CN110204238B - Water-soluble powdery alkali-free accelerator and preparation method thereof - Google Patents
Water-soluble powdery alkali-free accelerator and preparation method thereof Download PDFInfo
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- CN110204238B CN110204238B CN201910507900.8A CN201910507900A CN110204238B CN 110204238 B CN110204238 B CN 110204238B CN 201910507900 A CN201910507900 A CN 201910507900A CN 110204238 B CN110204238 B CN 110204238B
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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
Abstract
The invention provides a water-soluble powdery alkali-free accelerator and a preparation method thereof, wherein the accelerator comprises the following raw materials in percentage by mass: 45 to 52 percent of aluminum sulfate; 1 to 5 percent of lithium silicate; 5 to 10 percent of manganese fluosilicate; 1 to 3 percent of pH regulator; 0.5 to 1 percent of suspension stabilizer; the balance of water, and the total amount is up to 100%. The water-soluble powdery alkali-free accelerator can simultaneously meet 1) the alkali-free standard of GB/T35159-2017 accelerator for sprayed concrete; 2) the normal state is solid powdery raw materials, which is convenient for long-distance transportation; 3) has very good water solubility when in use; 4) the product has four requirements of ultrahigh stability after use, and has good application and popularization values.
Description
Technical Field
The invention belongs to the technical field of building material additives, and particularly relates to a water-soluble powdery alkali-free accelerator as well as a preparation method and application thereof.
Background
The accelerator is an additive capable of quickly setting and hardening concrete or cement mortar, and is widely applied to mine roadway support, tunnel concrete spraying and mortar spraying construction and emergency repair construction. The main technological process of spraying concrete is divided into dry spraying method and wet spraying method. The dry-spraying concrete spraying technique has been gradually replaced by the wet-spraying concrete technique due to the disadvantages of large dust, large rebound quantity, uneven distribution of the sprayed concrete strength, and the like. In recent years, liquid accelerators have come into play with the popularization of wet-sprayed concrete technology, but most of these accelerators are strongly alkaline, thus posing a threat to the personal safety of construction personnel during use, and causing various problems such as large loss of later strength of concrete, poor durability, large spraying rebound quantity and the like.
The alkali-free accelerator solves a series of problems caused by high alkali content of the traditional alkali accelerator, and has the advantages of safety, environmental protection, no corrosion, good durability, good mechanical property, small injection resilience and the like. The technology of the domestic alkali-free setting accelerator is developed quickly, particularly in recent two years, a large number of alkali-free setting accelerator patents are applied, and the technology development is mature day by day.
The patent CN1970487A discloses a powdery alkali-free accelerator, but the accelerator uses sodium silicate and sodium aluminate with sodium oxide equivalent of more than 1%. According to the definition of the alkali-free accelerator in GB/T35159-2017 accelerator for sprayed concrete, the patent does not belong to the alkali-free accelerator. The research on cement alkali-free accelerator, namely Panshihua, Xuyongdong, Wuchenjia, et al, J, proceedings of university of Nanjing industry (Nature science edition), 1997, 19(02):63-67, mentions that the cement mineral alkali-free accelerator can be synthesized by calcining alumina, limestone and a small amount of cosolvent at about 1330 ℃, but the powdery accelerator has no water solubility, so the powdery accelerator can only be used for spraying concrete by a dry spraying method.
Patent applications for alkali-free liquid accelerators also exist, for example, CN1974466A discloses a liquid alkali-free accelerator for shotcrete. CN103553406A discloses an alkali-free and chlorine-free liquid accelerator based on industrial polyaluminium sulfate. However, the alkali-free liquid accelerator has many problems in terms of stability, economy and product radiation range. That is, the current alkali-free liquid accelerator products have great limitations.
1) Poor stability and is not suitable for long-term storage. The existing alkali-free setting accelerator contains a large amount of aluminum ions, and the aluminum ions can be hydrolyzed and precipitated in an aqueous solution, so that the setting accelerator can be subjected to irreversible precipitation and crystallization when in use. An alkali-free liquid accelerator as disclosed in US patent (US2012/0085266 a1), having a stabilization period of only one month; an alkali-free liquid accelerator disclosed in U.S. Pat. No. 8, 8118930, 2 has a stabilization period of 8 weeks. The stabilization period is too short, and the accelerator can not be used again once irreversible precipitation occurs under the condition of untimely transportation and use.
2) The packaging cost is high. Because the pH value of the alkali-free accelerator is mostly acidic and reacts with an iron container, the alkali-free accelerator is generally packaged by a plastic barrel of 200 liters or 1000 liters, and the packaging cost of the alkali-free liquid accelerator is greatly increased.
