts of magnesium hydroxide, 3.5 parts of alcohol amine, 0.5 part of complexing agent, 2 parts of antifreezing agent and 30.5 parts of water.
The preparation method of the high-molecular coagulant comprises the following steps:
(1) synthesizing an auxiliary agent: putting 450 parts of acrylic acid into a container, adding 2 parts of hydroquinone and 1 part of thiamine, and uniformly stirring; gradually adding 520 parts of diethanolamine according to the mol ratio of acrylic acid to diethanolamine of 1.25:1, heating to 65 ℃ after the addition, adding 10 parts of p-toluenesulfonic acid, continuously heating to 105 ℃ and 110 ℃, and carrying out heat preservation reaction for 5 hours for later use;
(2) preparing a dripping material: uniformly mixing 10 parts by weight of water, 37 parts by weight of the auxiliary obtained in the step (1), 5 parts by weight of 2-methacrylamide and 0.6 part by weight of sodium methallylsulfonate to obtain a dropwise added material;
(3) synthetic high molecular coagulant: and (2) adding 39 parts of water and 8 parts of the auxiliary agent obtained in the step (1) into a container, adding 0.4 part of ammonium persulfate, stirring for 5min, starting to add dropwise addition for 2h, keeping the temperature for 2h, controlling the process temperature to be 60-75 ℃, and discharging after the temperature is kept.
The alcohol amine is triisopropanolamine.
The complexing agent is sodium ethylene diamine tetracetate.
The antifreezing agent is obtained by mixing diethylene glycol and isopropanol according to the mass ratio of 1.5: 1.
A preparation method of a fluorine-free antifreezing liquid alkali-free setting accelerator comprises the following steps:
(1) preparing a high-molecular coagulant;
(2) adding water into a container according to the weight part, starting stirring and heating, adding a high-molecular coagulant into the stirring container, stirring for 30min, and controlling the reaction temperature at 30 ℃;
(3) sequentially adding aluminum sulfate, an antifreezing agent, alcohol amine, magnesium hydroxide and a complexing agent into a reaction container, and controlling the reaction temperature to be 60-75 ℃;
(4) keeping the temperature, continuously stirring for 3h, and naturally cooling to obtain the fluorine-free anti-freezing liquid alkali-free accelerator.
Example 3
The fluorine-free antifreezing liquid alkali-free setting accelerator is prepared from the following raw materials in parts by weight: 30 parts of high-molecular coagulant, 32 parts of aluminum sulfate, 3 parts of magnesium hydroxide, 3 parts of alcohol amine, 0.3 part of complexing agent, 2.7 parts of antifreezing agent and 29 parts of water.
The preparation method of the high-molecular coagulant comprises the following steps:
(1) synthesizing an auxiliary agent: putting 440 parts of acrylic acid into a container, adding 2 parts of hydroquinone and 1.2 parts of thiamine, and uniformly stirring; gradually adding 525 parts of diethanolamine according to the mol ratio of acrylic acid to diethanolamine of 1.25:1, heating to 65 ℃ after the addition, adding 9 parts of p-toluenesulfonic acid, continuously heating to 105 ℃ and 110 ℃, and carrying out heat preservation reaction for 5 hours for later use;
(2) preparing a dripping material: uniformly mixing 10 parts by weight of water, 37 parts by weight of the auxiliary obtained in the step (1), 5 parts by weight of 2-methacrylamide and 0.6 part by weight of sodium methallylsulfonate to obtain a dropwise added material;
(3) synthetic high molecular coagulant: and (2) adding 39 parts of water and 8 parts of the auxiliary agent obtained in the step (1) into a container, adding 0.4 part of ammonium persulfate, stirring for 10min, starting to add dropwise addition for 2h, keeping the temperature for 2h, controlling the process temperature to be 60-75 ℃, and discharging after the temperature is kept.
The alcohol amine is triisopropanolamine.
The complexing agent is ethylenediamine tetraacetic acid.
The antifreezing agent is obtained by mixing diethylene glycol and isopropanol according to a mass ratio of 4: 5.
