A basalt fiber anti-cracking agent, its preparation method and application

Abstract

This application relates to a basalt fiber crack-resistant agent, its preparation method, and its application, belonging to the field of building material admixtures technology. By weight, the basalt fiber crack-resistant agent comprises the following components: component A 10-20 parts, component B 15-25 parts, component C 1-5 parts, heavy calcium carbonate powder 40-60 parts, and basalt fiber 5-15 parts. This invention, by using specific components A, B, and C in combination with heavy calcium carbonate powder and basalt fiber, produces a basalt fiber crack-resistant agent with excellent crack resistance, which can be applied to the manufacture of building materials such as concrete and has broad practical application value.

Description

Technical Field

[0001] This application relates to the field of building material admixtures, and in particular to a basalt fiber anti-cracking agent, its preparation method, and its application. Background Technology

[0002] Concrete cracks are often accompanied by leakage problems, and building leakage directly affects residents' living environment and safety. Concrete cracks take many forms and types. To fundamentally solve the problem of cracks in concrete, most are caused by temperature changes and shrinkage during the crack formation process. The resulting temperature shrinkage stress is the main cause of cracks in reinforced concrete.

[0003] Currently, numerous crack-resistant agents have appeared on the market to address the problem of concrete cracking, but their crack-resistant effects are not significant in actual use. Therefore, it is necessary to develop a building material admixture with excellent crack-resistant properties to solve the existing problem of concrete cracking. Summary of the Invention

[0004] To address the aforementioned issues, this application provides a basalt fiber anti-cracking agent, its preparation method, and its application.

[0005] In a first aspect, this application provides a basalt fiber anti-cracking agent, which, by weight, comprises the following components:

[0006] Component A 10-20 parts, component B 15-25 parts, component C 1-5 parts, heavy calcium carbonate powder 40-60 parts, and basalt fiber 5-15 parts;

[0007] Component A is obtained by refining, concentrating and crystallizing glucose as a starting material using a hydrogenation method;

[0008] Component B is obtained by using sorbitol as a starting material, followed by phosphoric acid-catalyzed dehydration to anhydride reaction and esterification reaction with stearic acid.

[0009] The preparation of component C includes: reacting maleic anhydride and hydrogen peroxide as raw materials to obtain an intermediate product system; hydrolyzing the intermediate product system with phosphomolybdic acid to obtain a solution containing epoxy succinic acid; cooling and crystallizing the solution containing epoxy succinic acid, and then filtering to obtain component C.

[0010] Furthermore, by weight, the basalt fiber anti-cracking agent comprises the following components:

[0011] Component A 15-20 parts, component B 15-20 parts, component C 1-5 parts, heavy calcium carbonate powder 50-60 parts, and basalt fiber 10-15 parts.

[0012] Furthermore, by weight, the basalt fiber anti-cracking agent comprises the following components:

[0013] Component A: 17 parts; Component B: 18 parts; Component C: 2 parts; Heavy calcium carbonate powder: 53 parts; Basalt fiber: 10 parts.

[0014] Furthermore, the preparation method of component A includes the following steps:

[0015] Using glucose as raw material, pure water is used for saccharification at a concentration of 45%–52%, and the pH is adjusted to 7.5–8.0 to obtain a colorless or very pale yellow glucose solution. A nickel powder catalyst, comprising 1–3 wt% of the glucose solution, is added to a glucose solution feed metering tank and mixed well. This mixture is then pumped into a hydrogenation reactor using a high-pressure feed pump. After feeding is complete, the hydrogenation reactor is stirred at a speed of 240–360 r / min, and the hydrogen pressure is increased to a set pressure of 10.0 MPa. Simultaneously, the jacket steam is activated. The temperature of the liquid mixture is gradually increased and maintained at 110-145℃. The hydrogenation reaction is continued for 2-3 hours within this temperature range. After the hydrogenation reaction is completed, the mixture is purified by decolorization and ion exchange. The purified and decolorized liquid is clear and transparent, yielding a liquid product. Then, in a static crystallizer, the concentration of the liquid product is controlled at 40-60 wt%, and the crystallization temperature is controlled at 50-60℃. After the crystallization process is completed, the crystallized product is separated into solid and liquid components using a centrifuge. The separated wet cake is then spray-dried to obtain component A.