3) The transportation cost is greatly increased due to the special requirement of the packaging cost, and the conventional alkali-free liquid accelerator generally contains 30-60% of water, so that the transportation cost of accelerator products is increased undoubtedly; the defect causes a small radiation range of the product, is difficult to expand the application range of the product, and seriously influences the development and popularization of the accelerator in the construction industry.
Therefore, an alkali-free standard which simultaneously meets 1) GB/T35159-2017 accelerating agent for sprayed concrete is found; 2) the normal state is solid powdery raw materials, which is convenient for long-distance transportation; 3) has very good water solubility when in use; 4) the accelerator which has four requirements of ultrahigh stability after being used is a technical problem which is urgently needed to be solved.
Disclosure of Invention
The invention aims to solve the problems of the alkali-free liquid accelerator, provides a water-soluble powdery alkali-free accelerator and a preparation method thereof, and also provides an application method of the water-soluble powdery accelerator. The accelerator provided by the invention meets the four technical requirements, can be widely used in the construction industry, and can meet the more severe technical requirements of the construction industry.
The invention is realized by adopting the following technical scheme.
The invention discloses a water-soluble powdery alkali-free accelerator which comprises the following raw materials in percentage by mass:
45 to 52 percent of aluminum sulfate;
1 to 5 percent of lithium silicate;
5 to 10 percent of manganese fluosilicate;
1 to 3 percent of pH regulator;
0.5 to 1 percent of suspension stabilizer;
the balance of water, and the total amount is up to 100%.
Further, the aluminum sulfate contains 15.6-17% of alumina and has a moisture content of no more than 4%.
Further, the solid content of the lithium silicate is 20-30%.
Furthermore, the manganese content in the manganese fluosilicate is not less than 8%, the fluorine content is not less than 50%, and the moisture content is not more than 1%.
Further, the pH regulator is formic acid or tartaric acid.
Further, the suspension stabilizer is sepiolite
The invention discloses a preparation method of a water-soluble powdery alkali-free accelerator, which comprises the following steps:
1) adding water into a reaction kettle, heating to 65-85 ℃, then sequentially adding aluminum sulfate, lithium silicate and manganese fluosilicate, and continuously stirring for 0.5-1 h;
2) dripping a pH regulator into the material obtained in the step (1) by using a constant flow pump, wherein the dripping time is controlled to be 0.5-1 h;
3) continuously stirring for 1-1.5 h under the condition of keeping the temperature at 65-85 ℃;
4) adding a suspension stabilizer, starting a high-speed shearing emulsifying machine, wherein the rotating speed is 6000 r/min-8000 r/min, and the emulsifying time is 0.5 h-1 h to obtain an alkali-free liquid accelerator;
5) and (5) passing the material obtained in the step (4) through a spray drying tower to obtain a white powdery alkali-free accelerator.
Further, in the step (5), the spray drying pressure is 0.1-0.3 times of the standard atmospheric pressure, and the temperature in the spray drying chamber is 250-300 ℃.
The preparation method of the water-soluble powdery alkali-free accelerator comprises the following raw materials in percentage by mass:
45 to 52 percent of aluminum sulfate;
1 to 5 percent of lithium silicate;
5 to 10 percent of manganese fluosilicate;
1 to 3 percent of pH regulator;
0.5 to 1 percent of suspension stabilizer;
the balance of water, and the total amount is up to 100%.
A preparation method of a water-soluble powdery alkali-free accelerator comprises the following steps of preparing an alkali-free liquid accelerator from the white powdery alkali-free accelerator prepared in the step 5 and water in a mass ratio of 1: 0.8-1: 1.5; the cement mortar is used in the construction of sprayed concrete, and the mixing amount of the cement mortar is 4-6% of the mass of cement.
