Sand consolidating agent and method for preparing the same

Abstract

The application belongs to the technical field of sand consolidation agent preparation, and particularly relates to a sand consolidation agent and a preparation method thereof. The sand consolidation agent is composed of component A and component B. The component A is composed of the following raw materials: a diphenyl phenolic epoxy resin, hexakis(4-hydroxymethylphenoxy)cyclotriphosphazene, modified nano calcium zirconate, cage octakis(aminophenyl)silsesquioxane, n-butyl glycidyl ether, KH-550 silane coupling agent, polyether amine, fumed silica and defoaming agent. The component B is composed of the following raw materials: polyborosilazane and 2-ethyl-4-methyl imidazole. The cage octakis(aminophenyl)silsesquioxane in the raw material of the sand consolidation agent strengthens the network structure stability through chemical bonding, the hexakis(4-hydroxymethylphenoxy)cyclotriphosphazene realizes thermal stabilization through chemical bonding and physical dispersion, and the modified nano calcium zirconate provides physical support. The three components synergistically improve the heat resistance of the system.

Description

Technical Field

[0001] This invention belongs to the field of sand-fixing agent preparation technology, specifically relating to a sand-fixing agent and its preparation method. Background Technology

[0002] Currently, sand control technologies mainly include chemical sand control and mechanical sand control. Mechanical sand control is widely used due to its strong adaptability and high success rate, but it has not fundamentally solved the problem of sand production from formations. Chemical sand fixation uses chemical agents to bind sand particles together, fundamentally solving the problem of sand production from formations. A large category of chemical sand control is resin sand control (i.e., using resin as the main raw material for sand control agents), and commonly used resins include phenolic resin, urea-formaldehyde resin, furan resin, and their modified forms.

[0003] Patent CN110655911A discloses a modified resin sand-fixing agent and its preparation method. The components of this resin sand-fixing agent are calculated according to the following weight ratio: modified resin: proppant: diluent: curing agent: coupling agent = 100: 50: 30: 5: 0.1, and the components are mixed in proportion. This modified resin sand-fixing agent can achieve rapid curing and has a certain porosity. The modified resin is a mixture of urea-formaldehyde resin and furfural resin. The modified resin, diluent, curing agent, and coupling agent are mixed together, stirred evenly, and then cured to complete the preparation of the modified resin sand-fixing agent. However, patent CN110655911A is a mixed system of urea-formaldehyde resin and furfural resin. Both types of resins are low-temperature condensation resins with a large number of amide bonds and aldehyde groups in their molecular chains. They are prone to pyrolysis and hydrolysis at high temperatures, and the curing temperature is only 25-55℃. This system will experience a sharp drop in strength and pulverization above 80℃, and can only be used in shallow wells and low-temperature formations.

[0004] As oil formations become deeper, the operating temperature of sand-fixing agents increases, especially in the exploitation of heavy oil wells, which typically employ thermal recovery methods such as steam injection and steam drive. This requires sand-fixing agents to have excellent temperature resistance. Therefore, developing sand-fixing agents with good sand-control effects and high-temperature resistance has become an urgent technical problem to be solved. Summary of the Invention

[0005] The purpose of this invention is to provide a sand-fixing agent that exhibits good compressive strength of cemented rock cores at high temperatures. In addition, this invention also provides a method for its preparation.

[0006] The sand-fixing agent of the present invention is composed of component A and component B, with a mass ratio of component A to component B of 100:29. Component A, by weight, is composed of the following raw materials: 100 parts of biphenyl-type phenolic epoxy resin, 6.5-7.0 parts of hexa(4-hydroxymethylphenoxy)cyclotriphosphazene, 3.0-3.2 parts of modified nano-calcium zirconate, 3.0-3.3 parts of cage-like octa(aminophenyl)silsesquioxane, 19.5-20 parts of n-butyl glycidyl ether, 1.3-1.5 parts of KH-550 silane coupling agent, 0.9-1.0 parts of polyetheramine D230, 0.3-0.5 parts of fumed silica, and 0.5 parts of defoamer. Component B, by weight, is composed of the following raw materials: 25-26 parts of polyborosilazane and 6-7 parts of 2-ethyl-4-methylimidazolium.

[0007] The defoamer is polyoxypropylene polyoxyethylene glycerol ether.

