Lepidolite slag water-based epoxy rapid repair mortar and preparation method thereof
By combining a modified lithium mica slag/sepiolite fiber/lithium titanate whisker composite with an epoxy resin curing system, the problems of insufficient compressive strength and impermeability of water-based epoxy emulsion repair mortar are solved, achieving a high-efficiency, environmentally friendly, and rapid repair effect, which is suitable for highway, bridge, and airport projects.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- JIANGXI BUILDING MATERIALS RES & DESIGN INST CO LTD
- Filing Date
- 2024-07-16
- Publication Date
- 2026-04-24
AI Technical Summary
Existing water-based epoxy emulsion repair mortars are insufficient in terms of compressive strength, impermeability, and rapid repair capabilities, making it difficult to meet the high requirements of special engineering fields such as highways, bridges, and airports.
A modified lithium mica slag/sepiolite fiber/lithium titanate whisker composite and epoxy resin curing system are adopted, combined with ordinary silicate cement and sulfoaluminate cement, and a modified amine water-based curing agent is used to accelerate the curing speed to form a dense system to improve compressive strength and impermeability. The compactness of the composite is enhanced by coupling agent.
It significantly improves the compressive strength, impermeability, crack resistance, dimensional stability and adhesion of mortar, meeting the needs of rapid repair, while reducing the environmental pollution caused by organic solvents.
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Abstract
Description
Technical Field
[0001] This invention relates to the field of repair polymer mortar technology, and in particular to a lithium mica slag water-based epoxy rapid repair mortar and its preparation method. Background Technology
[0002] Concrete is subject to long-term environmental corrosion, and its surface is prone to various defects. To improve the durability of concrete, surface repair is necessary. Polymer repair mortar is a new type of material widely used in the field of building maintenance. In particular, epoxy mortar has high bonding strength and good resistance to media erosion, and has broad application prospects. Current maintenance in special engineering fields such as highways, bridges, airports, and beam structures places high demands on repair mortars, including rapid repair, environmentally friendly construction, dimensional stability, excellent mechanical properties, and good impermeability.
[0003] Existing technologies disclose waterborne epoxy emulsion repair mortar and its preparation method. The raw materials include: 1.5%–24% waterborne epoxy emulsion, 0.15%–4.8% curing agent, 15%–30% cement, 33%–66% aggregate, 4%–8% mineral admixture, 0.01%–0.2% chemical additives, and 2%–8% water, with the sum of the weight percentages of all components being 100%. The waterborne epoxy emulsion repair mortar prepared by this patent exhibits excellent flexural strength, corrosion resistance, and workability; however, its compressive strength, impermeability, and rapid repair properties are generally average. Summary of the Invention
[0004] The purpose of this invention is to at least solve one of the technical problems existing in the prior art. To meet the above repair requirements, this invention provides a water-based epoxy rapid repair mortar made from lithium mica slag and its preparation method. Modification of ordinary silicate / sulfoaluminate cement blends and epoxy resin curing of modified amines accelerates the mortar repair speed. The modified lithium mica slag / sepiolite fiber / lithium titanate whisker composite reduces voids and defects between the resin matrix and aggregates, improving the compressive strength of the mortar. The polymer, cement gel material, lithium mica slag, sepiolite fiber, lithium titanate whiskers, and coarse and fine sand form a dense system. The addition of a coupling agent further enhances the tightness between the lithium mica slag, sepiolite fiber, lithium titanate whiskers, and polymer, improving the mortar's impermeability, crack resistance, and dimensional stability. The epoxy resin curing system improves the mortar's impermeability, adhesion, and toughness. In addition, compared with oil-soluble mortar systems, water-based epoxy mortar significantly reduces the environmental pollution caused by organic solvents.
[0005] The technical solution of the present invention is as follows:
[0006] A water-based epoxy rapid repair mortar made from lithium mica slag comprises the following raw materials in parts by weight:
[0007] Aggregate 1100-1300 parts, ordinary silicate cement 400-600 parts, sulfoaluminate cement 200-400 parts, water-based epoxy emulsion 100-120 parts, defoamer 0.5-0.7 parts, wetting agent 0.5-0.7 parts, water-reducing agent 3-5 parts, deionized water 140-160 parts, modified lithium mica slag / sepiolite fiber / lithium titanate whisker composite 30-60 parts, modified amine water-based curing agent 50-60 parts.
[0008] Preferably, the preparation raw materials include the following parts by weight:
[0009] Aggregate 1150-1250 parts, ordinary silicate cement 450-550 parts, sulfoaluminate cement 250-350 parts, waterborne epoxy emulsion 105-115 parts, defoamer 0.55-0.65 parts, wetting agent 0.55-0.65 parts, water-reducing agent 3.5-4.5 parts, deionized water 145-155 parts, modified lepidolite slag / sepiolite fiber / lithium titanate whisker composite 40-50 parts, modified amine waterborne curing agent 52-58 parts.
[0010] Preferably, the preparation method of the modified lithium mica slag / sepiolite fiber / lithium titanate whisker composite includes:
[0011] Lithium methane slag was ball-milled to obtain a specific surface area of 200-800 m². 2 / kg of lithium mica residue particles;
[0012] An epoxy group silane coupling agent is mixed with ethanol to prepare an epoxy group silane coupling agent / ethanol mixture;
[0013] Sepiol fiber was added to ethanol and ultrasonically dispersed. Potassium titanate whiskers were then added and ultrasonically dispersed again. The mixture was then dried to obtain a sepiolite fiber / potassium titanate whisker mixture.
[0014] The lithium mica slag particles are stirred, and the epoxy group silane coupling agent / ethanol mixture is sprayed onto the surface of the lithium mica slag particles. The sepiolite fiber and potassium titanate whisker mixture is then added and stirred evenly. The mixture is then heated to 80-100℃ for 30-90 minutes to obtain the modified lithium mica slag / sepiolite fiber / lithium titanate whisker composite.
[0015] Preferably, in the preparation method of the modified lepidolite slag / sepiolite fiber / lithium titanate whisker composite, the mass ratio of the epoxy group silane coupling agent to ethanol is 1-2:5-10, the mass ratio of the lepidolite slag to the epoxy group silane coupling agent is 30-60:1-2, and the mass ratio of the lepidolite slag, sepiolite fiber, and potassium titanate whiskers is 30-60:1-5:1-5.
[0016] Preferably, the epoxy group silane coupling agent is at least one of KBM-303, KBM-403, and KBE-402.
[0017] Preferably, the preparation method of the modified amine waterborne curing agent includes:
[0018] Triethylenetetramine and bisphenol A type epoxy resin were reacted at 60-70℃ for 3-5 hours to obtain an epoxy-amine adduct intermediate.
[0019] The double-ended epoxy polyether is reacted with the epoxy-amine adduct intermediate at 90-100°C for 2-5 hours to obtain the modified amine waterborne curing agent.
[0020] Preferably, in the preparation method of the modified amine waterborne curing agent, the molar ratio of triethylenetetramine to bisphenol A type epoxy resin is 2-3:1; and the molar ratio of the double-terminated epoxy polyether to the epoxy-amine adduct intermediate is 0.3-0.7:1.