The invention has the beneficial effects that: 1) the water-soluble powdery alkali-free accelerator has the advantages of no alkali and no corrosion: the alkali content of the water-soluble alkali-free powdery accelerator is less than 1 percent, and the alkali-free powdery accelerator reaches the alkali-free standard of GB/T35159-2017 accelerator for sprayed concrete; the possibility of alkali aggregate reaction of the sprayed concrete is greatly reduced, and the durability of the sprayed concrete is improved; in addition, different from the alkaline accelerator, the pH value of the alkali-free accelerator is weakly acidic, so that the alkali-free accelerator does not corrode the body of a worker, and the personal safety and health of the worker are greatly improved. 2) The product of the invention has ultrahigh strength: the 1d strength of the mortar of the accelerator prepared by the invention is up to more than 17MPa, the later strength is not lost and is increased, wherein the 28d compressive strength ratio of the mortar is up to more than 110%, and the 90-day strength retention rate is more than 105%. The concrete is used for the sprayed concrete, has higher early strength, can also ensure that the later strength is increased to some extent, and is safe to a tunnel supporting structure. 3) The product of the invention has excellent stability and is convenient for long-term storage: the water-soluble powdery alkali-free accelerator is solid powder, so that the phenomenon that a finished product of the liquid accelerator is easy to precipitate or even crystallize in the transportation and storage processes is avoided. When the product is stored in a warehouse for one year, the product can be reused without affecting the performance. 4) The packaging cost is greatly reduced: the invention uses the plastic woven bag with the waterproof plastic inner bag for packaging, and the packaging cost per ton is far lower than that of the alkali-free liquid accelerator. 5) The transportation cost is greatly reduced. The water-soluble powdery alkali-free accelerator can be added with water to prepare 1.8-2.5 tons of finished alkali-free liquid accelerator per ton. Compared with the conventional alkali-free liquid accelerator, the product of the invention reduces the transportation cost by 40-60%. 6) The dissolubility is good: the water-soluble powdery alkali-free accelerator has good solubility in water, and can be instantly prepared into an alkali-free liquid accelerator by adding water and stirring according to a proportion in a normal-temperature field environment.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
The invention discloses a water-soluble powdery alkali-free accelerator which comprises the following raw materials in percentage by mass: 45 to 52 percent of aluminum sulfate; 1 to 5 percent of lithium silicate; 5 to 10 percent of manganese fluosilicate; 1 to 3 percent of pH regulator; 0.5 to 1 percent of suspension stabilizer; the balance of water, and the total amount is up to 100%.
Further, the aluminum sulfate contains 15.6-17% of alumina and has a moisture content of no more than 4%.
Further, the solid content of the lithium silicate is 20-30%.
Furthermore, the manganese content in the manganese fluosilicate is not less than 8%, the fluorine content is not less than 50%, and the moisture content is not more than 1%.
Further, the pH regulator is formic acid or tartaric acid.
Further, the suspension stabilizer is sepiolite
The invention discloses a preparation method of a water-soluble powdery alkali-free accelerator, which comprises the following steps:
1) adding water into a reaction kettle, heating to 65-85 ℃, then sequentially adding aluminum sulfate, lithium silicate and manganese fluosilicate, and continuously stirring for 0.5-1 h;
2) dripping a pH regulator into the material obtained in the step (1) by using a constant flow pump, wherein the dripping time is controlled to be 0.5-1 h;
3) continuously stirring for 1-1.5 h under the condition of keeping the temperature at 65-85 ℃;
4) adding a suspension stabilizer, starting a high-speed shearing emulsifying machine, wherein the rotating speed is 6000 r/min-8000 r/min, and the emulsifying time is 0.5 h-1 h to obtain an alkali-free liquid accelerator;
5) and (5) passing the material obtained in the step (4) through a spray drying tower to obtain a white powdery alkali-free accelerator.
Further, in the step (5), the spray drying pressure is 0.1-0.3 times of the standard atmospheric pressure, and the temperature in the spray drying chamber is 250-300 ℃.
The preparation method of the water-soluble powdery alkali-free accelerator comprises the following raw materials in percentage by mass: 45 to 52 percent of aluminum sulfate; 1 to 5 percent of lithium silicate; 5 to 10 percent of manganese fluosilicate; 1 to 3 percent of pH regulator; 0.5 to 1 percent of suspension stabilizer; the balance of water, and the total amount is up to 100%.
Detailed comparison of specific experiments
The percentages are mass percentages unless otherwise specified. The starting materials are available from published commercial sources unless otherwise specified.
The present invention will be understood by reference to the following examples, which are provided for illustrative purposes and are not intended to limit the scope of the present invention.
Examples 1 to 5 Water-soluble alkali-free accelerators in powder form and comparative examples are shown in Table 1, and their preparation methods are shown in Table 2:
TABLE 1 EXAMPLES 1-5 raw material formulation of water-soluble alkali-free accelerator powder
TABLE 2 EXAMPLES 1-5 preparation method parameters of water-soluble alkali-free accelerator powder
The comparative example used an alkali-free liquid accelerator prepared by the method of application publication No. CN 102173630A.