[0008] The preparation method of the modified nano-calcium zirconate comprises the following steps: ① Drying nano-calcium zirconate under vacuum at 120℃ and -0.095MPa for 4 hours to obtain dried nano-calcium zirconate; ② Mixing KH-550 silane coupling agent, anhydrous ethanol, and deionized water in a mass ratio of 1:8:1, then adding acetic acid to adjust the pH of the system to 4.5, and stirring and hydrolyzing at 25℃ for 30 minutes to obtain a silane hydrolysate; ③ Adding the dried nano-calcium zirconate to the silane hydrolysate, wherein the mass ratio of nano-calcium zirconate to KH-550 silane coupling agent is 100: 3. Stir the reaction mixture at 70℃ under nitrogen protection for 6 hours at a stirring speed of 600 r / min; ④ Centrifuge the reaction mixture at a speed of 8000 r / min for 10 minutes. Wash the precipitate five times with anhydrous ethanol, ensuring that the last washing solution is neutral; ⑤ After washing, vacuum dry the precipitate at 80℃ for 12 hours, grind and sieve through a 200-mesh sieve to obtain modified nano-calcium zirconate.

[0009] The structural formula of hexa(4-hydroxymethylphenoxy)cyclotriphosphazene is: .

[0010] The structural formula of cage-like octa(aminophenyl)silsesquioxane is: .

[0011] The preparation of cage-like octa(aminophenyl)silsesquioxanes can be found in the following literature: Du Jianke, Yang Rongjie. Synthesis and characterization of cage-like octa(aminophenyl)silsesquioxanes [J]. Journal of Beijing Institute of Technology, 2007, 27(4): 358-361.

[0012] The method for preparing the sand-stabilizing agent according to the present invention comprises the following steps:

[0013] (1) Preparation of component A

[0014] ① Mix n-butyl glycidyl ether, KH-550 silane coupling agent, polyetheramine D230 and fumed silica, add modified nano calcium zirconate, first ultrasonically disperse and then stir.

[0015] ② Add 50 parts of biphenyl-type phenolic epoxy resin to the mixture in step ① and stir at 60℃ for 30-35 minutes until uniform. Then add the remaining 50 parts of biphenyl-type phenolic epoxy resin and continue stirring for 30-35 minutes.

[0016] ③ Add cage-like octa(aminophenyl)silsesquioxane and hexa(4-hydroxymethylphenoxy)cyclotriphosphazene to the mixture prepared in step ② and stir to dissolve;

[0017] ④ Add defoamer to the mixing system in step ③, and then perform vacuum degassing to prepare component A;

[0018] (2) Preparation of component B

[0019] 2-Ethyl-4-methylimidazolium was added to polyborosilazane and stirred and mixed, then sieved to prepare component B;

[0020] (3) Preparation of sand-fixing agent

[0021] When using, mix component A and component B at a mass ratio of 100:29 to prepare the sand-fixing agent.

[0022] Among them: the ultrasonic dispersion in step (1) ① of component A is to first sonicate at 35℃ with an ultrasonic power of 150W for 20-23min, and then sonicate at an ultrasonic power of 300W for 50-55min, with a stirring speed of 1000r / min, a stirring time of 40-45min, and a stirring temperature of room temperature.

[0023] In step (1) ③ of the preparation of component A, the stirring and dissolving time is 40-45 min and the stirring and dissolving temperature is 80℃.

[0024] In step (1)④ of the preparation of component A, the vacuum degassing temperature is 50℃, the vacuum degassing time is 40-42min, and the vacuum degassing pressure is -0.095MPa.

[0025] When preparing component B, the stirring temperature is room temperature, the stirring time is 30-35 minutes, the stirring speed is 400 r / min, and it is passed through a 100-mesh sieve.

[0026] In step (3), component B is added dropwise to component A while stirring at a high speed of 1000 r / min to ensure uniform dispersion.

[0027] Once component A is prepared, it should be sealed and stored immediately, and mixed and injected with component B within 24 hours.