A preparation method of a fluorine-free antifreezing liquid alkali-free setting accelerator comprises the following steps:
(1) preparing a high-molecular coagulant;
(2) adding water into a container according to the weight part, starting stirring and heating, adding a high-molecular coagulant into the stirring container, stirring for 30min, and controlling the reaction temperature at 30 ℃;
(3) sequentially adding aluminum sulfate, an antifreezing agent, alcohol amine, magnesium hydroxide and a complexing agent into a reaction container, and controlling the reaction temperature to be 50-60 ℃;
(4) keeping the temperature, continuously stirring for 3h, and naturally cooling to obtain the fluorine-free anti-freezing liquid alkali-free accelerator.
Example 4
The fluorine-free antifreezing liquid alkali-free setting accelerator is prepared from the following raw materials in parts by weight: 36.5 parts of high-molecular coagulant, 27.5 parts of aluminum sulfate, 2 parts of magnesium hydroxide, 3 parts of alcohol amine, 0.3 part of complexing agent, 3 parts of antifreezing agent and 27.7 parts of water.
The preparation method of the high-molecular coagulant comprises the following steps:
(1) synthesizing an auxiliary agent: putting 460 parts of acrylic acid into a container, adding 3 parts of hydroquinone and 1.5 parts of thiamine, and uniformly stirring; gradually adding 535 parts of diethanolamine according to the mol ratio of acrylic acid to diethanolamine of 1.25:1, heating to 65 ℃ after the addition, adding 11 parts of p-toluenesulfonic acid, continuously heating to 105 ℃ and 110 ℃, and carrying out heat preservation reaction for 5 hours for later use;
(2) preparing a dripping material: uniformly mixing 8 parts of water, 35 parts of the auxiliary obtained in the step (1), 6.8 parts of 2-methacrylamide and 0.8 part of sodium methallylsulfonate to obtain a dropwise added material;
(3) synthetic high molecular coagulant: adding 39 parts of water and 10 parts of the auxiliary agent obtained in the step (1) into a container, adding 0.4 part of ammonium persulfate, stirring for 10min, starting to add dropwise addition for 2h, keeping the temperature for 2h, controlling the process temperature to be 60-75 ℃, and discharging after the temperature is kept.
The alcohol amine is diethanol amine.
The complexing agent is ethylenediamine tetraacetic acid.
The antifreezing agent is prepared by mixing urea and glycol according to the mass ratio of 1: 1.
A preparation method of a fluorine-free antifreezing liquid alkali-free setting accelerator comprises the following steps:
(1) preparing a high-molecular coagulant;
(2) adding water into a container according to the weight part, starting stirring and heating, adding a high-molecular coagulant into the stirring container, stirring for 30min, and controlling the reaction temperature at 30 ℃;
(3) sequentially adding aluminum sulfate, an antifreezing agent, alcohol amine, magnesium hydroxide and a complexing agent into a reaction container, and controlling the reaction temperature to be 40-50 ℃;
(4) keeping the temperature, continuously stirring for 4h, and naturally cooling to obtain the fluorine-free anti-freezing liquid alkali-free accelerator.
Performance testing
The products prepared in the above examples and comparative examples are subjected to performance tests, and the test detection standard is as follows:
GB/T35159 and 2017 accelerator for shotcrete;
Q/CR 807-.
The selected test materials are standard cement and standard sand, a stability test device thermometer and a 100ml stopcock measuring cylinder, the mixing amount of the liquid alkali-free accelerator is 8 percent, and two types of commercially available accelerator products are selected as a comparison test group, namely an HQ alkali-free liquid accelerator sold in Kaiwate market in comparison example 1 and an SA160 alkali-free liquid accelerator sold in Basff market in comparison example 2.
The results obtained are shown in table 1 below.
Table 1 results of performance testing
The test data show that the liquid alkali-free accelerator prepared by the invention has good setting time and mortar strength test effect and excellent negative temperature stability, meets the latest specification requirement of accelerator products, does not contain fluorine-containing substances, and has more remarkable comprehensive performance compared with the mature products sold in the market.
