A quick-setting cement-based repair material and preparation method thereof
By preparing low-viscosity fast-setting cement-based repair materials and utilizing cardanol structure and siloxane technology, the problems of high viscosity and short gel time of epoxy resin were solved, the fluidity and bonding of the material were improved, and the repair effect was enhanced.
Patent Information
- Application Number
- CN202510309943.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-03-17
- Publication Date
- 2025-09-23
- Estimated Expiration
- 2045-03-17
AI Technical Summary
Existing epoxy resin repair materials have high viscosity and poor fluidity, making it difficult to enter small cracks. They also have short gelling time and short construction operation time, which affects the repair effect.
Low-viscosity epoxy resin, iron tailings sand and ceramic powder are combined with epoxy polyurethane to prepare a fast-setting cement-based repair material through specific steps. Cardanol structure and silanol oxidation technology are used to reduce viscosity and improve compatibility. Diluents and curing agents are added to ensure material uniformity and toughening effect.
The fluidity and rapid solidification of low-viscosity repair materials are achieved, the bonding and durability with the original road are improved, and the repair effect is enhanced.
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Abstract
Description
Technical Field
[0001] The invention relates to the technical field of lightweight building materials, and in particular to a quick-setting cement-based repair material and a preparation method thereof. Background Art
[0002] In recent years, the transportation and logistics industries have developed rapidly, and the load on roads has become increasingly heavier, and damage has become more frequent. Road damage often starts from a small area. If it is not repaired in time, it may cause traffic accidents and damage to a larger area. Therefore, road repair projects are one of the important tasks of municipal engineering and road management departments. Road repair materials play a decisive role in the entire repair process and repair effect. For cement concrete roads, if existing ordinary Portland cement concrete materials are used for repair, there will be long maintenance cycles and long road closures, which seriously affect the smooth flow of traffic. Therefore, it is very important to use repair materials with fast-hardening and early-strengthening properties to repair roads. Epoxy resin mortar, as a material with fast hardening, high strength, good adhesion and strong corrosion resistance, is a more ideal road repair material.
[0003] However, due to the high viscosity of epoxy resin, excessive viscosity means that the fluidity of the repair material is poor. For cracks with relatively small widths, it is difficult for the repair material to enter the crack, resulting in the repair material and the crack interface not being bonded together; the shorter gel time means that in actual construction operations, the construction operation time given is shorter. Summary of the Invention
[0004] In order to solve the above technical problems, the present invention provides a quick-setting cement-based repair material and a preparation method thereof.
[0005] The purpose of the present invention can be achieved through the following technical solutions:
[0006] A quick-setting cement-based repair material comprises the following raw materials in parts by weight: 100-120 parts of low-viscosity epoxy resin, 5-8 parts of epoxy polyurethane, 5-10 parts of diluent, 50-80 parts of iron tailings sand, 80-100 parts of ceramic powder, 300-500 parts of medium sand, and 30-50 parts of curing agent;
[0007] The low-viscosity epoxy resin is prepared by the following steps:
[0008] Step S1, adding cardanol and zinc acetate into a three-necked flask, introducing nitrogen to expel air, raising the temperature to 80-90° C., slowly adding dropwise a 35% formaldehyde aqueous solution by mass, and then keeping the temperature and reacting for 4 hours. After the reaction, the obtained product was washed three times with 55° C. deionized water to obtain reaction product 1;
[0009] In step S1, cardanol is first condensed with formaldehyde to prepare a reaction product 1;
[0010] Step S2, adding the obtained reaction product 1 and epichlorohydrin to a four-necked flask, adding tetrabutylammonium bromide, passing nitrogen to expel air, stirring at a constant speed and heating to 90-95° C., keeping the temperature for reaction for 4 hours, cooling to 60° C. after the reaction, adding sodium hydroxide, and continuing the reaction for 3 hours. After the reaction, washing the obtained product with deionized water until neutral and then rotary evaporation to obtain reaction product 2;
[0011] In step S2, the reaction product 1 reacts with epichlorohydrin, thereby introducing epoxy groups to prepare an intermediate product 2, which is an epoxy resin containing a cardanol structure.
[0012] Step S3: Add the reaction product 2 and KH570 to N,N-dimethylformamide, raise the temperature to 55-65° C., add azobisisobutyronitrile, stir at a constant speed and react for 4-6 hours. After the reaction is completed, a low-viscosity epoxy resin is obtained.