[0028] Compared with the prior art, the present invention has the following advantages:

[0029] (1) The sand-fixing agent of the present invention has a main component of component A, which is a biphenyl-type phenolic epoxy resin. The molecular chain carries epoxy active groups that can open the ring and crosslink, which is the bonding matrix for sand fixation. Under the catalysis of 2-ethyl-4-methylimidazole, the -NH2 group at the end of the polyborosilicate molecular chain undergoes a ring-opening addition reaction with the epoxy group in component A to form Si-NC covalent bonds. 2-ethyl-4-methylimidazole acts as a curing accelerator and can reduce the activation energy of the curing reaction of the epoxy resin system. At the same time, the cage-like octa(aminophenyl)silsesquioxane, KH-550 silane coupling agent, and polyetheramine D230 in component A all carry active amino groups, which can synergistically participate in the epoxy ring-opening addition reaction and supplement the curing active sites. After mixing component A and component B, the mixture is injected into the sandstone pores. Under the downhole temperature conditions, a rapid ring-opening addition crosslinking occurs to form an organic-inorganic hybrid curing network that can withstand high temperatures of 300℃, which physically bonds the transportable sand particles into a rigid whole.

[0030] (2) In the sand-fixing agent of the present invention, the eight active amino groups of the cage-like octa(aminophenyl)silsesquioxane participate in the epoxy ring-opening curing reaction, forming multifunctional crosslinking points and significantly increasing the crosslinking density; its inorganic silicon-oxygen cage-like skeleton maintains structural stability at high temperature, preventing molecular chain segment movement and increasing the glass transition temperature. The polyborosilicate in component B undergoes condensation and ceramicization at high temperature to form a SiBCN inorganic skeleton, which, together with the cage-like structure of the cage-like octa(aminophenyl)silsesquioxane, synergistically constructs an organic-inorganic hybrid heat-resistant network. The hydroxymethyl group of hexa(4-hydroxymethylphenoxy)cyclotriphosphazene can also participate in the epoxy curing reaction, making the phosphazene heterocycle chemically bonded in the network, and at high temperature, P and N elements can uniformly play a free radical capturing role. Modified nano-calcium zirconate possesses excellent high-temperature resistance, chemical stability, and high-temperature strength. When added to a sand-fixing agent as a filler, it provides continuous structural support for the sand body, improving the heat resistance and long-term stability of the sand-fixing agent in high-temperature reservoir environments, and ensuring that the solidified body retains high mechanical strength under high-temperature conditions. The cyclic skeleton of hexa(4-hydroxymethylphenoxy)cyclotriphosphazene acts as a rigid barrier, delaying heat transfer to the molecular chain. Cage-shaped octa(aminophenyl)silsesquioxane strengthens the network structure stability through chemical bonding, while hexa(4-hydroxymethylphenoxy)cyclotriphosphazene achieves thermal stabilization through chemical bonding and physical dispersion. Modified nano-calcium zirconate provides physical support. These three components synergistically enhance the system's heat resistance from three dimensions: "network strengthening, degradation inhibition, and homogenization temperature," enabling the sand-fixing agent to maintain structural integrity and bonding strength even at 300℃.

[0031] (3) In the preparation method of the sand-fixing agent described in this invention, n-butyl glycidyl ether is used as an active diluent to reduce the viscosity of the system and ensure that the sand-fixing agent can be smoothly injected into the pores of loose sandstone and fully wet the sand particles; polyetheramine D230 is used as an auxiliary dispersant to assist in the dispersion of modified nano-calcium zirconate; fumed silica is used as an anti-settling agent to physically constrain the particles using its three-dimensional network structure; vacuum degassing eliminates air bubbles in the system to ensure that the solidified body has a dense structure and no pore defects; component B is mixed at room temperature and with gentle stirring to avoid pre-crosslinking of polyborosilicate and ensure uniform downhole solidification, thereby ensuring that the properties of the sand-fixing agent prepared by this preparation method are stable and controllable. Detailed Implementation

[0032] The preparation methods of modified nano-calcium zirconate, the structural formulas of hexa(4-hydroxymethylphenoxy)cyclotriphosphazene and cage-like octa(aminophenyl)silsesquioxane, and their preparation methods used in the following examples are shown below:

[0033] The preparation method of modified nano-calcium zirconate consists of the following steps: ① Drying nano-calcium zirconate under vacuum at 120℃ and -0.095MPa for 4h to obtain dried nano-calcium zirconate; ② Mixing KH-550 silane coupling agent, anhydrous ethanol, and deionized water in a mass ratio of 1:8:1, then adding acetic acid to adjust the pH of the system to 4.5, and stirring and hydrolyzing at 25℃ for 30min to obtain a silane hydrolysate; ③ Adding the dried nano-calcium zirconate to the silane hydrolysate, wherein the mass ratio of nano-calcium zirconate to KH-550 silane coupling agent is 100:1. 3. Stir the reaction mixture at 70℃ under nitrogen protection for 6 hours at a stirring speed of 600 r / min; ④ Centrifuge the reaction mixture at a speed of 8000 r / min for 10 minutes. Wash the precipitate five times with anhydrous ethanol, ensuring that the last washing solution is neutral; ⑤ After washing, vacuum dry the precipitate at 80℃ for 12 hours, grind and sieve through a 200-mesh sieve to obtain modified nano-calcium zirconate.