It should be noted that the above-mentioned embodiments are only some of the preferred modes for implementing the invention, and not all of them. Obviously, all other embodiments obtained by persons of ordinary skill in the art based on the above-mentioned embodiments of the present invention without any creative effort shall fall within the protection scope of the present invention.
Claims (6)
1. The fluorine-free antifreezing liquid alkali-free setting accelerator is characterized by being prepared from the following raw materials in parts by weight: 20-40 parts of high-molecular coagulant, 25-45 parts of aluminum sulfate, 2-7 parts of magnesium hydroxide, 2-6 parts of alcohol amine, 0.3-1.0 part of complexing agent, 1-4 parts of antifreezing agent and 25-45 parts of water.
2. The fluorine-free antifreezing liquid alkali-free setting accelerator as claimed in claim 1, wherein the polymeric coagulant is prepared by the following steps:
(1) synthesizing an auxiliary agent: putting 430 and 460 parts of acrylic acid into a container, adding 1-3 parts of hydroquinone and 0.5-1.5 parts of thiamine, and uniformly stirring; gradually adding 510-535 parts of diethanolamine according to the mol ratio of acrylic acid to diethanolamine of 1.25:1, heating to 65 ℃ after the charging, adding 9-11 parts of p-toluenesulfonic acid, continuously heating to 105-110 ℃, carrying out heat preservation reaction for 5 hours, and discharging for later use;
(2) preparing a dripping material: 8-14 parts of water, 35-45 parts of the auxiliary obtained in the step (1), 5-10 parts of 2-methacrylamide and 0.2-0.9 part of sodium methacylate are uniformly mixed to obtain a dropwise added material;
(3) synthetic high molecular coagulant: adding 35-40 parts of water and 4-10 parts of the auxiliary agent obtained in the step (1) into a container, adding 0.3-0.6 part of ammonium persulfate, stirring for 5-10min, starting to add dropwise addition, wherein the dropwise addition time is 2h, the heat preservation time is 2h, the process temperature is controlled to be 60-75 ℃, and discharging after the heat preservation is finished.
3. The fluorine-free antifreeze liquid alkali-free accelerator as claimed in claim 1, wherein said alcohol amine is one or more of diethanolamine, triethanolamine, triisopropanolamine, and diethylisopropanolamine.
4. The fluorine-free antifreeze type liquid alkali-free accelerator as claimed in claim 1, wherein said complexing agent is one or more of ethylenediaminetetraacetic acid and sodium salts thereof.
5. The fluorine-free antifreeze liquid alkali-free accelerator as claimed in claim 1, wherein said antifreeze is one or more of diethylene glycol, triethylene glycol, urea, isopropyl alcohol, ethylene glycol.
6. A method for preparing the fluorine-free antifreezing liquid alkali-free accelerator as described in any one of claims 1 to 5, comprising the steps of:
(1) preparing a high-molecular coagulant;
(2) adding water into a container according to the weight part, starting stirring and heating, adding a high-molecular coagulant into the stirring container, stirring for 30min, and controlling the reaction temperature to be 25-40 ℃;
(3) adding aluminum sulfate into a reaction container, then adding an antifreezing agent, alcohol amine and magnesium hydroxide, and finally adding a complexing agent, wherein the reaction temperature is controlled to be 40-75 ℃;
(4) and (4) preserving the temperature, continuously stirring for 3-4 hours, and naturally cooling to obtain the fluorine-free antifreezing liquid alkali-free accelerator.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115772010A (en) * | 2022-12-09 | 2023-03-10 | 山东高强新材料科技有限公司 | Anti-flocculant for efficiently treating flocculation material in washing sand for building concrete and preparation method thereof |
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2021
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115772010A (en) * | 2022-12-09 | 2023-03-10 | 山东高强新材料科技有限公司 | Anti-flocculant for efficiently treating flocculation material in washing sand for building concrete and preparation method thereof |
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Application publication date: 20211130 |