[0016] Furthermore, the preparation method of component B includes the following steps:

[0017] Sorbitol was added to a vacuum reactor, along with phosphoric acid. The mixture was stirred and heated to 145-150°C. The mixture was then dehydrated under vacuum to form anhydride for 3-4 hours. Nitrogen gas was then introduced to release the vacuum, and samples were taken for testing. The required hydroxyl value of the sorbitol anhydride was 1260-1380, thus obtaining the first reaction mixture system.

[0018] Stearic acid was added to the first reaction mixture system, and an alkaline catalyst was added under stirring. Esterification was carried out under vacuum at a temperature of 200-205℃ for 3-4 hours and a vacuum degree of 0.096-0.098 MPa to obtain the second reaction mixture system.

[0019] Nitrogen gas was introduced into the second reaction mixture system, and the temperature was rapidly reduced to 88-92°C. Hydrogen peroxide was then added for bleaching. The mixture was kept at the temperature and stirred indirectly. After 2 hours, the mixture was discharged, dried, and the component B was obtained.

[0020] Further, the weight ratio of the sorbitol, the stearic acid, the alkaline catalyst, the phosphoric acid and the hydrogen peroxide is (820-830):(1150-1250):(15-20):(1-5):(10-15).

[0021] Furthermore, the preparation method of component C includes the following steps:

[0022] Deionized water, maleic anhydride, and 28% hydrogen peroxide were added sequentially to a reaction vessel and mixed. The mixture was heated to 40–60°C and reacted for 2–4 hours to obtain the intermediate product system.

[0023] After adding phosphomolybdic acid as a catalyst to the intermediate product system, the temperature was slowly increased at a rate of 6°C / h. When the temperature reached 70-75°C, the heating was stopped. The reaction was maintained at 70-75°C for 18-24 hours. The temperature was then increased to 105-115°C, and the hydrolysis reaction was carried out for 2-5 hours to obtain a solution containing epoxy succinic acid.

[0024] The solution containing epoxy succinic acid was cooled with cooling water. When the temperature dropped to 20-28°C, ice-salt water was used instead. When the temperature dropped to 6-8°C, it crystallized naturally. Then, it was filtered by a rotary vacuum pump and dried to constant weight to obtain component C.

[0025] The weight ratio of deionized water, maleic anhydride, 28% hydrogen peroxide, and phosphomolybdic acid is (15-25):(15-25):(25-35):1.

[0026] Furthermore, the basalt fiber is a short-cut fiber with a diameter of 15–22 μm and a length of 15–30 mm.

[0027] Secondly, this application provides a method for preparing the basalt fiber anti-cracking agent according to any one of the first aspects, the preparation method comprising the following steps:

[0028] Components A, B, C, heavy calcium carbonate powder, and basalt fiber are added to water and heated and stirred until a thick consistency is reached to obtain the first mixture.

[0029] Under negative pressure, the first mixture is subjected to liquid nitrogen freezing treatment, and then restored to normal temperature and pressure to obtain the second mixture;

[0030] The second mixture is subjected to low-temperature plasma treatment to obtain the basalt fiber anti-cracking agent.

[0031] Furthermore, the operating parameters of the liquid nitrogen freezing treatment include: pressure of 50-60 kPa and time of 15-25 minutes; the operating parameters of the low-temperature plasma treatment include: working gas is oxygen, gas pressure is 75-90 Pa, discharge power is 150-200 W, discharge treatment time is 30-50 s, and discharge form is glow discharge.

[0032] Thirdly, the embodiments of this application provide the application of the basalt fiber anti-cracking agent as described in any one of the first aspects, and / or the basalt fiber anti-cracking agent obtained by the preparation method as described in any one of the second aspects, in the preparation of concrete products.

[0033] The technical solutions provided in this application have at least the following advantages compared with the prior art:

[0034] This application provides a basalt fiber anti-cracking agent, its preparation method, and its application. By using specific components A, B, and C in combination with heavy calcium carbonate powder and basalt fiber, a basalt fiber anti-cracking agent with excellent crack resistance is obtained. It can be applied to the manufacture of building materials such as concrete and has broad practical application value. Detailed Implementation

[0035] To make the objectives, technical solutions, and advantages of the embodiments of this application clearer, the technical solutions of this application will be clearly and completely described below in conjunction with the embodiments of this application. Obviously, the described embodiments are only some embodiments of this application, not all embodiments. Based on the embodiments of this application, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of this application.