[0034] The structural formula of hexa(4-hydroxymethylphenoxy)cyclotriphosphazene is: .

[0035] The structural formula of cage-like octa(aminophenyl)silsesquioxane is: .

[0036] The preparation of cage-like octa(aminophenyl)silsesquioxanes can be found in the following literature: Du Jianke, Yang Rongjie. Synthesis and characterization of cage-like octa(aminophenyl)silsesquioxanes [J]. Journal of Beijing Institute of Technology, 2007, 27(4): 358-361.

[0037] Example 1

[0038] The sand-fixing agent described in Example 1 consists of component A and component B, with a mass ratio of 100:29. Component A, by weight, is composed of the following raw materials: 100 parts of biphenyl-type phenolic epoxy resin, 6.8 parts of hexa(4-hydroxymethylphenoxy)cyclotriphosphazene, 3.1 parts of modified nano-calcium zirconate, 3.2 parts of cage-like octa(aminophenyl)silsesquioxane, 19.7 parts of n-butyl glycidyl ether, 1.4 parts of KH-550 silane coupling agent, 0.95 parts of polyetheramine D230, 0.4 parts of fumed silica, and 0.5 parts of defoamer. Component B, by weight, is composed of the following raw materials: 25.5 parts of polyborosilazane and 6.5 parts of 2-ethyl-4-methylimidazolium.

[0039] The defoamer is polyoxypropylene polyoxyethylene glycerol ether.

[0040] The method for preparing the sand-stabilizing agent described in Example 1 consists of the following steps:

[0041] (1) Preparation of component A

[0042] ① Mix n-butyl glycidyl ether, KH-550 silane coupling agent, polyetheramine D230 and fumed silica, add modified nano calcium zirconate, first ultrasonically disperse and then stir.

[0043] ② Add 50 parts of biphenyl-type phenolic epoxy resin to the mixture in step ① and stir at 60℃ for 33 minutes until uniform. Then add the remaining 50 parts of biphenyl-type phenolic epoxy resin and continue stirring for 33 minutes.

[0044] ③ Add cage-like octa(aminophenyl)silsesquioxane and hexa(4-hydroxymethylphenoxy)cyclotriphosphazene to the mixture prepared in step ② and stir to dissolve;

[0045] ④ Add defoamer to the mixing system in step ③, and then perform vacuum degassing to prepare component A;

[0046] (2) Preparation of component B

[0047] 2-Ethyl-4-methylimidazolium was added to polyborosilazane and stirred and mixed, then sieved to prepare component B;

[0048] (3) Preparation of sand-fixing agent

[0049] When using, mix component A and component B at a mass ratio of 100:29 to prepare the sand-fixing agent.

[0050] Among them: the ultrasonic dispersion in step (1) ① of component A is first ultrasonically dispersed at 35℃ with an ultrasonic power of 150W for 21min, and then ultrasonically dispersed at an ultrasonic power of 300W for 53min, with a stirring speed of 1000r / min, a stirring time of 43min, and a stirring temperature of room temperature.

[0051] In step (1) ③ of the preparation of component A, the stirring and dissolving time is 43 min and the stirring and dissolving temperature is 80℃.

[0052] In step (1)④ of the preparation of component A, the vacuum degassing temperature is 50℃, the vacuum degassing time is 41min, and the vacuum degassing pressure is -0.095MPa.

[0053] Component B was prepared at room temperature for 33 minutes, at a speed of 400 rpm, and passed through a 100-mesh sieve.

[0054] In step (3), component B is added dropwise to component A while stirring at a high speed of 1000 r / min to ensure uniform dispersion.

[0055] Once component A is prepared, it should be sealed and stored immediately, and mixed and injected with component B within 24 hours.