[0021] Preferably, the method for preparing the aqueous epoxy emulsion includes:
[0022] 1) Epoxy resin E44 and polyethylene glycol 6000 with a molar ratio of 2:1 were added to a round-bottom flask and heated to 85°C under the protection of dry nitrogen. After the two were completely melted, they were mixed evenly with stirring to obtain an epoxy resin E44 / polyethylene glycol 6000 blend.
[0023] 2) The catalyst BF3 diethyl ether was diluted 10 times with acetone and added dropwise to the epoxy resin E44 / polyethylene glycol 6000 blend. The reaction was carried out at 85°C for 4 hours. Then, the mixture was vacuum distilled until no solvent was removed, thus obtaining the epoxy resin emulsifier.
[0024] 3) Add epoxy resin E44 and epoxy resin emulsifier to a stirred tank, heat to 70°C, and mix evenly at high speed of 1000-1500 r / min. Gradually add water to the stirred tank and prepare an aqueous epoxy emulsion with a solid content of 40%-60% by the phase inversion method. The mass ratio of epoxy resin E44 to epoxy resin emulsifier is 1:9.
[0025] The amount of catalyst BF3 diethyl ether added is 0.2 to 0.4% of the total mass of epoxy resin E44 and polyethylene glycol 6000.
[0026] Preferably, the aggregate is artificial sand or natural sand with a particle size of less than 4.75 mm and a mud content of ≤0.45 wt%.
[0027] The ordinary silicate cement is at least one of P·O 42.5, 52.5, and 62.5, and the sulfoaluminate cement is rapid-hardening sulfoaluminate cement.
[0028] A second aspect of this invention provides a method for preparing a water-based epoxy rapid repair mortar made from lithium mica slag, comprising the following steps:
[0029] S1. Weigh out the water-based epoxy emulsion, wetting agent, and deionized water according to the proportion, stir evenly for 0.5-2 minutes, then add the modified amine water-based curing agent and defoamer respectively and stir evenly to prepare a multi-component mixture.
[0030] S2. Weigh out the aggregate, ordinary silicate cement, sulfoaluminate cement, modified lepidolite slag / sepiolite fiber / lithium titanate whisker composite, and water-reducing agent according to the proportions, mix and stir for 0.5-2 minutes, then add the multi-component mixture from step S1 and stir together for 3-5 minutes to prepare lepidolite slag water-based epoxy rapid repair mortar.
[0031] This invention has at least one of the following beneficial effects:
[0032] This invention incorporates a modified lepidolite slag / sepiolite fiber / lithium titanate whisker composite. The finely ground lepidolite slag is mostly in the form of flakes and spherical particles, exhibiting good reinforcement and bulk density. This reduces voids and defects between the resin matrix and aggregate, improving the compressive strength of the mortar, as well as its flexural and tensile bond strength. Furthermore, this invention modifies the mixture of lepidolite slag, sepiolite fiber, and lithium titanate whiskers, reducing the agglomeration of sepiolite fiber and lithium titanate whiskers, thus enhancing the mortar's tensile strength. Lithium silicate fiber and lithium titanate whiskers are uniformly dispersed in lepidolite slag. The addition of an epoxy group silane coupling agent further enhances the tightness between the modified lepidolite slag / sepiolite fiber / lithium titanate whisker composite and the polymer, thereby enabling the sepiolite fiber and lithium titanate whiskers to be uniformly dispersed in the cement. The modified sepiolite fiber, lithium titanate whiskers, and lepidolite slag work together to significantly improve the mortar's impermeability, crack resistance, dimensional stability, compressive strength, flexural strength, and tensile bond strength. On the other hand, the repair mortar of this invention uses a certain proportion of ordinary silicate cement and sulfoaluminate cement to modify and shorten the setting time of the cement system. The modified amine waterborne curing agent increases the curing speed of epoxy resin, giving the mortar a rapid repair function. The epoxy resin improves the mortar's impermeability, adhesion, and toughness. In addition, the waterborne epoxy mortar greatly reduces the environmental pollution of organic solvents compared to oil-soluble mortar systems, greatly meeting the current demand for rapid repair of highways, bridges, airports, and beam structures that require environmental protection and quality assurance. Detailed Implementation
[0033] To make the technical problems solved, technical solutions, and beneficial effects of the present invention clearer, the present invention will be further described in detail below with reference to embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the present invention and are not intended to limit the present invention.
[0034] One embodiment of the present invention provides a lithium mica slag water-based epoxy rapid repair mortar, comprising the following raw materials in parts by weight:
[0035] Aggregate 1100-1300 parts, ordinary silicate cement 400-600 parts, sulfoaluminate cement 200-400 parts, water-based epoxy emulsion 100-120 parts, defoamer 0.5-0.7 parts, wetting agent 0.5-0.7 parts, water-reducing agent 3-5 parts, deionized water 140-160 parts, modified lithium mica slag / sepiolite fiber / lithium titanate whisker composite 30-60 parts, modified amine water-based curing agent 50-60 parts.
[0036] Preferably, the mass fractions of each raw material are as follows:
[0037] Aggregate 1150-1250 parts, ordinary silicate cement 450-550 parts, sulfoaluminate cement 250-350 parts, waterborne epoxy emulsion 105-115 parts, defoamer 0.55-0.65 parts, wetting agent 0.55-0.65 parts, water-reducing agent 3.5-4.5 parts, deionized water 145-155 parts, modified lepidolite slag / sepiolite fiber / lithium titanate whisker composite 40-50 parts, modified amine waterborne curing agent 52-58 parts.
[0038] More preferably, the mass fractions of each raw material are as follows:
[0039] 1100 parts aggregate, 400 parts ordinary silicate cement, 400 parts sulfoaluminate cement, 110 parts waterborne epoxy emulsion, 0.6 parts defoamer, 0.6 parts wetting agent, 4 parts water-reducing agent, 150 parts deionized water, 45 parts modified lithium mica slag / sepiolite fiber / lithium titanate whisker composite, and 50 parts modified amine waterborne curing agent.
[0040] The aggregate is artificial sand or natural sand with a particle size of less than 4.75 mm and a mud content of ≤0.45 wt%.
[0041] Ordinary Portland cement is at least one of P·O 42.5, 52.5, and 62.5; specifically, it can be P·O 52.5. Sulfoaluminate cement is rapid-hardening sulfoaluminate cement. Specifically, it can be rapid-hardening sulfoaluminate 52.5 cement (R·SAC 52.5).
[0042] The method for preparing the aqueous epoxy emulsion includes:
[0043] 1) Epoxy resin E44 and polyethylene glycol 6000 with a molar ratio of 2:1 were added to a round-bottom flask and heated to 85°C under the protection of dry nitrogen. After the two were completely melted, they were mixed evenly with stirring to obtain an epoxy resin E44 / polyethylene glycol 6000 blend.
[0044] 2) The catalyst BF3 diethyl ether was diluted 10 times with acetone and added dropwise to the epoxy resin E44 / polyethylene glycol 6000 blend. The reaction was carried out at 85°C for 4 hours. Then, the mixture was vacuum distilled until no solvent was removed, thus obtaining the epoxy resin emulsifier.