[0036] Unless otherwise specified, all raw materials, reagents, instruments and equipment used in this application can be purchased from the market or prepared by existing methods.

[0037] In a first aspect, this application provides a basalt fiber anti-cracking agent, which, by weight, comprises the following components:

[0038] Component A 10-20 parts, component B 15-25 parts, component C 1-5 parts, heavy calcium carbonate powder 40-60 parts, and basalt fiber 5-15 parts;

[0039] Component A is obtained by refining, concentrating and crystallizing glucose as a starting material using a hydrogenation method;

[0040] Component B is obtained by using sorbitol as a starting material, followed by phosphoric acid-catalyzed dehydration to anhydride reaction and esterification reaction with stearic acid.

[0041] The preparation of component C includes: reacting maleic anhydride and hydrogen peroxide as raw materials to obtain an intermediate product system; hydrolyzing the intermediate product system with phosphomolybdic acid to obtain a solution containing epoxy succinic acid; cooling and crystallizing the solution containing epoxy succinic acid, and then filtering to obtain component C.

[0042] This application provides a basalt fiber anti-cracking agent, its preparation method, and its application. By using specific components A, B, and C in combination with heavy calcium carbonate powder and basalt fiber, a basalt fiber anti-cracking agent with excellent crack resistance is obtained. It can be applied to the manufacture of building materials such as concrete and has broad practical application value.

[0043] In some specific embodiments, the basalt fiber anti-cracking agent comprises the following components by weight:

[0044] Component A 15-20 parts, component B 15-20 parts, component C 1-5 parts, heavy calcium carbonate powder 50-60 parts, and basalt fiber 10-15 parts.

[0045] In some specific embodiments, the basalt fiber anti-cracking agent comprises the following components by weight:

[0046] Component A: 17 parts; Component B: 18 parts; Component C: 2 parts; Heavy calcium carbonate powder: 53 parts; Basalt fiber: 10 parts.

[0047] In some specific embodiments, the preparation method of component A includes the following steps:

[0048] Using glucose as raw material, pure water is used for saccharification at a concentration of 45%–52%, and the pH is adjusted to 7.5–8.0 to obtain a colorless or very pale yellow glucose solution. A nickel powder catalyst, comprising 1–3 wt% of the glucose solution, is added to a glucose solution feed metering tank and mixed well. This mixture is then pumped into a hydrogenation reactor using a high-pressure feed pump. After feeding is complete, the hydrogenation reactor is stirred at a speed of 240–360 r / min, and the hydrogen pressure is increased to a set pressure of 10.0 MPa. Simultaneously, the jacket steam is activated. The temperature of the liquid mixture is gradually increased and maintained at 110-145℃. The hydrogenation reaction is continued for 2-3 hours within this temperature range. After the hydrogenation reaction is completed, the mixture is purified by decolorization and ion exchange. The purified and decolorized liquid is clear and transparent, yielding a liquid product. Then, in a static crystallizer, the concentration of the liquid product is controlled at 40-60 wt%, and the crystallization temperature is controlled at 50-60℃. After the crystallization process is completed, the crystallized product is separated into solid and liquid components using a centrifuge. The separated wet cake is then spray-dried to obtain component A.

[0049] In some specific embodiments, the preparation method of component B includes the following steps:

[0050] Sorbitol was added to a vacuum reactor, along with phosphoric acid. The mixture was stirred and heated to 145-150°C. The mixture was then dehydrated under vacuum to form anhydride for 3-4 hours. Nitrogen gas was then introduced to release the vacuum, and samples were taken for testing. The required hydroxyl value of the sorbitol anhydride was 1260-1380, thus obtaining the first reaction mixture system.

[0051] Stearic acid was added to the first reaction mixture system, and an alkaline catalyst was added under stirring. Esterification was carried out under vacuum at a temperature of 200-205℃ for 3-4 hours and a vacuum degree of 0.096-0.098 MPa to obtain the second reaction mixture system.