[0013] In step S3, azobisisobutyronitrile is used as an initiator to polymerize the reaction product 2 and KH570, and siloxane is introduced into the structure of the reaction product 2 to obtain a low-viscosity epoxy resin. On the one hand, the epoxy resin structure has a cardanol structure. The internal plasticizing effect of the cardanol C15 alkyl chain makes the epoxy resin have a lower viscosity, which is more suitable for the application of repair materials. On the other hand, the introduced siloxane structure can be hydrolyzed and then attached to the filler surface, thereby improving the compatibility of the inorganic filler and the epoxy resin and ensuring the uniform performance of the system.
[0014] Furthermore, the diluent is anhydrous ethanol or ethyl acetate.
[0015] Furthermore, the curing agent is phenalkamine T31 or polyamide resin.
[0016] Furthermore, in step S1, the dosage ratio of cardanol, zinc acetate and formaldehyde aqueous solution is controlled to be 1-2 g: 0.015-0.02 g: 15-25 mL.
[0017] Furthermore, in step S2, the dosage ratio of the reaction product 1, epichlorohydrin, sodium hydroxide and tetrabutylammonium bromide is controlled to be 0.5-1 g: 2-3 g: 0.2-0.4 g: 20 mL.
[0018] Furthermore, in step S3, the dosage ratio of the reaction product 2, KH570, azobisisobutyronitrile and N,N-dimethylformamide is controlled to be 1-2 g: 0.5-1.2 g: 0.08-0.12 g: 10 mL.
[0019] A method for preparing a quick-setting cement-based repair material comprises the following steps:
[0020] The raw materials are mixed, stirred evenly, and solidified to obtain a cement-based repair material.
[0021] Beneficial effects of the present invention:
[0022] The present invention prepares a fast-setting cement-based repair material. The added iron tailings and ceramic powder can reduce the linear expansion coefficient of the repair material, making it closer to the linear expansion coefficient of the original road concrete, thereby improving the bonding between the repair material and the original road and enhancing its durability. In addition, a low-viscosity epoxy resin is prepared. The epoxy resin structure has a cardanol structure. The internal plasticizing effect of the cardanol C15 alkyl chain gives the epoxy resin a low viscosity, making it more suitable for use as a repair material. In addition, the introduced siloxane structure can be hydrolyzed and can adhere to the filler surface, thereby improving the compatibility between the inorganic filler and the epoxy resin and ensuring the uniform performance of the system.
[0023] In addition, the present application also adds an epoxy polyurethane, which has good compatibility with low-viscosity epoxy resin, so that the epoxy polyurethane has a good toughening effect. DETAILED DESCRIPTION
[0024] The following is a clear and complete description of the technical solutions in the embodiments of the present invention. Obviously, the embodiments described are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making any creative efforts are within the scope of protection of the present invention.
[0025] Example 1: A rapid-setting cement-based repair material comprising the following raw materials in parts by weight: 100 parts of low-viscosity epoxy resin, 5 parts of epoxy polyurethane (refer to Preparation and Performance Study of Epoxy-Terminated Polyurethane Toughened Modified Epoxy Resin, by Tan Yanfang, Zhao Haipeng, etc.), 5 parts of diluent, 50 parts of iron ore tailings, 80 parts of ceramic powder, 300 parts of medium sand, and 30 parts of curing agent;
[0026] A method for preparing a quick-setting cement-based repair material comprises the following steps:
[0027] The raw materials are mixed, stirred evenly, and solidified to obtain a cement-based repair material.
[0028] The low-viscosity epoxy resin is prepared by the following steps:
[0029] Step S1, adding cardanol and zinc acetate to a three-necked flask, introducing nitrogen to expel the air, heating to 80°C, slowly adding dropwise a 35% formaldehyde aqueous solution by mass, and keeping warm and reacting for 4 hours after the addition is completed. After the reaction is completed, the obtained product is washed three times with 55°C deionized water to obtain reaction product 1, and the amount ratio of cardanol, zinc acetate and formaldehyde aqueous solution is controlled to be 1g:0.015g:15mL;
[0030] Step S2, adding the obtained reaction product 1 and epichlorohydrin to a four-necked flask, adding tetrabutylammonium bromide, introducing nitrogen to expel air, stirring at a uniform speed and heating to 90° C., keeping the temperature for reaction for 4 hours, cooling to 60° C. after the reaction, adding sodium hydroxide, and continuing the reaction for 3 hours. After the reaction, the obtained product is washed with deionized water until neutral and then rotary evaporated to obtain reaction product 2, and the amount ratio of reaction product 1, epichlorohydrin, sodium hydroxide and tetrabutylammonium bromide is controlled to be 0.5 g:2 g:0.2 g:20 mL;
[0031] Step S3, adding the reaction product 2 and KH570 to N, N-dimethylformamide, heating to 55 ° C, adding azobisisobutyronitrile, stirring at a uniform speed and reacting for 4-6 hours, and obtaining a low-viscosity epoxy resin after the reaction is completed. The amount ratio of the reaction product 2, KH570, azobisisobutyronitrile and N, N-dimethylformamide is controlled to be 1g:0.5g:0.08g:10mL.
