Coating compounding process

Abstract

The coating compounding process comprises the following steps: preparation of an adhesive film solution: adding 5-10 parts of a cross-linking agent and 4-7 parts of a modified filler agent into 35-45 parts of an epoxy resin adhesive solution, and stirring to obtain the adhesive film solution after the stirring is finished. According to the coating and compounding process, the polyimide (PI) film is coated with the adhesive film liquid, meanwhile, the adhesive film liquid is matched with the cross-linking agent through the epoxy resin adhesive liquid, the insulating property, the stripping property and the barrier property of the obtained adhesive films are excellent through co-matching and coordination of the raw materials and the optimized synergistic effect of the raw materials, and the coordination of the product can be balanced and improved.

Description

Technical Field

[0001] The present invention relates to the field of coating technology, in particular to a coating composite process. Background Art

[0002] In the production of chip attach films, the coating and lamination process is a key step in combining the film with other functional films or substrates to improve the film's overall performance. However, films produced using this coating and lamination process suffer from poor insulation and inter-film peelability, as well as mediocre barrier properties. This makes it difficult to achieve a balanced performance balance. The present invention addresses this challenge by providing a coating and lamination process. Summary of the Invention

[0003] In view of the defects of the prior art, the object of the present invention is to provide a coating composite process to solve the problems raised in the above background technology.

[0004] The present invention solves the technical problem by adopting the following technical solutions:

[0005] The present invention provides a coating composite process, comprising the following steps:

[0006] Step 1, preparation of film solution:

[0007] Add 5-10 parts of a crosslinking agent and 4-7 parts of a modified filler to 35-45 parts of an epoxy resin glue solution, stirring the mixture until the stirring is complete to obtain a film solution;

[0008] Step 2: Use a polyimide (PI) film as the base film, and then apply the adhesive film liquid to the surface of the polyimide (PI) film with a coating thickness of 1-2 mm.

[0009] Preferably, the stirring speed of the stirring treatment is 350-400 r / min, the stirring time is 2 h, and the stirring temperature is 55-60°C.

[0010] Preferably, the cross-linking agent is tricyclohexylphosphine; the epoxy resin glue is an epoxy resin diluent to maintain the viscosity of the epoxy resin at 0.3-0.7 Pa.s.

[0011] Preferably, the preparation method of the modified filler is:

[0012] S1: preheating nano-aluminum nitride at 55-60°C for 1 hour, and evenly mixing 4-7 parts of the preheated nano-aluminum nitride and 3-5 parts of kaolin solution to obtain a mixed modifier;

[0013] S2: stirring the carbon nanotubes in a modification solution that is 3-5 times the total amount of the carbon nanotubes for modification treatment, filtering and drying after the stirring is completed to obtain modified carbon nanotubes;

[0014] The preparation method of the modified liquid is as follows:

[0015] 2-5 parts of sodium silicate solution, 3-5 parts of boron nitride and 1-3 parts of yttrium nitrate solution are uniformly mixed to prepare a modified solution;

[0016] S3: The modified carbon nanotubes, titanium oxide and lanthanum oxide are mixed and sintered in a weight ratio of (5-8): (3-5): 3, and the sintering is completed to obtain a sintered body;

[0017] S4: The sintered body and the modified modifier are mixed in a weight ratio of 7:(3-5) and ball-milled at a ball-milling speed of 1500 r / min for 2 h. After the ball-milling is completed, the mixture is filtered and dried to obtain a modified filler.

[0018] Preferably, the stirring speed of the stirring modification treatment is 450-500 r / min, and the stirring is for 1 hour; the sintering temperature of the blending sintering treatment is 210-220° C., and the sintering is for 1 hour.

[0019] Preferably, the mass fraction of the sodium silicate solution is 2-5%; the mass fraction of the yttrium nitrate solution is 4-7%.

[0020] Preferably, the preparation method of kaolin liquid is:

[0021] The kaolin is heat-treated at 145-155°C for 1 hour, then cooled to 55°C at a rate of 2-5°C / min, kept warm, and the kept warm kaolin is fully stirred in a treatment liquid that is 3-5 times the total amount of the kept warm kaolin to obtain a kaolin liquid.

[0022] Preferably, the treatment solution comprises the following raw materials in parts by weight: 2-5 parts of nanocellulose, 1-3 parts of calcium carbonate, 4-7 parts of dopamine hydrochloride solution and 1-2 parts of silicon carbide.

[0023] Preferably, the mass fraction of the dopamine hydrochloride solution is 2-5%.