[0052] Nitrogen gas was introduced into the second reaction mixture system, and the temperature was rapidly reduced to 88-92°C. Hydrogen peroxide was then added for bleaching. The mixture was kept at the temperature and stirred indirectly. After 2 hours, the mixture was discharged, dried, and the component B was obtained.

[0053] In some specific embodiments, the preparation method of component C includes the following steps:

[0054] Deionized water, maleic anhydride, and 28% hydrogen peroxide were added sequentially to a reaction vessel and mixed. The mixture was heated to 40–60°C and reacted for 2–4 hours to obtain the intermediate product system.

[0055] Add phosphomolybdic acid as a catalyst to the intermediate product system and slowly raise the temperature at a rate of 6°C / h; when the temperature reaches 70-75°C, stop raising the temperature; (3) keep the reaction at 70-75°C for 18-24 hours; then raise the temperature to 105-115°C and hydrolyze for 2-5 hours to obtain a solution containing epoxy succinic acid.

[0056] The solution containing epoxy succinic acid was cooled with cooling water. When the temperature dropped to 20-28°C, ice-salt water was used instead. When the temperature dropped to 6-8°C, it crystallized naturally. Then, it was filtered by a rotary vacuum pump and dried to constant weight to obtain component C.

[0057] The weight ratio of deionized water, maleic anhydride, 28% hydrogen peroxide, and phosphomolybdic acid is (15-25):(15-25):(25-35):1.

[0058] Preferably, the preparation method of component C includes the following steps:

[0059] (1) Add 1000 kg of deionized water, 1000 kg of maleic anhydride, and 1500 kg of hydrogen peroxide with a mass concentration of 28% to the reactor in sequence; heat to 50°C and react for 3 hours.

[0060] (2) Add 50 kg of phosphomolybdic acid as a catalyst to the product obtained in step 1 and slowly raise the temperature at a rate of 6 °C / h; when the temperature reaches 72 °C, stop raising the temperature.

[0061] (3) The reaction was kept at 72℃ for 20 hours; then the temperature was raised to 110℃ and the hydrolysis reaction was carried out for 3.5 hours to obtain a solution containing epoxy succinic acid.

[0062] (4) Cool the solution containing epoxy succinic acid with cooling water. When the temperature drops to about 25°C, switch to ice-salt water. When the temperature drops to 6-8°C, crystallize naturally. Then filter it with a rotary vacuum pump (vacuum degree 0.08; filter screen pore size 15-20 micrometers) to obtain C crystalline coarse matter and the first mother liquor as filtrate. Then dry the coarse matter (crystalline matter) in a 50°C drying equipment to constant weight to obtain crystals. After pulverizing the crystals, component C can be obtained.

[0063] In some specific embodiments, the basalt fibers are chopped fibers with a diameter of 15–22 μm and a length of 15–30 mm.

[0064] Secondly, based on a general inventive concept, this application provides a method for preparing the basalt fiber anti-cracking agent according to any one of the first aspects, the preparation method comprising the following steps:

[0065] Components A, B, C, heavy calcium carbonate powder, and basalt fiber are added to water and heated and stirred until a thick consistency is reached to obtain the first mixture.

[0066] Under negative pressure, the first mixture is subjected to liquid nitrogen freezing treatment, and then restored to normal temperature and pressure to obtain the second mixture;

[0067] The second mixture is subjected to low-temperature plasma treatment to obtain the basalt fiber anti-cracking agent.

[0068] The preparation method of the basalt fiber anti-cracking agent provided in this application embodiment is simple, requires no additional specific equipment, and is suitable for mass industrial production. Furthermore, this preparation method of the basalt fiber anti-cracking agent is based on the basalt fiber anti-cracking agent described in any one of the first aspects, and therefore possesses at least the beneficial effects brought about by the technical solutions described in any one of the first aspects, which will not be elaborated further here.

[0069] In some specific embodiments, the working parameters of the liquid nitrogen freezing treatment include: pressure of 50-60 kPa and time of 15-25 minutes; the working parameters of the low-temperature plasma treatment include: working gas is oxygen, gas pressure is 75-90 Pa, discharge power is 150-200 W, discharge treatment time is 30-50 s, and discharge form is glow discharge.