[0032] The diluent is anhydrous ethanol or ethyl acetate.
[0033] The curing agent is phenalkamine T31 or polyamide resin.
[0034] Example 2: A rapid-setting cement-based repair material comprising the following raw materials in parts by weight: 110 parts of low-viscosity epoxy resin, 6 parts of epoxy polyurethane (refer to Preparation and Performance Study of Epoxy-Terminated Polyurethane Toughened Modified Epoxy Resin, by Tan Yanfang, Zhao Haipeng, etc.), 8 parts of diluent, 60 parts of iron ore tailings, 90 parts of ceramic powder, 400 parts of medium sand, and 40 parts of curing agent;
[0035] A method for preparing a quick-setting cement-based repair material comprises the following steps:
[0036] The raw materials are mixed, stirred evenly, and solidified to obtain a cement-based repair material.
[0037] The low-viscosity epoxy resin is prepared by the following steps:
[0038] Step S1, adding cardanol and zinc acetate to a three-necked flask, introducing nitrogen to expel the air, heating to 85°C, slowly adding dropwise a 35% formaldehyde aqueous solution by mass, and keeping warm and reacting for 4 hours after the addition is completed. After the reaction is completed, the obtained product is washed three times with 55°C deionized water to obtain reaction product 1, and the amount ratio of cardanol, zinc acetate and formaldehyde aqueous solution is controlled to be 1.5g:0.018g:20mL;
[0039] Step S2, adding the obtained reaction product 1 and epichlorohydrin to a four-necked flask, adding tetrabutylammonium bromide, introducing nitrogen to expel air, stirring at a uniform speed and heating to 94° C., keeping the temperature for reaction for 4 hours, cooling to 60° C. after the reaction, adding sodium hydroxide, and continuing the reaction for 3 hours. After the reaction, the obtained product is washed with deionized water until neutral and then rotary evaporated to obtain reaction product 2, and the amount ratio of reaction product 1, epichlorohydrin, sodium hydroxide and tetrabutylammonium bromide is controlled to be 0.8 g:2.5 g:0.3 g:20 mL;
[0040] Step S3, adding the reaction product 2 and KH570 to N, N-dimethylformamide, heating to 60 ° C, adding azobisisobutyronitrile, stirring at a uniform speed and reacting for 5 hours, and obtaining a low-viscosity epoxy resin after the reaction is completed. The amount ratio of the reaction product 2, KH570, azobisisobutyronitrile and N, N-dimethylformamide is controlled to be 1.5 g: 1 g: 0.1 g: 10 mL.
[0041] The diluent is anhydrous ethanol or ethyl acetate.
[0042] The curing agent is phenalkamine T31 or polyamide resin.
[0043] Example 3: A rapid-setting cement-based repair material, comprising the following raw materials in parts by weight: 20 parts of low-viscosity epoxy resin, 8 parts of epoxy polyurethane (refer to Preparation and Performance Study of Epoxy-Terminated Polyurethane Toughened Modified Epoxy Resin, by Tan Yanfang, Zhao Haipeng, etc.), 10 parts of diluent, 80 parts of iron ore tailings, 100 parts of ceramic powder, 500 parts of medium sand, and 50 parts of curing agent;
[0044] A method for preparing a quick-setting cement-based repair material comprises the following steps:
[0045] The raw materials are mixed, stirred evenly, and solidified to obtain a cement-based repair material.
[0046] The low-viscosity epoxy resin is prepared by the following steps:
[0047] Step S1, adding cardanol and zinc acetate to a three-necked flask, introducing nitrogen to expel the air, heating to 90°C, slowly adding dropwise a 35% formaldehyde aqueous solution by mass, and keeping warm and reacting for 4 hours after the addition is completed. After the reaction is completed, the obtained product is washed three times with 55°C deionized water to obtain reaction product 1, and the amount ratio of cardanol, zinc acetate and formaldehyde aqueous solution is controlled to be 2g:0.02g:25mL;
[0048] Step S2, adding the obtained reaction product 1 and epichlorohydrin to a four-necked flask, adding tetrabutylammonium bromide, introducing nitrogen to expel air, stirring at a uniform speed and heating to 95° C., keeping the temperature for reaction for 4 hours, cooling to 60° C. after the reaction, adding sodium hydroxide, and continuing the reaction for 3 hours. After the reaction, the obtained product is washed with deionized water until neutral and then rotary evaporated to obtain reaction product 2, and the amount ratio of reaction product 1, epichlorohydrin, sodium hydroxide and tetrabutylammonium bromide is controlled to be 1g:3g:0.4g:20mL;
[0049] Step S3, adding the reaction product 2 and KH570 to N, N-dimethylformamide, raising the temperature to 65 ° C, adding azobisisobutyronitrile, stirring at a uniform speed and reacting for 4-6 hours, and obtaining a low-viscosity epoxy resin after the reaction is completed. The amount ratio of the reaction product 2, KH570, azobisisobutyronitrile and N, N-dimethylformamide is controlled to be 2g:1.2g:0.12g:10mL.