[0024] Compared with the prior art, the present invention has the following beneficial effects:

[0025] The coating composite process of the present invention is to coat the film liquid onto the polyimide (PI) film, and at the same time, the film liquid is mixed with a cross-linking agent through an epoxy resin glue, and then blended and coordinated with a modified filler. The nano-aluminum nitride in the modified filler is preheated and then blended with a kaolin liquid to form a mixed modifier. At the same time, the carbon nanotubes are improved by a specific modifying liquid, and the sodium silicate solution, boron nitride and yttrium nitrate solution in the modifying liquid are blended and coordinated. Through the synergistic effect between the raw materials, the kaolin liquid adopts kaolin that has been heat-treated at 145-155°C for 1h, and then It is then cooled to 55°C at a rate of 2-5°C / min. The interlamellar spacing of kaolin is optimized through thermal improvement. The kaolin liquid is improved by using kaolin in combination with the treatment liquid. The raw materials in the treatment liquid are improved by mutual coordination. The modified carbon nanotubes, titanium oxide and lanthanum oxide are sintered to form a sintered body. The sintered body and miscellaneous modifiers are blended and ball milled to improve the insulation, inter-film peeling and barrier properties of the obtained films through the coordination between the raw materials and the optimized synergy between the raw materials. The coordination of the products can be balanced and improved. DETAILED DESCRIPTION

[0026] The following is a clear and complete description of the technical solutions in the embodiments of the present invention in conjunction with specific embodiments. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.

[0027] The coating and laminating process of this embodiment includes the following steps:

[0028] Step 1, preparation of film solution:

[0029] Add 5-10 parts of a crosslinking agent and 4-7 parts of a modified filler to 35-45 parts of an epoxy resin glue solution, stirring the mixture until the stirring is complete to obtain a film solution;

[0030] Step 2: Use a polyimide (PI) film as the base film, and then apply the adhesive film liquid to the surface of the polyimide (PI) film with a coating thickness of 1-2 mm.

[0031] Preferably, the stirring speed of the stirring treatment is 350-400 r / min, the stirring time is 2 h, and the stirring temperature is 55-60°C.

[0032] The cross-linking agent in this embodiment is tricyclohexylphosphine; the epoxy resin glue is an epoxy resin diluent to maintain the viscosity of the epoxy resin at 0.3-0.7 Pa.s.

[0033] The preparation method of the modified filler of this embodiment is:

[0034] S1: preheating nano-aluminum nitride at 55-60°C for 1 hour, and evenly mixing 4-7 parts of the preheated nano-aluminum nitride and 3-5 parts of kaolin solution to obtain a mixed modifier;

[0035] S2: stirring the carbon nanotubes in a modification solution that is 3-5 times the total amount of the carbon nanotubes for modification treatment, filtering and drying after the stirring is completed to obtain modified carbon nanotubes;

[0036] The preparation method of the modified liquid is as follows:

[0037] 2-5 parts of sodium silicate solution, 3-5 parts of boron nitride and 1-3 parts of yttrium nitrate solution are uniformly mixed to prepare a modified solution;

[0038] S3: The modified carbon nanotubes, titanium oxide and lanthanum oxide are mixed and sintered in a weight ratio of (5-8): (3-5): 3, and the sintering is completed to obtain a sintered body;

[0039] S4: The sintered body and the modified modifier are mixed in a weight ratio of 7:(3-5) and ball-milled at a ball-milling speed of 1500 r / min for 2 h. After the ball-milling is completed, the mixture is filtered and dried to obtain a modified filler.

[0040] In the present embodiment, the stirring speed of the stirring modification treatment is 450-500 r / min, and the stirring is performed for 1 hour. The sintering temperature of the blending sintering treatment is 210-220° C., and the sintering is performed for 1 hour.

[0041] The mass fraction of the sodium silicate solution in this embodiment is 2-5%; the mass fraction of the yttrium nitrate solution is 4-7%.

[0042] The preparation method of the kaolin liquid of this embodiment is:

[0043] The kaolin is heat-treated at 145-155°C for 1 hour, then cooled to 55°C at a rate of 2-5°C / min, kept warm, and the kept warm kaolin is fully stirred in a treatment liquid that is 3-5 times the total amount of the kept warm kaolin to obtain a kaolin liquid.

[0044] The treatment solution of this embodiment includes the following raw materials in parts by weight: 2-5 parts of nanocellulose, 1-3 parts of calcium carbonate, 4-7 parts of dopamine hydrochloride solution, and 1-2 parts of silicon carbide.