[0045] 3) Add epoxy resin E44 and epoxy resin emulsifier to a stirred tank, heat to 70°C, and mix evenly at high speed of 1000-1500 r / min. Gradually add water to the stirred tank and prepare an aqueous epoxy emulsion with a solid content of 40%-60% by the phase inversion method. The mass ratio of epoxy resin E44 to epoxy resin emulsifier is 1:9.
[0046] The amount of catalyst BF3 diethyl ether added is 0.2 to 0.4% of the total mass of epoxy resin E44 and polyethylene glycol 6000.
[0047] The preparation method of the modified lithium mica slag / sepiolite fiber / lithium titanate whisker composite includes:
[0048] Lithium methane slag was ball-milled to obtain a specific surface area of 200-800 m². 2 / kg of lithium mica residue particles;
[0049] An epoxy group silane coupling agent is mixed with ethanol to prepare an epoxy group silane coupling agent / ethanol mixture;
[0050] Sepiol fiber was added to ethanol and ultrasonically dispersed. Potassium titanate whiskers were then added and ultrasonically dispersed again. The mixture was then dried to obtain a sepiolite fiber / potassium titanate whisker mixture.
[0051] The lithium mica slag particles are stirred, and the epoxy group silane coupling agent / ethanol mixture is sprayed onto the surface of the lithium mica slag particles. The sepiolite fiber and potassium titanate whisker mixture is then added and stirred evenly. The mixture is then heated to 80-100℃ for 30-90 minutes to obtain the modified lithium mica slag / sepiolite fiber / lithium titanate whisker composite.
[0052] The mass ratio of the epoxy group silane coupling agent to ethanol is 1-2:5-10, the mass ratio of the lepidolite slag to the epoxy group silane coupling agent is 30-60:1-2, and the mass ratio of the lepidolite slag, sepiolite fiber, and potassium titanate whiskers is 30-60:1-5:1-5.
[0053] The epoxy group silane coupling agent is at least one of KBM-303, KBM-403, and KBE-402.
[0054] The preparation method of the modified amine waterborne curing agent includes:
[0055] Triethylenetetramine and bisphenol A type epoxy resin were reacted at 60-70℃ for 3-5 hours to obtain an epoxy-amine adduct intermediate.
[0056] The double-ended epoxy polyether is reacted with the epoxy-amine adduct intermediate at 90-100°C for 2-5 hours to obtain the modified amine waterborne curing agent.
[0057] The molar ratio of triethylenetetramine to bisphenol A epoxy resin is 2-3:1; preferably 2.2-2.8:1, and more preferably 2.5:1.
[0058] The molar ratio of the di-terminated epoxy polyether to the epoxy-amine adduct intermediate is 0.3-0.7:1, preferably 0.4-0.6:1, and more preferably 0.5:1.
[0059] The bisphenol A type epoxy resin is specifically bisphenol A type epoxy resin E51.
[0060] A second aspect of the present invention provides a method for preparing a water-based epoxy rapid repair mortar made from lithium mica slag, comprising:
[0061] S1. Weigh out the water-based epoxy emulsion, wetting agent, and deionized water according to the proportion, stir evenly for 0.5-2 minutes, then add the modified amine water-based curing agent and defoamer respectively and stir evenly to prepare a multi-component mixture.
[0062] S2. Weigh out the aggregate, ordinary silicate cement, sulfoaluminate cement, modified lepidolite slag / sepiolite fiber / lithium titanate whisker composite, and water-reducing agent according to the proportions, mix and stir for 0.5-2 minutes, then add the multi-component mixture from step S1 and stir together for 3-5 minutes to prepare lepidolite slag water-based epoxy rapid repair mortar.
[0063] The present invention will be further described in detail below with reference to specific embodiments, but the present invention is not limited to the following specific embodiments.
[0064] In the following examples and comparative examples, the wetting agent is model 9440, the water-reducing agent is model LonS-P, the defoamer is model AF-706, the double-terminated epoxy polyether is model SF-260 / 400, and the bisphenol A type epoxy resin is model E51 (Baling Petrochemical) and epoxy resin is model E44 (Baling Petrochemical).
[0065] Example 1
[0066] I. Preparation of modified lithium mica slag / sepiolite fiber / lithium titanate whisker composite:
[0067] 1) Take a certain amount of lepidolite slag and put it into a ball mill for ball milling treatment. Its specific surface area is 500 m². 2 / kg of granules, for later use;
[0068] 2) Simply mix 1g of KBM-303 with 5g of ethanol to prepare a KBM-303 / ethanol mixture;
[0069] 3) Add 5g of sepiolite fiber to 10g of ethanol and disperse by ultrasonication; continue to add 3g of potassium titanate whiskers and disperse by ultrasonication, then dry to obtain a mixture of sepiolite fiber and potassium titanate whiskers.
[0070] 4) Take 30g of lepidolite slag and put it into a mixer for stirring. At the same time, spray 6g of KBM-303 / ethanol mixture from step 2 onto the surface of the lepidolite slag particles. After the mixture is added, add 5g of sepiolite fiber / potassium titanate whisker mixture and mix evenly. Heat to 90℃ and dry for 50min to prepare modified lepidolite slag / sepiolite fiber / lithium titanate whisker composite.
[0071] II. Preparation of modified amine waterborne curing agent:
[0072] 1) Weigh triethylenetetramine (TETA) and bisphenol A epoxy resin E51 into a round-bottom flask at a molar ratio of 2.5:1 and react them. Heat the mixture to 70°C and react for 3 hours to prepare an epoxy-amine adduct intermediate.
[0073] 2) Weigh the double-ended epoxy polyether and the epoxy-amine adduct intermediate into a round-bottom flask at a molar ratio of 0.5:1 to carry out the addition reaction. Heat to 90°C and react for 3 hours to prepare the modified amine water-based curing agent.
[0074] III. Methods for preparing waterborne epoxy emulsions include:
[0075] 1) Epoxy resin E44 and polyethylene glycol 6000 with a molar ratio of 2:1 were added to a round-bottom flask and heated to 85°C under the protection of dry nitrogen. After the two were completely melted, they were mixed evenly with stirring to obtain an epoxy resin E44 / polyethylene glycol 6000 blend.
[0076] 2) The catalyst BF3 diethyl ether (0.3% of the total mass of epoxy resin E44 and polyethylene glycol 6000) was diluted 10 times with acetone and added dropwise to the epoxy resin E44 / polyethylene glycol 6000 blend. The catalytic reaction was carried out at 85°C for 4 hours. Then, the mixture was vacuum distilled until no solvent was removed, thus obtaining the epoxy resin emulsifier.
[0077] 3) Add epoxy resin E44 and epoxy resin emulsifier to a mixing tank, heat to 70°C, and mix evenly at high speed of 1200 r / min. Gradually add water to the mixing tank and prepare an aqueous epoxy emulsion with a solid content of 50% by the phase inversion method. The mass ratio of epoxy resin E44 to epoxy resin emulsifier is 1:9.