[0056] Example 2

[0057] The sand-fixing agent described in Example 2 consists of component A and component B, with a mass ratio of 100:29. Component A, by weight, is composed of the following raw materials: 100 parts of biphenyl-type phenolic epoxy resin, 6.5 parts of hexa(4-hydroxymethylphenoxy)cyclotriphosphazene, 3.2 parts of modified nano-calcium zirconate, 3.0 parts of cage-like octa(aminophenyl)silsesquioxane, 19.5 parts of n-butyl glycidyl ether, 1.5 parts of KH-550 silane coupling agent, 0.9 parts of polyetheramine D230, 0.3 parts of fumed silica, and 0.5 parts of defoamer. Component B, by weight, is composed of the following raw materials: 25 parts of polyborosilazane and 6 parts of 2-ethyl-4-methylimidazolium.

[0058] The defoamer is polyoxypropylene polyoxyethylene glycerol ether.

[0059] The method for preparing the sand-stabilizing agent described in Example 2 consists of the following steps:

[0060] (1) Preparation of component A

[0061] ① Mix n-butyl glycidyl ether, KH-550 silane coupling agent, polyetheramine D230 and fumed silica, add modified nano calcium zirconate, first ultrasonically disperse and then stir.

[0062] ② Add 50 parts of biphenyl-type phenolic epoxy resin to the mixture in step ① and stir at 60℃ for 30 minutes until uniform. Then add the remaining 50 parts of biphenyl-type phenolic epoxy resin and continue stirring for 35 minutes.

[0063] ③ Add cage-like octa(aminophenyl)silsesquioxane and hexa(4-hydroxymethylphenoxy)cyclotriphosphazene to the mixture prepared in step ② and stir to dissolve;

[0064] ④ Add defoamer to the mixing system in step ③, and then perform vacuum degassing to prepare component A;

[0065] (2) Preparation of component B

[0066] 2-Ethyl-4-methylimidazolium was added to polyborosilazane and stirred and mixed, then sieved to prepare component B;

[0067] (3) Preparation of sand-fixing agent

[0068] When using, mix component A and component B at a mass ratio of 100:29 to prepare the sand-fixing agent.

[0069] Among them: the ultrasonic dispersion in step (1) ① of component A is first ultrasonically dispersed at 35℃ with an ultrasonic power of 150W for 20min, and then ultrasonically dispersed at an ultrasonic power of 300W for 50min, with a stirring speed of 1000r / min, a stirring time of 40min, and a stirring temperature of room temperature.

[0070] In step (1) ③ of the preparation of component A, the stirring and dissolving time is 40 min and the stirring and dissolving temperature is 80℃.

[0071] In step (1)④ of the preparation of component A, the vacuum degassing temperature is 50℃, the vacuum degassing time is 40min, and the vacuum degassing pressure is -0.095MPa.

[0072] Component B was prepared at room temperature for 30 minutes, at a stirring speed of 400 r / min, and passed through a 100-mesh sieve.

[0073] In step (3), component B is added dropwise to component A while stirring at a high speed of 1000 r / min to ensure uniform dispersion.

[0074] Once component A is prepared, it should be sealed and stored immediately, and mixed and injected with component B within 24 hours.

[0075] Example 3

[0076] The sand-fixing agent described in Example 3 consists of component A and component B, with a mass ratio of 100:29. Component A, by weight, is composed of the following raw materials: 100 parts of biphenyl-type phenolic epoxy resin, 7.0 parts of hexa(4-hydroxymethylphenoxy)cyclotriphosphazene, 3.0 parts of modified nano-calcium zirconate, 3.3 parts of cage-like octa(aminophenyl)silsesquioxane, 20 parts of n-butyl glycidyl ether, 1.3 parts of KH-550 silane coupling agent, 1.0 part of polyetheramine D230, 0.5 parts of fumed silica, and 0.5 parts of defoamer. Component B, by weight, is composed of the following raw materials: 26 parts of polyborosilazane and 7 parts of 2-ethyl-4-methylimidazole.

[0077] The defoamer is polyoxypropylene polyoxyethylene glycerol ether.

[0078] The method for preparing the sand-stabilizing agent described in Example 3 consists of the following steps:

[0079] (1) Preparation of component A

[0080] ① Mix n-butyl glycidyl ether, KH-550 silane coupling agent, polyetheramine D230 and fumed silica, add modified nano calcium zirconate, first ultrasonically disperse and then stir.