[0050] The diluent is anhydrous ethanol or ethyl acetate.
[0051] The curing agent is phenalkamine T31 or polyamide resin.
[0052] Comparative Example 1: Compared with Example 1, this comparative example uses commercially available epoxy resin E51 instead of the low-viscosity epoxy resin of the present invention, and the rest is the same as Example 1.
[0053] Comparative Example 2: Compared with Example 1, this comparative example uses commercially available thermoplastic polyurethane instead of the epoxy polyurethane of the present invention.
[0054] According to the tensile bond strength test method and frost resistance test method in JGJ / T70-2009 "Test Methods for Basic Properties of Building Mortar", the properties of the rapid-setting cement-based repair materials prepared in Examples 1-3 and Comparative Examples 1-2 were tested. The results are shown in Table 1 below:
[0055] Table 1
[0056]
[0057] It can be seen from Table 1 above that the repair materials prepared in Examples 1-3 of the present invention have good mechanical properties.
[0058] The above content is merely an example and explanation of the concept of the present invention. Those skilled in the art may make various modifications or additions to the described specific embodiments or replace them in a similar manner. As long as they do not deviate from the concept of the invention or exceed the scope defined by the claims, they should all fall within the scope of protection of the present invention.
Claims
1. A quick-setting cement-based repair material, characterized in that: The raw materials include the following parts by weight: 100-120 parts of low-viscosity epoxy resin, 5-8 parts of epoxy polyurethane, 5-10 parts of diluent, 50-80 parts of iron tailings sand, 80-100 parts of ceramic powder, 300-500 parts of medium sand, and 30-50 parts of curing agent; The low-viscosity epoxy resin is prepared by the following steps: Step S1, adding cardanol and zinc acetate into a three-necked flask, introducing nitrogen to expel air, raising the temperature to 80-90° C., slowly adding dropwise a 35% formaldehyde aqueous solution by mass, and then keeping the temperature and reacting for 4 hours. After the reaction, the obtained product was washed three times with 55° C. deionized water to obtain reaction product 1; Step S2, adding the obtained reaction product 1 and epichlorohydrin to a four-necked flask, adding tetrabutylammonium bromide, passing nitrogen to expel air, stirring at a constant speed and heating to 90-95° C., keeping the temperature for reaction for 4 hours, cooling to 60° C. after the reaction, adding sodium hydroxide, and continuing the reaction for 3 hours. After the reaction, washing the obtained product with deionized water until neutral and then rotary evaporation to obtain reaction product 2; Step S3: Add the reaction product 2 and KH570 to N,N-dimethylformamide, raise the temperature to 55-65° C., add azobisisobutyronitrile, stir at a constant speed and react for 4-6 hours. After the reaction is completed, a low-viscosity epoxy resin is obtained.
2. The rapid-setting cement-based repair material according to claim 1, characterized in that: The diluent is anhydrous ethanol or ethyl acetate.
3. The rapid-setting cement-based repair material according to claim 1, characterized in that: The curing agent is phenalkamine T31 or polyamide resin.
4. The rapid-setting cement-based repair material according to claim 1, characterized in that: In step S1, the dosage ratio of cardanol, zinc acetate and formaldehyde aqueous solution is controlled to be 1-2 g: 0.015-0.02g:15-25mL.
5. The rapid-setting cement-based repair material according to claim 1, characterized in that: In step S2, the dosage ratio of the reaction product 1, epichlorohydrin, sodium hydroxide and tetrabutylammonium bromide is controlled to be 0.5-1 g: 2-3 g: 0.2-0.4 g: 20 mL.
6. The rapid-setting cement-based repair material according to claim 1, characterized in that: In step S3, the amount ratio of the reaction product 2, KH570, azobisisobutyronitrile and N,N-dimethylformamide is controlled to be 1-2 g: 0.5-1.2g: 0.08-0.12g: 10mL.
7. The method for preparing a rapid-setting cement-based repair material according to claim 1, characterized in that: The steps include: The raw materials are mixed, stirred evenly, and solidified to prepare a quick-setting cement-based repair material.
Citation Information
Patent Citations
Preparation method of novel cardanol modified epoxy resin
CN112250645A
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