[0078] IV. Preparation of Lithium Mica Slag Waterborne Epoxy Rapid Repair Mortar:
[0079] (1) Weigh 100g of waterborne epoxy emulsion (solid content 50%), 0.6g of wetting agent and 150g of deionized water and stir evenly for 1min. Then add 50g of modified amine waterborne curing agent and 0.6g of defoamer and stir evenly to prepare a multi-component mixture.
[0080] (2) Weigh 1200g of aggregate, 600g of P·O 52.5, 200g of R·SAC 52.5, 30g of modified lithium mica slag / sepiolite fiber / lithium titanate whisker composite and 4g of water-reducing agent, put them into a mixer and mix for 1 minute. Then add the multi-component mixture from step 1 and mix them together for 3 minutes. Form mortar test blocks and perform relevant performance tests.
[0081] Example 2
[0082] I. Preparation of modified lithium mica slag / sepiolite fiber / lithium titanate whisker composite:
[0083] 1) Take a certain amount of lepidolite slag and put it into a ball mill for ball milling treatment. Its specific surface area is 500 m². 2 / kg of granules, for later use;
[0084] 2) Simply mix 1g of KBM-303 with 5g of ethanol to prepare a KBM-303 / ethanol mixture;
[0085] 3) Add 3g of sepiolite fiber to 10g of ethanol and disperse by ultrasonication; continue to add 2g of potassium titanate whiskers and disperse by ultrasonication, then dry to obtain a mixture of sepiolite fiber and potassium titanate whiskers.
[0086] 4) Take 30g of lepidolite slag and put it into a mixer for stirring. At the same time, spray 6g of KBM-303 / ethanol mixture from step 2 onto the surface of the lepidolite slag particles. After the mixture is added, add 5g of sepiolite fiber / potassium titanate whisker mixture and mix evenly. Heat to 90℃ and dry for 50min to prepare modified lepidolite slag / sepiolite fiber / lithium titanate whisker composite.
[0087] II. Preparation of modified amine water-based curing agent:
[0088] 1) Weigh triethylenetetramine (TETA) and bisphenol A epoxy resin E51 into a round-bottom flask at a molar ratio of 2.5:1 and react them. Heat the mixture to 70°C and react for 3 hours to prepare an epoxy-amine adduct intermediate.
[0089] 2) Weigh the double-ended epoxy polyether and the epoxy-amine adduct intermediate into a round-bottom flask at a molar ratio of 0.5:1 to carry out the addition reaction. Heat to 90°C and react for 3 hours to prepare the modified amine waterborne curing agent.
[0090] III. Methods for preparing waterborne epoxy emulsions include:
[0091] 1) Epoxy resin E44 and polyethylene glycol 6000 with a molar ratio of 2:1 were added to a round-bottom flask and heated to 85°C under the protection of dry nitrogen. After the two were completely melted, they were mixed evenly with stirring to obtain an epoxy resin E44 / polyethylene glycol 6000 blend.
[0092] 2) The catalyst BF3 diethyl ether (0.3% of the total mass of epoxy resin E44 and polyethylene glycol 6000) was diluted 10 times with acetone and added dropwise to the epoxy resin E44 / polyethylene glycol 6000 blend. The catalytic reaction was carried out at 85°C for 4 hours. Then, the mixture was vacuum distilled until no solvent was removed, thus obtaining the epoxy resin emulsifier.
[0093] 3) Add epoxy resin E44 and epoxy resin emulsifier to a mixing tank, heat to 70°C, and mix evenly at high speed of 1200 r / min. Gradually add water to the mixing tank and prepare an aqueous epoxy emulsion with a solid content of 50% by the phase inversion method. The mass ratio of epoxy resin E44 to epoxy resin emulsifier is 1:9.
[0094] IV. Preparation of Lithium Mica Slag Waterborne Epoxy Rapid Repair Mortar
[0095] (1) Weigh 100g of waterborne epoxy emulsion (solid content 50%), 0.6g of wetting agent and 150g of deionized water and stir evenly for 1min. Then add 50g of modified amine waterborne curing agent and 0.6g of defoamer and stir evenly to prepare a multi-component mixture.
[0096] (2) Weigh 1200g of aggregate, 400g of P·O 52.5, 400g of R·SAC 52.5, 30g of modified lithium mica slag / sepiolite fiber / lithium titanate whisker composite, and 4g of water-reducing agent, put them into a mixer and mix for 1 minute. Then add the multi-component mixture from step 1 and mix them together for 3 minutes. Form mortar test blocks and conduct relevant performance tests.
[0097] Example 3
[0098] I. Preparation of modified lithium mica slag / sepiolite fiber / lithium titanate whisker composite:
[0099] 1) Take a certain amount of lepidolite slag and put it into a ball mill for ball milling treatment. Its specific surface area is 500 m². 2 / kg of granules, for later use;
[0100] 2) Mix 2g of KBM-303 and 10g of ethanol in a certain ratio to prepare a KBM-303 / ethanol mixture;
[0101] 3) Add 3g of sepiolite fiber to 10g of ethanol and disperse by ultrasonication; continue to add 5g of potassium titanate whiskers and disperse by ultrasonication, then dry to obtain a mixture of sepiolite fiber and potassium titanate whiskers.
[0102] 4) Take 60g of lepidolite slag and put it into a mixer for stirring. At the same time, spray 12g of KBM-303 / ethanol mixture from step 2 onto the surface of the lepidolite slag particles. After the mixture is added, add 5g of sepiolite fiber / potassium titanate whisker mixture and mix evenly. Heat to 90℃ and dry for 50min to prepare modified lepidolite slag / sepiolite fiber / lithium titanate whisker composite.
[0103] II. Preparation of modified amine water-based curing agent:
[0104] 1) Weigh triethylenetetramine (TETA) and bisphenol A epoxy resin E51 into a round-bottom flask at a molar ratio of 2.5:1 and react them. Heat the mixture to 70°C and react for 3 hours to prepare an epoxy-amine adduct intermediate.
[0105] 2) Weigh the double-ended epoxy polyether and the epoxy-amine adduct intermediate into a round-bottom flask at a molar ratio of 0.5:1 to carry out the addition reaction. Heat to 90°C and react for 3 hours to prepare the modified amine waterborne curing agent.
[0106] III. Methods for preparing waterborne epoxy emulsions include:
[0107] 1) Epoxy resin E44 and polyethylene glycol 6000 with a molar ratio of 2:1 were added to a round-bottom flask and heated to 85°C under the protection of dry nitrogen. After the two were completely melted, they were mixed evenly with stirring to obtain an epoxy resin E44 / polyethylene glycol 6000 blend.
[0108] 2) The catalyst BF3 diethyl ether (0.3% of the total mass of epoxy resin E44 and polyethylene glycol 6000) was diluted 10 times with acetone and added dropwise to the epoxy resin E44 / polyethylene glycol 6000 blend. The catalytic reaction was carried out at 85°C for 4 hours. Then, the mixture was vacuum distilled until no solvent was removed, thus obtaining the epoxy resin emulsifier.