[0070] It should be noted that, unless otherwise specified or limited, the raw materials used in the basalt fiber anti-cracking agent and its preparation method provided in this application embodiment can all be commercially available products; at the same time, the process steps and parameters involved can be carried out in accordance with the existing basalt fiber anti-cracking agent preparation process or using existing equipment in a conventional operating manner.

[0071] Thirdly, the embodiments of this application provide the application of the basalt fiber anti-cracking agent as described in any one of the first aspects, and / or the basalt fiber anti-cracking agent obtained by the preparation method as described in any one of the second aspects, in the preparation of concrete products.

[0072] The present application is further illustrated below with reference to specific embodiments. It should be understood that these embodiments are for illustrative purposes only and are not intended to limit the scope of the application. Experimental methods in the following embodiments that do not specify specific conditions are generally determined according to national standards. If there is no corresponding national standard, then general international standards, conventional conditions, or conditions recommended by the manufacturer are followed.

[0073] Example 1

[0074] This example provides a basalt fiber anti-cracking agent, which, by weight, comprises the following components:

[0075] Component A: 17 parts; Component B: 18 parts; Component C: 2 parts; Heavy calcium carbonate powder: 53 parts; Basalt fiber (specifically, chopped fiber): 10 parts.

[0076] The preparation method of the above-mentioned basalt fiber anti-cracking agent includes the following steps:

[0077] Step (1) Preparation of component A: Using glucose as raw material, pure water is used for sugar saccharification, with a sugar concentration of 48% and pH adjusted to 7.5-8.0, to obtain a colorless or very pale yellow glucose solution; the nitrated catalyst is placed in the glucose solution feed metering tank, and after mixing with the glucose solution, it is pumped into the hydrogenation reactor using a high-pressure feed pump; after the feed is completed, the hydrogenation reactor is stirred at a stirring speed of 280 r / min, and the hydrogen pressure is increased to the set pressure of 10.0 MPa. At the same time, the jacket steam is turned on to gradually raise the temperature of the mixture and maintain it at 135-140℃. The hydrogenation reaction is continued in this temperature range for 2-3 hours. After the hydrogenation reaction is completed, decolorization and ion exchange are used for purification. The purified and decolorized liquid is clear and transparent, and a liquid product is obtained; then in a static crystallizer, the concentration of the liquid product is controlled at 50 wt%, and the crystallization temperature is 55℃. After the crystallization process is completed, a centrifuge is used to separate the solid and liquid products. The separated wet cake is spray-dried to obtain component A;

[0078] Step (2), Preparation of component B: Sorbitol is added to a vacuum reactor, phosphoric acid is added, the mixture is stirred and heated, and vacuum dehydrated into anhydride at 148°C for 3.5 hours. Then nitrogen is purged and the vacuum is released. Samples are taken for testing. The required hydroxyl value of sorbitol anhydride is 1260-1380, and the first reaction mixture system is obtained.

[0079] Stearic acid was added to the first reaction mixture system, and an alkaline catalyst was added under stirring conditions. Esterification was carried out under vacuum at a temperature of 202°C for 3.5 hours and a vacuum degree of 0.096-0.098 MPa to obtain the second reaction mixture system.

[0080] Nitrogen gas was introduced into the second reaction mixture system, and the temperature was rapidly reduced to 90°C. Hydrogen peroxide was then added for bleaching. The mixture was kept at the temperature and stirred indirectly. After 2 hours, the mixture was discharged, dried, and the component B was obtained.

[0081] Step (3), Preparation of component C: Add 1000 kg of deionized water, 1000 kg of maleic anhydride, and 1500 kg of 28% hydrogen peroxide to the reactor in sequence; heat to 50°C and react for 3 hours; add 50 kg of phosphomolybdic heteropoly acid as a catalyst to the product obtained in the above steps and slowly heat at a rate of 6°C / h; stop heating when the temperature reaches 72°C; keep the temperature at 72°C for 20 hours; then heat to 110°C for hydrolysis reaction 3. After 5 hours, a solution containing epoxy succinic acid was obtained. The solution containing epoxy succinic acid was cooled with cooling water. When the temperature dropped to about 25°C, ice-salt water was used. When the temperature dropped to 6-8°C, it crystallized naturally. Then, it was filtered by a rotary vacuum pump (vacuum degree 0.08; filter screen pore size 15-20 micrometers) to obtain C crystalline coarse matter and the first mother liquor as filtrate. The coarse matter (crystalline matter) was then placed in a drying device at 50°C and dried to constant weight to obtain crystals. The crystals were then powdered to obtain component C.