[0045] The mass fraction of the dopamine hydrochloride solution in this embodiment is 2-5%.

[0046] Example 1

[0047] The coating and laminating process of this embodiment includes the following steps:

[0048] Step 1, preparation of film solution:

[0049] Add 5 parts of a crosslinking agent and 4 parts of a modified filler to 35 parts of an epoxy resin glue solution and stir until the stirring is complete to obtain a film solution;

[0050] Step 2: Use a polyimide (PI) film as the base film, and then apply the adhesive film liquid to the surface of the polyimide (PI) film with a coating thickness of 1 mm.

[0051] The stirring speed of the stirring process was 350 r / min, the stirring time was 2 h, and the stirring temperature was 55°C.

[0052] The cross-linking agent in this embodiment is tricyclohexylphosphine; the epoxy resin glue is an epoxy resin diluent to keep the viscosity of the epoxy resin at 0.3 Pa.s.

[0053] The preparation method of the modified filler of this embodiment is:

[0054] S1: preheating nano-aluminum nitride at 55°C for 1 hour, and evenly mixing 4 parts of the preheated nano-aluminum nitride and 3 parts of kaolin solution to obtain a mixed modifier;

[0055] S2: stirring the carbon nanotubes in a modification solution that is three times the total amount of the carbon nanotubes for modification treatment. After stirring, filtering and drying to obtain modified carbon nanotubes;

[0056] The preparation method of the modified liquid is as follows:

[0057] 2 parts of sodium silicate solution, 3 parts of boron nitride and 1 part of yttrium nitrate solution are mixed evenly to prepare a modified solution;

[0058] S3: The modified carbon nanotubes, titanium oxide, and lanthanum oxide are mixed and sintered in a weight ratio of 5:3:3, and the sintering is completed to obtain a sintered body;

[0059] S4: The sintered body and the modified modifier are mixed in a weight ratio of 7:3 and ball-milled at a ball-milling speed of 1500 r / min for 2 h. After the ball-milling is completed, the mixture is filtered and dried to obtain a modified filler.

[0060] In the present embodiment, the stirring speed of the stirring modification treatment is 450 r / min, and the stirring is performed for 1 hour; the sintering temperature of the blending sintering treatment is 210° C., and the sintering is performed for 1 hour.

[0061] The mass fraction of the sodium silicate solution in this embodiment is 2%; the mass fraction of the yttrium nitrate solution is 4%.

[0062] The preparation method of the kaolin liquid of this embodiment is:

[0063] The kaolin was heat-treated at 145°C for 1 hour, then cooled to 55°C at a rate of 2°C / min and kept warm. The kept warm kaolin was fully stirred in a treatment liquid that was 3 times the total amount of the kept warm kaolin to obtain a kaolin liquid.

[0064] The treatment solution of this embodiment includes the following raw materials in parts by weight: 2 parts of nanocellulose, 1 part of calcium carbonate, 4 parts of dopamine hydrochloride solution and 1 part of silicon carbide.

[0065] The mass fraction of the dopamine hydrochloride solution in this embodiment is 2%.

[0066] Example 2

[0067] The coating and laminating process of this embodiment includes the following steps:

[0068] Step 1, preparation of film solution:

[0069] Add 10 parts of a crosslinking agent and 7 parts of a modified filler to 45 parts of an epoxy resin glue solution and stir until the stirring is complete to obtain a film solution;

[0070] Step 2: Use a polyimide (PI) film as the base film, and then apply the adhesive film liquid to the surface of the polyimide (PI) film with a coating thickness of 2 mm.

[0071] The stirring process in this embodiment has a stirring speed of 400 r / min, a stirring time of 2 h, and a stirring temperature of 60°C.

[0072] The crosslinking agent in this embodiment is tricyclohexylphosphine; the epoxy resin glue is an epoxy resin diluent to maintain the viscosity of the epoxy resin at 0.7 Pa.s.