[0109] 3) Add epoxy resin E44 and epoxy resin emulsifier to a mixing tank, heat to 70°C, and mix evenly at high speed of 1200 r / min. Gradually add water to the mixing tank and prepare an aqueous epoxy emulsion with a solid content of 50% by the phase inversion method. The mass ratio of epoxy resin E44 to epoxy resin emulsifier is 1:9.
[0110] IV. Preparation of Lithium Mica Slag Water-Based Epoxy Rapid Repair Mortar
[0111] (1) Weigh 100g of waterborne epoxy emulsion (solid content 50%), 0.6g of wetting agent and 150g of deionized water and stir evenly for 1min. Then add 50g of modified amine waterborne curing agent and 0.6g of defoamer and stir evenly to prepare a multi-component mixture.
[0112] (2) Weigh 1200g of aggregate, 500g of P·O 52.5, 300g of R·SAC 52.5, 60g of modified lithium mica slag / sepiolite fiber / lithium titanate whisker composite, and 4g of water-reducing agent, put them into a mixer and mix for 1 minute. Then add the multi-component mixture from step 1 and mix them together for 3 minutes. Form mortar test blocks and perform relevant performance tests.
[0113] Comparative Example 1
[0114] I. Preparation of modified lithium mica slag / sepiolite fiber / lithium titanate whisker composite:
[0115] 1) Take a certain amount of lepidolite slag and put it into a ball mill for ball milling treatment. Its specific surface area is 500 m². 2 / kg of granules, for later use;
[0116] 2) Simply mix 1g of KBM-303 with 5g of ethanol to prepare a KBM-303 / ethanol mixture;
[0117] 3) Add 1g of sepiolite fiber to 10g of ethanol and disperse by ultrasonication; continue to add 4g of potassium titanate whiskers and disperse by ultrasonication, then dry to obtain a mixture of sepiolite fiber and potassium titanate whiskers.
[0118] 4) Take 30g of lepidolite slag and put it into a mixer for stirring. At the same time, spray 6g of KBM-303 / ethanol mixture from step 2 onto the surface of the lepidolite slag particles. After the mixture is added, add 5g of sepiolite fiber / potassium titanate whisker mixture and mix evenly. Heat to 90℃ and dry for 50min to prepare modified lepidolite slag / sepiolite fiber / lithium titanate whisker composite.
[0119] II. Preparation of modified amine waterborne curing agent:
[0120] 1) Weigh triethylenetetramine (TETA) and bisphenol A epoxy resin E51 into a round-bottom flask at a molar ratio of 2.5:1 and react them. Heat the mixture to 70°C and react for 3 hours to prepare an epoxy-amine adduct intermediate.
[0121] 2) Weigh the double-ended epoxy polyether and the epoxy-amine adduct intermediate into a round-bottom flask at a molar ratio of 0.5:1 to carry out the addition reaction. Heat to 90°C and react for 3 hours to prepare the modified amine waterborne curing agent.
[0122] III. Methods for preparing waterborne epoxy emulsions include:
[0123] 1) Epoxy resin E44 and polyethylene glycol 6000 with a molar ratio of 2:1 were added to a round-bottom flask and heated to 85°C under the protection of dry nitrogen. After the two were completely melted, they were mixed evenly with stirring to obtain an epoxy resin E44 / polyethylene glycol 6000 blend.
[0124] 2) The catalyst BF3 diethyl ether (0.3% of the total mass of epoxy resin E44 and polyethylene glycol 6000) was diluted 10 times with acetone and added dropwise to the epoxy resin E44 / polyethylene glycol 6000 blend. The catalytic reaction was carried out at 85°C for 4 hours. Then, the mixture was vacuum distilled until no solvent was removed, thus obtaining the epoxy resin emulsifier.
[0125] 3) Add epoxy resin E44 and epoxy resin emulsifier to a mixing tank, heat to 70°C, and mix evenly at high speed of 1200 r / min. Gradually add water to the mixing tank and prepare an aqueous epoxy emulsion with a solid content of 50% by the phase inversion method. The mass ratio of epoxy resin E44 to epoxy resin emulsifier is 1:9.
[0126] IV. Preparation of Lithium Mica Slag Waterborne Epoxy Rapid Repair Mortar
[0127] (1) Weigh 100g of waterborne epoxy emulsion (solid content 50%), 0.6g of wetting agent and 150g of deionized water and stir evenly for 1min. Then add 50g of modified amine waterborne curing agent and 0.6g of defoamer and stir evenly to prepare a multi-component mixture.
[0128] (2) Weigh 1200g of aggregate, 800g of P·O 52.5, 30g of modified lithium mica slag / sepiolite fiber / lithium titanate whisker composite and 4g of water-reducing agent, put them into a mixer and mix for 1 minute. Then add the multi-component mixture from step 1 and mix them together for 3 minutes. Then form mortar test blocks and perform relevant performance tests.
[0129] Comparative Example 2
[0130] I. Preparation of modified lithium mica slag / sepiolite fiber / lithium titanate whisker composite:
[0131] 1) Take a certain amount of lepidolite slag and put it into a ball mill for ball milling treatment. Its specific surface area is 500 m². 2 / kg of granules, for later use;
[0132] 2) Mix 2g of KBM-303 with 10g of ethanol until homogeneous to prepare a KBM-303 / ethanol mixture;
[0133] 3) Add 2g of sepiolite fiber to 10g of ethanol and disperse by ultrasonication; continue to add 3g of potassium titanate whiskers and disperse by ultrasonication, then dry to obtain a mixture of sepiolite fiber and potassium titanate whiskers.
[0134] 4) Take 30g of lepidolite slag and put it into a mixer for stirring. At the same time, spray 12g of KBM-303 / ethanol mixture from step 2 onto the surface of the lepidolite slag particles. After the mixture is added, add 5g of sepiolite fiber / potassium titanate whisker mixture and mix evenly. Heat to 90℃ and dry for 50min to prepare modified lepidolite slag / sepiolite fiber / lithium titanate whisker composite.
[0135] II. Preparation of modified amine water-based curing agent:
[0136] 1) Weigh triethylenetetramine (TETA) and bisphenol A epoxy resin E51 into a round-bottom flask at a molar ratio of 2.5:1 and react them. Heat the mixture to 70°C and react for 3 hours to prepare an epoxy-amine adduct intermediate.
[0137] 2) Weigh the double-ended epoxy polyether and the epoxy-amine adduct intermediate into a round-bottom flask at a molar ratio of 0.5:1 to carry out the addition reaction. Heat to 90°C and react for 3 hours to prepare the modified amine waterborne curing agent.
[0138] III. Methods for preparing waterborne epoxy emulsions include:
[0139] 1) Epoxy resin E44 and polyethylene glycol 6000 with a molar ratio of 2:1 were added to a round-bottom flask and heated to 85°C under the protection of dry nitrogen. After the two were completely melted, they were mixed evenly with stirring to obtain an epoxy resin E44 / polyethylene glycol 6000 blend.