[0081] ② Add 50 parts of biphenyl-type phenolic epoxy resin to the mixture in step ① and stir at 60℃ for 35 minutes until uniform. Then add the remaining 50 parts of biphenyl-type phenolic epoxy resin and continue stirring for 30 minutes.

[0082] ③ Add cage-like octa(aminophenyl)silsesquioxane and hexa(4-hydroxymethylphenoxy)cyclotriphosphazene to the mixture prepared in step ② and stir to dissolve;

[0083] ④ Add defoamer to the mixing system in step ③, and then perform vacuum degassing to prepare component A;

[0084] (2) Preparation of component B

[0085] 2-Ethyl-4-methylimidazolium was added to polyborosilazane and stirred and mixed, then sieved to prepare component B;

[0086] (3) Preparation of sand-fixing agent

[0087] When using, mix component A and component B at a mass ratio of 100:29 to prepare the sand-fixing agent.

[0088] Among them: the ultrasonic dispersion in step (1)① of component A is first ultrasonically dispersed at 35℃ with an ultrasonic power of 150W for 23min, and then ultrasonically dispersed at an ultrasonic power of 300W for 55min, with a stirring speed of 1000r / min, a stirring time of 45min, and a stirring temperature of room temperature.

[0089] In step (1) ③ of the preparation of component A, the stirring and dissolving time is 45 min and the stirring and dissolving temperature is 80℃.

[0090] In step (1)④ of the preparation of component A, the vacuum degassing temperature is 50℃, the vacuum degassing time is 42min, and the vacuum degassing pressure is -0.095MPa.

[0091] Component B was prepared at room temperature for 33 minutes, at a stirring speed of 400 rpm, and passed through a 100-mesh sieve.

[0092] In step (3), component B is added dropwise to component A while stirring at a high speed of 1000 r / min to ensure uniform dispersion.

[0093] Once component A is prepared, it should be sealed and stored immediately, and mixed and injected with component B within 24 hours.

[0094] Comparative Example 1

[0095] The preparation method of the sand-fixing agent described in Comparative Example 1 is the same as that in Example 1, except that hexa(4-hydroxymethylphenoxy)cyclotriphosphazene is not added to component A.

[0096] Comparative Example 2

[0097] The preparation method of the sand-fixing agent described in Comparative Example 2 is the same as that in Example 1, except that modified nano-calcium zirconate is not added to component A.

[0098] Comparative Example 3

[0099] The preparation method of the sand-fixing agent described in Comparative Example 3 is the same as that in Example 1, except that no cage-like octa(aminophenyl)silsesquioxane is added to component A.

[0100] The performance of the sand-stabilizing agents prepared in Examples 1-3 and Comparative Examples 1-3 was tested. The mass of the sand-stabilizing agent was 5% of the mass of the quartz sand. The compressive strength test was conducted according to Q / SH1020 1969-2016 "General Technical Conditions for Sand-Stabilizing Agents". The curing conditions were optimized to 110℃×6h (simulating high-temperature downhole conditions), and the high-temperature aging conditions were 300℃×72h under nitrogen protection. The results are shown in Table 1 below:

[0101] Table 1. Test results of sand-stabilizing agent performance

[0102]

[0103] As can be seen from Table 1 above, the compressive strength of the cores in Examples 1-3 is significantly higher than that in Comparative Examples 1-3. In Comparative Examples 1-3, the compressive strength of the cemented cores decreased due to the absence of hexa(4-hydroxymethylphenoxy)cyclotriphosphazene, modified nano-calcium zirconate, and cage-like octa(aminophenyl)silsesquioxane.

[0104] The above description is merely a preferred embodiment of the present invention and is not intended to limit the present invention in any way. Although the present invention has been disclosed above with reference to preferred embodiments, it is not intended to limit the present invention. Any person skilled in the art can make some modifications or alterations to the above-disclosed technical content to create equivalent embodiments without departing from the scope of the present invention. Any simple modifications, equivalent changes and alterations made to the above embodiments based on the technical essence of the present invention without departing from the scope of the present invention shall still fall within the scope of the present invention.