Application example
Mixing the water-soluble powdery accelerator of preparation example 1-5 with water according to a mass ratio of 1: 0.8-1: 1.5 preparing a conventional alkali-free liquid accelerator, adding the accelerator into a cement paste or cement mortar sample in an amount of 4-6% of the weight of cement, and testing the setting time and the compressive strength according to the standard of GB/T35159-2017 accelerator for sprayed concrete, wherein the performance indexes required by the standard are shown in Table 3. The comparative example and the non-alkali setting accelerator (MEYCO SA160) with more advanced performance at foreign countries are used as the contrast, and the blank is that no setting accelerator is added.
TABLE 3 Property requirements of slurries and mortars incorporating accelerators
TABLE 4 correlation Performance test results
The test results are shown in Table 4, and the alkali content of each example is less than 1%, and the examples belong to alkali-free setting accelerators; according to the standard analysis of GB/T35159-2017 accelerator for sprayed concrete, the mixing amount of the alkali-free accelerator prepared by the invention is 4%, and the alkali-free accelerator can meet the standard requirement. In addition, the alkali-free setting accelerator prepared by the invention has the characteristics of high strength, such as example 5, the 1d compressive strength of the mortar is up to 20.5MPa, the 28d compressive strength ratio is up to 115%, and the 90d strength retention rate is even up to 123%.
In the comparative example, the setting time of the prepared accelerator is qualified, but the indexes of 1d compressive strength, 28d compressive strength ratio and 90d strength retention rate are all lower than those of the example. As a contrast, the mixing amount of the commercially available alkali-free accelerator MEYCO SA160 is up to 8-10% to meet the requirement. Compared with the prior art, the alkali-free accelerator prepared by the invention has lower mixing amount and higher compressive strength, which shows that the performance of the alkali-free accelerator prepared by the invention is superior to that of the similar products (MEYCO SA160) at home and abroad.
TABLE 5 Effect of storage time of Water-soluble alkali-free powdery accelerators on the performances of the accelerators
The experimental results are shown in Table 5, which shows that the properties of the water-soluble alkali-free powder accelerator such as setting time, strength and the like are slightly different from those of the product which is just produced when the water-soluble alkali-free powder accelerator is used after being stored for one year. It is sufficient to show that the invention has an ultra-long storage time.
TABLE 6 Adaptation of alkali-free setting accelerator with cement, formulated from water-soluble powdery alkali-free setting accelerator
As can be seen from Table 6, the alkali-free accelerator can enable different brands and different types of cement to meet the construction requirements of concrete for spraying under the condition of low mixing amount, and has strong adaptability to engineering cement.
The above description is only a part of specific embodiments of the present invention (since the formula of the present invention belongs to the numerical range, the embodiments are not exhaustive, and the protection scope of the present invention is subject to the numerical range and other technical point ranges), and the detailed contents or common knowledge known in the schemes are not described too much. It should be noted that the above-mentioned embodiments do not limit the present invention in any way, and all technical solutions obtained by means of equivalent substitution or equivalent transformation for those skilled in the art are within the protection scope of the present invention. The scope of the claims of the present application shall be determined by the contents of the claims, and the description of the embodiments and the like in the specification shall be used to explain the contents of the claims.
Claims (8)
1. The water-soluble powdery alkali-free accelerator is characterized by comprising the following raw materials in percentage by mass:
45% -52% of aluminum sulfate;
1% -5% of lithium silicate;
5% -10% of manganese fluosilicate;
1% -3% of a pH regulator; the pH regulator is formic acid or tartaric acid;
0.5% -1% of suspension stabilizer; the suspension stabilizer is sepiolite;
the balance of water, and the total amount is up to 100%.
2. The water-soluble powdery alkali-free accelerator as claimed in claim 1, wherein the aluminum sulfate contains 15.6-17% of alumina and has a water content of not more than 4%.
3. The water-soluble alkali-free powdery accelerator according to claim 1, wherein the solid content of the lithium silicate is 20-30%.
4. The water-soluble powdery alkali-free accelerator as claimed in claim 1, wherein the manganese fluorosilicate contains not less than 8% of manganese, not less than 50% of fluorine, and not more than 1% of water.