[0140] 2) The catalyst BF3 diethyl ether (0.3% of the total mass of epoxy resin E44 and polyethylene glycol 6000) was diluted 10 times with acetone and added dropwise to the epoxy resin E44 / polyethylene glycol 6000 blend. The catalytic reaction was carried out at 85°C for 4 hours. Then, the mixture was vacuum distilled until no solvent was removed, thus obtaining the epoxy resin emulsifier.
[0141] 3) Add epoxy resin E44 and epoxy resin emulsifier to a mixing tank, heat to 70°C, and mix evenly at high speed of 1200 r / min. Gradually add water to the mixing tank and prepare an aqueous epoxy emulsion with a solid content of 50% by the phase inversion method. The mass ratio of epoxy resin E44 to epoxy resin emulsifier is 1:9.
[0142] IV. Preparation of Lithium Mica Slag Waterborne Epoxy Rapid Repair Mortar
[0143] (1) Weigh 100g of waterborne epoxy emulsion (solid content 50%), 0.6g of wetting agent and 150g of deionized water and stir evenly for 1min. Then add 50g of modified amine water-based curing agent and 0.6g of defoamer and stir evenly to prepare a multi-component mixture.
[0144] (2) Weigh 1200g of aggregate, 800g of P·O 52.5, 30g of modified lithium mica slag / sepiolite fiber / lithium titanate whisker composite and 4g of water-reducing agent, put them into a mixer and mix for 1 minute. Then add the multi-component mixture from step 1 and mix them together for 3 minutes. Then form mortar test blocks and perform relevant performance tests.
[0145] Comparative Example 3
[0146] I. Preparation of modified lithium mica slag / sepiolite fiber / lithium titanate whisker composite:
[0147] 1) Take a certain amount of lepidolite slag and put it into a ball mill for ball milling treatment. Its specific surface area is 500 m². 2 / kg of granules, for later use;
[0148] 2) Mix 2g of KBM-303 / ethanol with 10g of ethanol until homogeneous to prepare the KBM-303 / ethanol mixture;
[0149] 3) Add 3g of sepiolite fiber to 10g of ethanol and disperse by ultrasonication; continue to add 5g of potassium titanate whiskers and disperse by ultrasonication, then dry to obtain a mixture of sepiolite fiber and potassium titanate whiskers.
[0150] 4) Take 60g of lepidolite slag and put it into a mixer for stirring. At the same time, spray 12g of KBM-303 / ethanol mixture from step 2 onto the surface of the lepidolite slag particles. After the mixture is added, add 5g of sepiolite fiber / potassium titanate whisker mixture and mix evenly. Heat to 90℃ and dry for 50min to prepare modified lepidolite slag / sepiolite fiber / lithium titanate whisker composite.
[0151] II. Preparation of modified amine waterborne curing agent:
[0152] 1) Weigh triethylenetetramine (TETA) and bisphenol A epoxy resin E51 into a round-bottom flask at a molar ratio of 2.5:1 and react them. Heat the mixture to 70°C and react for 3 hours to prepare an epoxy-amine adduct intermediate.
[0153] 2) Weigh the double-ended epoxy polyether and the epoxy-amine adduct intermediate into a round-bottom flask at a molar ratio of 0.5:1 to carry out the addition reaction. Heat to 90°C and react for 3 hours to prepare the modified amine water-based curing agent.
[0154] III. Methods for preparing waterborne epoxy emulsions include:
[0155] 1) Epoxy resin E44 and polyethylene glycol 6000 with a molar ratio of 2:1 were added to a round-bottom flask and heated to 85°C under the protection of dry nitrogen. After the two were completely melted, they were mixed evenly with stirring to obtain an epoxy resin E44 / polyethylene glycol 6000 blend.
[0156] 2) The catalyst BF3 diethyl ether (0.3% of the total mass of epoxy resin E44 and polyethylene glycol 6000) was diluted 10 times with acetone and added dropwise to the epoxy resin E44 / polyethylene glycol 6000 blend. The catalytic reaction was carried out at 85°C for 4 hours. Then, the mixture was vacuum distilled until no solvent was removed, thus obtaining the epoxy resin emulsifier.
[0157] 3) Add epoxy resin E44 and epoxy resin emulsifier to a mixing tank, heat to 70°C, and mix evenly at high speed of 1200 r / min. Gradually add water to the mixing tank and prepare an aqueous epoxy emulsion with a solid content of 50% by the phase inversion method. The mass ratio of epoxy resin E44 to epoxy resin emulsifier is 1:9.
[0158] IV. Preparation of Lithium Mica Slag Waterborne Epoxy Rapid Repair Mortar
[0159] (1) Weigh 100g of waterborne epoxy emulsion (solid content 50%), 0.6g of wetting agent and 150g of deionized water and stir evenly for 1min. Then add 50g of modified amine waterborne curing agent and 0.6g of defoamer and stir evenly to prepare a multi-component mixture.
[0160] (2) Weigh 1200g of aggregate, 800g of P·O 52.5, 60g of modified lithium mica slag / sepiolite fiber / lithium titanate whisker composite and 4g of water-reducing agent, put them into a mixer and mix for 1 minute. Then add the multi-component mixture from step 1 and mix them together for 3 minutes. Then form mortar test blocks and perform relevant performance tests.
[0161] Comparative Example 4
[0162] I. Preparation of modified lithium mica slag / sepiolite fiber / lithium titanate whisker composite:
[0163] 1) Take a certain amount of lepidolite slag and put it into a ball mill for ball milling treatment. Its specific surface area is 500 m². 2 / kg of granules, for later use;
[0164] 2) Simply mix 1g of KBM-303 with 5g of ethanol to prepare a KBM-303 / ethanol mixture;
[0165] 3) Add 4g of sepiolite fiber to 10g of ethanol and disperse by ultrasonication; continue to add 1g of potassium titanate whiskers and disperse by ultrasonication, then dry to obtain a mixture of sepiolite fiber and potassium titanate whiskers.
[0166] 4) Take 30g of lepidolite slag and put it into a mixer for stirring. At the same time, spray 6g of KBM-303 / ethanol mixture from step 2 onto the surface of the lepidolite slag particles. After the mixture is added, add 5g of sepiolite fiber / potassium titanate whisker mixture and mix evenly. Heat to 90℃ and dry for 50min to prepare modified lepidolite slag / sepiolite fiber / lithium titanate whisker composite.
[0167] II. Preparation of modified amine water-based curing agent:
[0168] 1) Weigh triethylenetetramine (TETA) and bisphenol A epoxy resin E51 into a round-bottom flask at a molar ratio of 2.5:1 and react them. Heat the mixture to 70°C and react for 3 hours to prepare an epoxy-amine adduct intermediate.
[0169] 2) Weigh the double-ended epoxy polyether and the epoxy-amine adduct intermediate into a round-bottom flask at a molar ratio of 0.5:1 to carry out the addition reaction. Heat to 90°C and react for 3 hours to prepare the modified amine waterborne curing agent.
[0170] III. Methods for preparing waterborne epoxy emulsions include:
[0171] 1) Epoxy resin E44 and polyethylene glycol 6000 with a molar ratio of 2:1 were added to a round-bottom flask and heated to 85°C under the protection of dry nitrogen. After the two were completely melted, they were mixed evenly with stirring to obtain an epoxy resin E44 / polyethylene glycol 6000 blend.