[0082] Step (4) Preparation of basalt fiber anti-cracking agent: Components A, B, and C, heavy calcium carbonate powder and basalt fiber are added to water and heated and stirred until thick to obtain a first mixture; under negative pressure, the first mixture is subjected to liquid nitrogen freezing treatment, and then restored to room temperature and pressure to obtain a second mixture; the second mixture is subjected to low-temperature plasma treatment to obtain the basalt fiber anti-cracking agent; the working parameters of the liquid nitrogen freezing treatment include: pressure of 55 kPa and time of 20 minutes; the working parameters of the low-temperature plasma treatment include: working gas is oxygen, gas pressure is 85 Pa, discharge power is 180 W, discharge treatment time is 40 s, and discharge form is glow discharge.

[0083] Example 2

[0084] This example provides a basalt fiber anti-cracking agent and its preparation method. The only difference from Example 1 is that, by weight, the basalt fiber anti-cracking agent includes the following components: 10 parts of component A, 15 parts of component B, 1 part of component C, 40 parts of heavy calcium carbonate powder, and 5 parts of basalt fiber.

[0085] Example 3

[0086] This example provides a basalt fiber anti-cracking agent and its preparation method. The only difference from Example 1 is that, by weight, the basalt fiber anti-cracking agent includes the following components: 20 parts of component A, 25 parts of component B, 5 parts of component C, 60 parts of heavy calcium carbonate powder, and 15 parts of basalt fiber.

[0087] Example 4

[0088] This example provides a basalt fiber anti-cracking agent and its preparation method. The only difference from Example 1 is that, by weight, the basalt fiber anti-cracking agent includes the following components: 15 parts of component A, 20 parts of component B, 5 parts of component C, 60 parts of heavy calcium carbonate powder, and 13 parts of basalt fiber.

[0089] Comparative Example 1

[0090] This example provides a basalt fiber anti-cracking agent and its preparation method. The only difference from Example 1 is that the amount of component A is 0 parts, and its preparation steps are omitted.

[0091] Comparative Example 2

[0092] This example provides a basalt fiber anti-cracking agent and its preparation method. The only difference from Example 1 is that the amount of component B is 0 parts, and its preparation steps are omitted.

[0093] Comparative Example 3

[0094] This example provides a basalt fiber anti-cracking agent and its preparation method. The only difference from Example 1 is that the amount of component C is 0 parts, and its preparation steps are omitted.

[0095] Comparative Example 4

[0096] This example provides a basalt fiber anti-cracking agent and its preparation method. The only difference from Example 1 is that step (4) of preparing the basalt fiber anti-cracking agent is adjusted as follows: Component A, Component B, Component C, heavy calcium carbonate powder and basalt fiber are added to water and heated and stirred until thick to obtain a first mixture; under negative pressure, the first mixture is subjected to liquid nitrogen freezing treatment, and then restored to normal temperature and pressure to obtain the basalt fiber anti-cracking agent; the working parameters of the liquid nitrogen freezing treatment include: pressure of 55 kPa and time of 20 minutes.

[0097] Comparative Example 5

[0098] This example provides a basalt fiber anti-cracking agent and its preparation method. The only difference from Example 1 is that step (4) of preparing the basalt fiber anti-cracking agent is adjusted as follows: Component A, Component B, Component C, heavy calcium carbonate powder and basalt fiber are added to water and heated and stirred until thick to obtain a first mixture; the first mixture is subjected to low-temperature plasma treatment to obtain the basalt fiber anti-cracking agent; the working parameters of the low-temperature plasma treatment include: working gas is oxygen, gas pressure is 85 Pa, discharge power is 180 W, discharge treatment time is 40 s, and discharge form is glow discharge.