5. A preparation method of a water-soluble powdery alkali-free accelerator is characterized by comprising the following steps:
1) adding water into a reaction kettle, heating to 65-85 ℃, then sequentially adding aluminum sulfate, lithium silicate and manganese fluosilicate, and continuously stirring for 0.5-1 h;
2) dropwise adding a pH regulator into the material obtained in the step (1) by using a constant flow pump, wherein the dropwise adding time is controlled to be 0.5-1 h; the pH regulator is formic acid or tartaric acid;
3) continuously stirring for 1-1.5 h under the condition of keeping the temperature at 65-85 ℃;
4) adding a suspension stabilizer, wherein the suspension stabilizer is sepiolite; starting a high-speed shearing emulsifying machine, wherein the rotating speed is 6000 r/min-8000 r/min, and the emulsifying time is 0.5 h-1 h, so as to obtain the alkali-free liquid accelerator;
5) and (5) passing the material obtained in the step (4) through a spray drying tower to obtain a white powdery alkali-free accelerator.
6. The method for preparing the water-soluble alkali-free powdery accelerator according to claim 5, wherein the spray drying pressure in the step (5) is 0.1 to 0.3 times of the standard atmospheric pressure, and the temperature in the spray drying chamber is 250 ℃ to 300 ℃.
7. The preparation method of the water-soluble alkali-free powdery accelerator as claimed in claim 5 or 6, wherein the preparation method comprises the following raw materials in percentage by mass:
45% -52% of aluminum sulfate;
1% -5% of lithium silicate;
5% -10% of manganese fluosilicate;
1% -3% of a pH regulator;
0.5% -1% of suspension stabilizer;
the balance of water, and the total amount is up to 100%.
8. The preparation method of the water-soluble alkali-free powdery accelerator as claimed in claim 5 or 6, wherein the white alkali-free powdery accelerator prepared in step 5 is used by preparing an alkali-free liquid accelerator from the white alkali-free powdery accelerator and water in a mass ratio of 1: 0.8-1: 1.5; the cement mortar is used in the construction of sprayed concrete, and the mixing amount of the cement mortar is 4-6% of the mass of cement.
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| CN110510900B (en) * | 2019-09-12 | 2021-08-13 | 云南凯威特新材料股份有限公司 | Modified villiaumite and method for preparing low-alkali liquid accelerator for sprayed concrete by using same |
| CN111056762B (en) * | 2019-12-13 | 2021-07-30 | 武汉比邻科技发展有限公司 | Alkali-free liquid accelerator and preparation method thereof |
| CN111574093A (en) * | 2020-05-22 | 2020-08-25 | 山西海裕隆建材有限公司 | High-performance alkali-free liquid accelerator and preparation method thereof |
| CN111499248A (en) * | 2020-05-22 | 2020-08-07 | 山西海裕隆建材有限公司 | High-performance alkali-free liquid accelerator special for moderate-heat low-heat cement and preparation method thereof |
| CN111939853A (en) * | 2020-07-06 | 2020-11-17 | 江苏奥莱特新材料股份有限公司 | Production device and method of solid alkali-free setting accelerator |
| CN112142359B (en) * | 2020-09-25 | 2022-05-27 | 福泉凯威特新材料有限公司 | Dry and wet spraying concrete dual-purpose powdery alkali-free accelerator and preparation and use methods thereof |
| CN112897919A (en) * | 2021-01-22 | 2021-06-04 | 广西新广建新材料有限公司 | Liquid accelerator and preparation method thereof |
| CN112691632A (en) * | 2021-01-22 | 2021-04-23 | 广西新广建新材料有限公司 | Alkali-free accelerator production system |
| CN113264711A (en) * | 2021-06-28 | 2021-08-17 | 山西佳维新材料股份有限公司 | Powder alkali-free accelerator and preparation method, use method and application thereof |
| CN113548825A (en) * | 2021-07-30 | 2021-10-26 | 江苏奥莱特新材料股份有限公司 | Solid master batch of fluoride-free alkali-free liquid accelerator and preparation and use methods thereof |
| CN113582573A (en) * | 2021-09-01 | 2021-11-02 | 多氟多新材料股份有限公司 | Accelerating agent and preparation method and application thereof |
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| JPH1143360A (en) * | 1997-07-23 | 1999-02-16 | Chichibu Onoda Cement Corp | Quick setting promoter |
| JPH11322397A (en) * | 1998-05-18 | 1999-11-24 | Onoda Co | Quick-setting spraying material |
| CN100448791C (en) * | 2005-11-29 | 2009-01-07 | 尚红利 | Alkali-free speed coagulating agent |
| CN106517871A (en) * | 2016-11-29 | 2017-03-22 | 广西大学 | Concrete accelerator and preparation method thereof |
| CN109231871A (en) * | 2018-09-19 | 2019-01-18 | 攀枝花市吉源科技有限责任公司 | A kind of low-mix quantity high performance alkali-free chlorine-free liquid accelerator and preparation method thereof |
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