[0172] 2) The catalyst BF3 diethyl ether (0.3% of the total mass of epoxy resin E44 and polyethylene glycol 6000) was diluted 10 times with acetone and added dropwise to the epoxy resin E44 / polyethylene glycol 6000 blend. The catalytic reaction was carried out at 85°C for 4 hours. Then, the mixture was vacuum distilled until no solvent was removed, thus obtaining the epoxy resin emulsifier.
[0173] 3) Add epoxy resin E44 and epoxy resin emulsifier to a mixing tank, heat to 70°C, and mix evenly at high speed of 1200 r / min. Gradually add water to the mixing tank and prepare an aqueous epoxy emulsion with a solid content of 50% by the phase inversion method. The mass ratio of epoxy resin E44 to epoxy resin emulsifier is 1:9.
[0174] IV. Preparation of Lithium Mica Slag Waterborne Epoxy Rapid Repair Mortar
[0175] (1) Weigh 120g of waterborne epoxy emulsion (solid content 50%), 0.6g of wetting agent and 140g of deionized water and stir evenly for 1 min. Then add 60g of modified amine water-based curing agent and 0.6g of defoamer and stir evenly to prepare a multi-component mixture.
[0176] (2) Weigh 1200g of aggregate, 800g of P·O 52.5, 30g of modified lithium mica slag / sepiolite fiber / lithium titanate whisker composite and 4g of water-reducing agent, put them into a mixer and mix for 1 minute. Then add the multi-component mixture from step 1 and mix them together for 3 minutes. Then form mortar test blocks and perform relevant performance tests.
[0177] Comparative Example 5
[0178] The difference from Example 1 is that the "modified lithium mica slag / sepiolite fiber / lithium titanate whisker composite" is removed, otherwise it is the same as Example 1.
[0179] Comparative Example 6
[0180] The difference from Example 1 is that the "modified lepidolite slag / sepiolite fiber / lithium titanate whisker composite" is changed to "modified lepidolite slag", that is, sepiolite fiber and lithium titanate whiskers are not added. Otherwise, it is the same as Example 1.
[0181] Comparative Example 7
[0182] The difference from Example 1 is that the "modified lepidolite slag / sepiolite fiber / lithium titanate whisker composite" is replaced with "unmodified lepidolite slag, sepiolite fiber, and lithium titanate whiskers", and the preparation method is modified as follows:
[0183] 1) Take a certain amount of lepidolite slag and put it into a ball mill for ball milling treatment. Its specific surface area is 400 m². 2 / kg of granules, for later use;
[0184] 2) Add 3g of sepiolite fiber to 10g of ethanol and disperse by ultrasonication; continue to add 2g of potassium titanate whiskers and disperse by ultrasonication, then dry to obtain a mixture of sepiolite fiber and potassium titanate whiskers.
[0185] 4) Take 30g of lithium mica residue and put it into a mixer for stirring. Add 5g of sepiolite fiber / potassium titanate whisker mixture and mix evenly to obtain a mixture of unmodified lithium mica residue, sepiolite fiber and lithium titanate whiskers.
[0186] Everything else is the same as in Example 1.
[0187] Comparative Example 8
[0188] The difference from Example 1 is that the modified amine water-based curing agent is replaced with a commercially available amine curing agent, otherwise it is the same as Example 1.
[0189] The specific amounts of each raw material added in Examples 1-3 and Comparative Examples 1-8 are shown in Table 1.
[0190] Table 1 shows the specific amounts of each ingredient added in Examples 1-3 and Comparative Examples 1-8.
[0191]
[0192]
[0193] The performance of the lithium mica slag water-based epoxy rapid repair mortar of Examples 1-3 and Comparative Examples 1-8 and commercially available ordinary mortar were tested. The performance tests were conducted according to the following standards: (1) setting time was tested according to Chapter 5 of DL / T 5126-2001 "Test Procedure for Polymer Modified Cement Mortar"; (2) compressive strength and flexural strength were tested according to Chapter 9 of GB / T17671-1999 "Test Method for Strength of Cement Mortar"; (3) tensile bond strength was tested according to Chapter 5 of JC / T907-2002 "Concrete Interface Treatment Agent"; (4) shrinkage rate was tested according to Chapter 12 of JCJ 70-2009 "Basic Performance Test Method for Building Mortar".
[0194] Table 2 Performance Tests of Lithium Mica Slag Waterborne Epoxy Rapid Repair Mortar in Examples 1-3 and Comparative Examples 1-4
[0195]
[0196]
[0197] Table 3 Performance Tests of Lithium Mica Slag Waterborne Epoxy Rapid Repair Mortar (Comparative Examples 5-8)
[0198]
[0199] As can be seen from Tables 2-3, compared with commercially available ordinary epoxy mortar, the compressive strength, flexural strength and tensile bond strength of the repair mortar prepared in Examples 1-3 of this invention are significantly better than those of commercially available ordinary epoxy mortar, and the setting time is shorter than that of commercially available ordinary epoxy mortar, enabling rapid repair.
[0200] Compared with Comparative Examples 1-4 (none of which added sulfoaluminate cement), it can be seen that the setting time of the repair mortar prepared in Examples 1-3 of the present invention is shorter than that of Comparative Examples 1-4. This shows that the present invention uses ordinary silicate / sulfoaluminate cement blending modification to accelerate the mortar repair speed.
[0201] Compared with Comparative Examples 5-7, it can be seen that the compressive strength, flexural strength, and tensile bond strength of the repair mortars prepared in Examples 1-3 are significantly better than those in Comparative Example 5 (without modified lepidolite slag / sepiolite fiber / lithium titanate whisker composite), Comparative Example 6 (without sepiolite fiber and lithium titanate whiskers), and Comparative Example 7 (using unmodified lepidolite slag, sepiolite fiber, and lithium titanate whiskers). This indicates that whether or not a modified lepidolite slag / sepiolite fiber / lithium titanate whisker composite is added, the amount of modified lepidolite slag / sepiolite fiber / lithium titanate whisker composite added, whether or not sepiolite fiber and lithium titanate whiskers are added, and whether or not the lepidolite slag, sepiolite fiber, and lithium titanate whiskers are modified all affect the compressive strength, flexural strength, and tensile bond strength of the prepared repair mortar.
[0202] Compared with Comparative Example 8, it can be seen that the setting time of the repair mortar prepared in Examples 1 to 3 is significantly shorter than that of Comparative Example 8, which shows that whether or not the curing agent is modified will affect the setting time of the repair mortar.