Claims

1. A sand-fixing agent, characterized in that: The product is composed of component A and component B, with a mass ratio of 100:

29. Component A, by weight, consists of the following raw materials: 100 parts of biphenyl-type phenolic epoxy resin, 6.5-7.0 parts of hexa(4-hydroxymethylphenoxy)cyclotriphosphazene, 3.0-3.2 parts of modified nano-calcium zirconate, 3.0-3.3 parts of cage-like octa(aminophenyl)silsesquioxane, 19.5-20 parts of n-butyl glycidyl ether, 1.3-1.5 parts of KH-550 silane coupling agent, 0.9-1.0 parts of polyetheramine D230, 0.3-0.5 parts of fumed silica, and 0.5 parts of defoamer. Component B, by weight, consists of the following raw materials: 25-26 parts of polyborosilazane and 6-7 parts of 2-ethyl-4-methylimidazolium. in: The preparation method of the modified nano-calcium zirconate comprises the following steps: ① Drying nano-calcium zirconate under vacuum at 120℃ and -0.095MPa for 4 hours to obtain dried nano-calcium zirconate; ② Mixing KH-550 silane coupling agent, anhydrous ethanol, and deionized water in a mass ratio of 1:8:1, then adding acetic acid to adjust the pH of the system to 4.5, and stirring and hydrolyzing at 25℃ for 30 minutes to obtain a silane hydrolysate; ③ Adding the dried nano-calcium zirconate to the silane hydrolysate, wherein the mass ratio of nano-calcium zirconate to KH-550 silane coupling agent is 100:

3. Stir the reaction mixture at 70℃ under nitrogen protection for 6 hours at a stirring speed of 600 r / min; ④ Centrifuge the reaction mixture at 8000 r / min for 10 minutes. Wash the precipitate five times with anhydrous ethanol, ensuring that the last washing solution is neutral; ⑤ After washing, vacuum dry the precipitate at 80℃ for 12 hours, grind and sieve through a 200-mesh sieve to obtain modified nano-calcium zirconate. The structural formula of cage-like octa(aminophenyl)silsesquioxane is: 。 2. The sand-fixing agent according to claim 1, characterized in that: The defoamer is polyoxypropylene polyoxyethylene glycerol ether.

3. A method for preparing the sand-fixing agent according to claim 1, characterized in that: It consists of the following steps: (1) Preparation of component A ① Mix n-butyl glycidyl ether, KH-550 silane coupling agent, polyetheramine D230 and fumed silica, add modified nano calcium zirconate, first ultrasonically disperse and then stir. ② Add 50 parts of biphenyl-type phenolic epoxy resin to the mixture in step ① and stir at 60℃ for 30-35 minutes until uniform. Then add the remaining 50 parts of biphenyl-type phenolic epoxy resin and continue stirring for 30-35 minutes. ③ Add cage-like octa(aminophenyl)silsesquioxane and hexa(4-hydroxymethylphenoxy)cyclotriphosphazene to the mixture prepared in step ② and stir to dissolve; ④ Add defoamer to the mixing system in step ③, and then perform vacuum degassing to prepare component A; (2) Preparation of component B 2-Ethyl-4-methylimidazolium was added to polyborosilazane and stirred and mixed, then sieved to prepare component B; (3) Preparation of sand-fixing agent When using, mix component A and component B at a mass ratio of 100:29 to prepare the sand-fixing agent.

4. The method for preparing the sand-stabilizing agent according to claim 3, characterized in that: The ultrasonic dispersion described in step (1)① of the preparation of component A is to first sonicate at 35℃ with an ultrasonic power of 150W for 20-23 minutes, and then sonicate at an ultrasonic power of 300W for 50-55 minutes, with a stirring speed of 1000r / min, a stirring time of 40-45 minutes, and a stirring temperature of room temperature.

5. The method for preparing the sand-stabilizing agent according to claim 3, characterized in that: In step (1) ③ of the preparation of component A, the stirring and dissolving time is 40-45 min and the stirring and dissolving temperature is 80℃.

6. The method for preparing the sand-stabilizing agent according to claim 3, characterized in that: In step (1)④ of the preparation of component A, the vacuum degassing temperature is 50℃, the vacuum degassing time is 40-42min, and the vacuum degassing pressure is -0.095MPa.

7. The method for preparing the sand-stabilizing agent according to claim 3, characterized in that: When preparing component B, the stirring temperature is room temperature, the stirring time is 30-35 minutes, the stirring speed is 400 r / min, and it is passed through a 100-mesh sieve.

8. The method for preparing the sand-stabilizing agent according to claim 3, characterized in that: In step (3), component B is added dropwise to component A while stirring at a high speed of 1000 r / min to ensure uniform dispersion.

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