[0099] Test case

[0100] In this example, the basalt fiber anti-cracking agents obtained in Examples 1-4 and Comparative Examples 1-5 were subjected to crack resistance performance tests.

[0101] Test Method: The basalt fiber crack-resistant agents obtained in Examples 1-4 and Comparative Examples 1-5 were added to concrete mortar at a mass percentage of 3.0% as experimental groups. The reference concrete mortar without additives was used as a blank group. The concrete mortar from both experimental and blank groups was evenly applied to a substrate with a side length of 100mm × 100mm, ensuring a thickness of 100mm. After natural drying, specimens were obtained. After 28 days, crack resistance tests were conducted on the specimens sequentially, according to the early crack resistance test method in GB / T50082—2009 "Standard for Test Methods of Long-Term Performance and Durability of Ordinary Concrete". An 800mm × 600mm × 100mm flat thin-plate mold containing 7 crack inducers was used. Additionally, the wind speed at the center of the specimen surface was maintained at no less than 5m / s. After the test, the crack width and length were recorded. According to CECS38—2004 "Technical Specification for Fiber Reinforced Concrete Structures", the crack width and length were calculated using the formula η = (A...). mer -A fer ) / A mer Among them, A mer A fer The crack reduction coefficient η was calculated for the total crack area per unit area of ​​the reference concrete and fiber-reinforced concrete, and the results are shown in Table 1. The larger the crack reduction coefficient η is, the better the crack resistance.

[0102] Table 1

[0103]

[0104]

[0105] As shown in Table 1, compared with the comparative example, the basalt fiber anti-cracking agent provided in this application has a significant effect, and the composition provided in Example 1 has the best effect.

[0106] In summary, the embodiments of this application provide a basalt fiber crack-resistant agent, its preparation method, and its application. By using specific components A, B, and C in combination with heavy calcium carbonate powder and basalt fiber, a basalt fiber crack-resistant agent with excellent crack resistance is obtained. It can be applied to the manufacture of building materials such as concrete and has broad practical application value.

[0107] Various embodiments of this application may exist in the form of a range; it should be understood that the description in the form of a range is merely for convenience and brevity and should not be construed as a hard limitation on the scope of this application; therefore, it should be considered that the range description has specifically disclosed all possible sub-ranges and single numerical values ​​within that range. For example, it should be considered that the range description from 1 to 6 has specifically disclosed sub-ranges such as from 1 to 3, from 1 to 4, from 1 to 5, from 2 to 4, from 2 to 6, from 3 to 6, etc., and single numbers within the range, such as 1, 2, 3, 4, 5, and 6, regardless of the range. Furthermore, whenever a numerical range is referred to herein, it means including any referenced number (fraction or integer) within the referred range.

[0108] The above description is merely a specific embodiment of this application, enabling those skilled in the art to understand or implement this application. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of this application. Therefore, this application is not to be limited to the embodiments shown herein, but is to be accorded the widest scope consistent with the principles and novel features claimed herein.