[0203] Therefore, this invention improves mortar performance by adding a modified lepidolite slag / sepiolite fiber / lithium titanate whisker composite. Specifically, the finely ground lepidolite slag is mostly in the form of flakes and round particles, possessing good reinforcement and bulk density. This reduces voids and defects between the resin matrix and aggregate, improving the compressive strength, flexural strength, and tensile bond strength of the mortar. Furthermore, this invention modifies the mixture of lepidolite slag, sepiolite fiber, and lithium titanate whiskers, reducing the porosity and defects caused by sepiolite fiber and lithium titanate whiskers. The agglomeration of the fibers ensures that sepiolite fibers and lithium titanate whiskers are uniformly dispersed in the lepidolite slag. The addition of an epoxy-based silane coupling agent further enhances the tightness between the modified lepidolite slag / sepiolite fiber / lithium titanate whisker composite and the polymer, thus enabling the sepiolite fibers and lithium titanate whiskers to be uniformly dispersed in the cement. The modified sepiolite fibers, lithium titanate whiskers, and lepidolite slag work together to significantly improve the mortar's impermeability, crack resistance, dimensional stability, compressive strength, flexural strength, and tensile bond strength. Furthermore, the modification of the curing agent in this invention accelerates the mortar repair process. Additionally, the blending modification of ordinary silicate and sulfoaluminate cement also accelerates the mortar repair process.
[0204] The above description is only a preferred embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any equivalent substitutions or modifications made by those skilled in the art within the scope of the technology disclosed in the present invention, based on the technical solution and inventive concept of the present invention, should be covered within the scope of protection of the present invention.
Claims
1. A water-based epoxy rapid repair mortar for lithium mica slag, characterized in that, The preparation raw materials include the following parts by weight: Aggregate 1100-1300 parts, ordinary Portland cement 400-600 parts, sulfoaluminate cement 200-400 parts, waterborne epoxy emulsion 100-120 parts, defoamer 0.5-0.7 parts, wetting agent 0.5-0.7 parts, water-reducing agent 3-5 parts, deionized water 140-160 parts, modified lepidolite slag / sepiolite fiber / lithium titanate whisker composite 30-60 parts, modified amine waterborne curing agent 50-60 parts; The preparation method of the modified lithium mica slag / sepiolite fiber / lithium titanate whisker composite includes: Lithium methane slag was ball-milled to obtain a specific surface area of 200-800 m². 2 / kg of lithium mica residue particles; An epoxy group silane coupling agent is mixed with ethanol to prepare an epoxy group silane coupling agent / ethanol mixture; Sepiol fiber was added to ethanol and ultrasonically dispersed. Potassium titanate whiskers were then added and ultrasonically dispersed again. The mixture was then dried to obtain a sepiolite fiber / potassium titanate whisker mixture. The lithium mica slag particles are stirred, and the epoxy group silane coupling agent / ethanol mixture is sprayed onto the surface of the lithium mica slag particles. The sepiolite fiber and potassium titanate whisker mixture is then added and stirred evenly. The mixture is then heated to 80-100℃ for 30-90 minutes to obtain the modified lithium mica slag / sepiolite fiber / lithium titanate whisker composite.
2. The lithium mica slag water-based epoxy rapid repair mortar according to claim 1, characterized in that, The preparation raw materials include the following parts by weight: Aggregate 1150-1250 parts, ordinary silicate cement 450-550 parts, sulfoaluminate cement 250-350 parts, waterborne epoxy emulsion 105-115 parts, defoamer 0.55-0.65 parts, wetting agent 0.55-0.65 parts, water-reducing agent 3.5-4.5 parts, deionized water 145-155 parts, modified lepidolite slag / sepiolite fiber / lithium titanate whisker composite 40-50 parts, modified amine waterborne curing agent 52-58 parts.
3. The lithium mica slag water-based epoxy rapid repair mortar according to claim 1, characterized in that, In the preparation method of the modified lepidolite slag / sepiolite fiber / lithium titanate whisker composite, the mass ratio of the epoxy group silane coupling agent to ethanol is 1-2:5-10, the mass ratio of the lepidolite slag to the epoxy group silane coupling agent is 30-60:1-2, and the mass ratio of the lepidolite slag, sepiolite fiber, and potassium titanate whiskers is 30-60:1-5:1-5.
4. The lithium mica slag water-based epoxy rapid repair mortar according to claim 1, characterized in that, The epoxy group silane coupling agent is at least one of KBM-303, KBM-403, and KBE-402.
5. The lithium mica slag water-based epoxy rapid repair mortar according to claim 1, characterized in that, The preparation method of the modified amine waterborne curing agent includes: Triethylenetetramine and bisphenol A type epoxy resin were reacted at 60-70℃ for 3-5 h to obtain an epoxy-amine adduct intermediate. The modified amine waterborne curing agent is obtained by reacting the double-ended epoxy polyether with the epoxy-amine adduct intermediate at 90-100℃ for 2-5 h.
6. The lithium mica slag water-based epoxy rapid repair mortar according to claim 5, characterized in that, In the preparation method of the modified amine waterborne curing agent, the molar ratio of triethylenetetramine to bisphenol A type epoxy resin is 2-3:1; the molar ratio of the double-terminated epoxy polyether to the epoxy-amine adduct intermediate is 0.3-0.7:
1.
7. The lithium mica slag water-based epoxy rapid repair mortar according to claim 1, characterized in that, The method for preparing the aqueous epoxy emulsion includes: 1) Epoxy resin E44 and polyethylene glycol 6000 with a molar ratio of 2:1 were added to a round-bottom flask and heated to 85°C under the protection of dry nitrogen. After the two were completely melted, they were mixed evenly with stirring to obtain an epoxy resin E44 / polyethylene glycol 6000 blend. 2) The catalyst BF3 diethyl ether was diluted 10 times with acetone and added dropwise to the epoxy resin E44 / polyethylene glycol 6000 blend. The reaction was carried out at 85 °C for 4 h. Then, the mixture was vacuum distilled until no solvent was removed, thus obtaining the epoxy resin emulsifier. 3) Add epoxy resin E44 and epoxy resin emulsifier to a stirred tank, heat to 70°C, and stir until uniformly mixed at 1000-1500 r / min. Gradually add water to the stirred tank and prepare an aqueous epoxy emulsion with a solid content of 40%-60% by the phase inversion method. The mass ratio of epoxy resin E44 to epoxy resin emulsifier is 1:
9.
8. The lithium mica slag water-based epoxy rapid repair mortar according to claim 1, characterized in that, The aggregate is artificial sand or natural sand with a particle size of less than 4.75 mm and a mud content of ≤0.45 wt%. The ordinary silicate cement is at least one of P·O 42.5, 52.5, and 62.5, and the sulfoaluminate cement is rapid-hardening sulfoaluminate cement.
9. A method for preparing a water-based epoxy rapid repair mortar based on lithium mica slag as described in any one of claims 1 to 8, characterized in that, Includes the following steps: S1. Weigh out the water-based epoxy emulsion, wetting agent, and deionized water according to the proportion, stir evenly for 0.5-2 minutes, then add the modified amine water-based curing agent and defoamer respectively and stir evenly to prepare a multi-component mixture. S2. Weigh out the aggregate, ordinary silicate cement, sulfoaluminate cement, modified lepidolite slag / sepiolite fiber / lithium titanate whisker composite and water-reducing agent according to the proportions, mix and stir for 0.5-2 minutes, then add the multi-component mixture from step S1 and stir together for 3-5 minutes to prepare lepidolite slag water-based epoxy rapid repair mortar.
Citation Information
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