Claims

1. A basalt fiber crack-resistant agent, characterized in that, The basalt fiber anti-cracking agent comprises the following components in parts by weight: Component A 10-20 parts, Component B 15-25 parts, Component C 1-5 parts, Heavy calcium carbonate powder 40-60 parts, and basalt fiber 5-15 parts; The preparation method of component A The process includes the following: Using glucose as raw material, pure water is used for saccharification at a concentration of 45%–52%, and the pH is adjusted to 7.5–8.0 to obtain a colorless or very pale yellow glucose solution. A nickel powder catalyst, comprising 1–3 wt% of the glucose solution, is added to a glucose solution feed metering tank and mixed well. The mixture is then pumped into a hydrogenation reactor using a high-pressure feed pump. After feeding is complete, the hydrogenation reactor is stirred at a speed of 240–360 rpm. The flow rate was increased by r / min, and the hydrogen pressure was raised to the set pressure of 10.0 MPa. At the same time, the jacket steam was turned on, and the temperature of the liquid mixture was gradually increased and maintained at 110~145℃. The hydrogenation reaction was continued in this temperature range for 2~3 hours. After the hydrogenation reaction was completed, the mixture was purified by decolorization and ion exchange. The purified and decolorized liquid was clear and transparent, and a liquid product was obtained. Then, in a static crystallizer, the concentration of the liquid product was controlled at 40-60 wt%, and the crystallization temperature was controlled at 50-60℃. After the crystallization process was completed, the crystallized product was separated into solid and liquid by centrifuge. The separated wet cake was spray-dried to obtain component A. The preparation method of component B The process includes the following: Sorbitol was added to a vacuum reactor, along with phosphoric acid. The mixture was stirred and heated to 145-150°C. The mixture was then dehydrated under vacuum to form anhydride for 3-4 hours. Nitrogen gas was then introduced to release the vacuum, and samples were taken for testing. The required hydroxyl value of the sorbitol anhydride was 1260-1380, thus obtaining the first reaction mixture system. Stearic acid was added to the first reaction mixture system, and an alkaline catalyst was added under stirring. Esterification was carried out under vacuum at a temperature of 200-205℃ for 3-4 hours and a vacuum degree of 0.096-0.098 MPa to obtain the second reaction mixture system. Nitrogen gas was introduced into the second reaction mixture system, and the temperature was rapidly reduced to 88-92°C. Then hydrogen peroxide was added for bleaching, and the mixture was kept at the temperature with indirect stirring. After 2 hours, the mixture was discharged, dried, and the component B was obtained. The preparation method of component C includes the following steps: Deionized water, maleic anhydride, and 28% hydrogen peroxide were added sequentially to a reaction vessel and mixed. The mixture was heated to 40-60°C and reacted for 2-4 hours to obtain the intermediate product system. After adding phosphomolybdic acid as a catalyst to the intermediate product system, the temperature is slowly increased at a rate of 6°C / h. When the temperature reaches 70-75°C, the heating is stopped. The reaction is maintained at 70-75°C for 18-24 hours. The temperature is then increased to 105-115°C, and the hydrolysis reaction is carried out for 2-5 hours to obtain a solution containing epoxy succinic acid. The solution containing epoxy succinic acid was cooled with cooling water. When the temperature dropped to 20-28°C, ice-salt water was used instead. When the temperature dropped to 6-8°C, it crystallized naturally. Then, it was filtered by a rotary vacuum pump and dried to constant weight to obtain component C. The weight ratio of the deionized water, maleic anhydride, 28% hydrogen peroxide, and phosphomolybdic acid is (15~25):(15~25):(25~35):

1.

2. The basalt fiber anti-cracking agent according to claim 1, characterized in that, The basalt fiber anti-cracking agent comprises the following components in parts by weight: Component A 15-20 parts, component B 15-20 parts, component C 1-5 parts, heavy calcium carbonate powder 50-60 parts, and basalt fiber 10-15 parts.

3. The basalt fiber anti-cracking agent according to claim 1, characterized in that, The basalt fiber anti-cracking agent comprises the following components in parts by weight: Component A: 17 parts; Component B: 18 parts; Component C: 2 parts; Heavy calcium carbonate powder: 53 parts; Basalt fiber: 10 parts.

4. A method for preparing the basalt fiber anti-cracking agent according to any one of claims 1 to 3, characterized in that, The preparation method includes the following steps: Components A, B, C, heavy calcium carbonate powder, and basalt fiber are added to water and heated and stirred until a thick consistency is reached to obtain the first mixture. Under negative pressure, the first mixture is subjected to liquid nitrogen freezing treatment, and then restored to normal temperature and pressure to obtain the second mixture; The second mixture is subjected to low-temperature plasma treatment to obtain the basalt fiber anti-cracking agent.

5. The method for preparing the basalt fiber anti-cracking agent according to claim 4, characterized in that, The working parameters for the liquid nitrogen freezing treatment include: pressure of 50-60 kPa and time of 15-25 minutes; the working parameters for the low-temperature plasma treatment include: working gas is oxygen, gas pressure is 75-90 Pa, discharge power is 150-200 W, discharge treatment time is 30-50 s, and discharge form is glow discharge.

6. The basalt fiber anti-cracking agent according to any one of claims 1 to 3, and / or the basalt fiber anti-cracking agent obtained by the preparation method according to any one of claims 4 to 5, in the preparation of concrete products.

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