[0073] The preparation method of the modified filler of this embodiment is:

[0074] S1: preheating nano-aluminum nitride at 60°C for 1 hour, and evenly blending 7 parts of the preheated nano-aluminum nitride and 5 parts of kaolin solution to obtain a mixed modifier;

[0075] S2: stirring the carbon nanotubes in a modification solution that is 3-5 times the total amount of the carbon nanotubes for modification treatment, filtering and drying after the stirring is completed to obtain modified carbon nanotubes;

[0076] The preparation method of the modified liquid is as follows:

[0077] 5 parts of sodium silicate solution, 5 parts of boron nitride solution and 3 parts of yttrium nitrate solution were evenly mixed to prepare a modified solution;

[0078] S3: The modified carbon nanotubes, titanium oxide, and lanthanum oxide are mixed and sintered in a weight ratio of 8:5:3, and the sintering is completed to obtain a sintered body;

[0079] S4: The sintered body and the modified modifier are mixed in a weight ratio of 7:5 and ball-milled at a ball-milling speed of 1500 r / min for 2 h. After the ball-milling is completed, the mixture is filtered and dried to obtain a modified filler.

[0080] In the present embodiment, the stirring speed of the stirring modification treatment is 500 r / min, and the stirring is performed for 1 hour; the sintering temperature of the blending sintering treatment is 220° C., and the sintering is performed for 1 hour.

[0081] The mass fraction of the sodium silicate solution in this embodiment is 5%; the mass fraction of the yttrium nitrate solution is 7%.

[0082] The preparation method of the kaolin liquid of this embodiment is:

[0083] The kaolin was heat treated at 155°C for 1 hour, then cooled to 55°C at a rate of 5°C / min and kept warm. The kept warm kaolin was fully stirred in a treatment liquid that was 5 times the total amount of the kept warm kaolin to obtain a kaolin liquid.

[0084] The treatment solution of this embodiment includes the following raw materials in parts by weight: 5 parts of nanocellulose, 3 parts of calcium carbonate, 7 parts of dopamine hydrochloride solution and 2 parts of silicon carbide.

[0085] The mass fraction of the dopamine hydrochloride solution in this embodiment is 5%.

[0086] Example 3

[0087] The coating and laminating process of this embodiment includes the following steps:

[0088] Step 1, preparation of film solution:

[0089] Add 7.5 parts of a crosslinking agent and 5.5 parts of a modified filler to 40 parts of an epoxy resin glue solution, stirring the mixture until the stirring is complete, to obtain a film solution;

[0090] Step 2: Use a polyimide (PI) film as the base film, and then apply the adhesive film liquid to the surface of the polyimide (PI) film with a coating thickness of 1.5 mm.

[0091] The stirring speed of the stirring process in this embodiment is 370 r / min, the stirring time is 2 h, and the stirring temperature is 58°C.

[0092] The cross-linking agent in this embodiment is tricyclohexylphosphine; the epoxy resin glue is an epoxy resin diluent to maintain the viscosity of the epoxy resin at 0.35 Pa.s.

[0093] The preparation method of the modified filler of this embodiment is:

[0094] S1: preheating nano-aluminum nitride at 58°C for 1 hour, and evenly mixing 5.5 parts of the preheated nano-aluminum nitride and 4 parts of kaolin solution to obtain a mixed modifier;

[0095] S2: stirring the carbon nanotubes in a modification solution that is 4 times the total amount of the carbon nanotubes for modification treatment, filtering and drying after the stirring is completed to obtain modified carbon nanotubes;

[0096] The preparation method of the modified liquid is as follows:

[0097] 3.5 parts of sodium silicate solution, 4 parts of boron nitride and 2 parts of yttrium nitrate solution were mixed evenly to prepare a modified solution;

[0098] S3: The modified carbon nanotubes, titanium oxide, and lanthanum oxide are mixed and sintered in a weight ratio of 6.5:4:3, and the sintering is completed to obtain a sintered body;

[0099] S4: The sintered body and the modified modifier are mixed in a weight ratio of 7:4 and ball-milled at a ball-milling speed of 1500 r / min for 2 h. After the ball-milling is completed, the mixture is filtered and dried to obtain a modified filler.

[0100] In the present embodiment, the stirring speed of the stirring modification treatment is 470 r / min, and the stirring is performed for 1 hour. The sintering temperature of the blending sintering treatment is 215° C., and the sintering is performed for 1 hour.

[0101] The mass fraction of the sodium silicate solution in this embodiment is 3.5%; the mass fraction of the yttrium nitrate solution is 5.5%.

[0102] The preparation method of the kaolin liquid of this embodiment is:

[0103] The kaolin is heat-treated at 145-155°C for 1 hour, then cooled to 55°C at a rate of 2-5°C / min, kept warm, and the kept warm kaolin is fully stirred in a treatment liquid that is 3-5 times the total amount of the kept warm kaolin to obtain a kaolin liquid.

[0104] The treatment solution of this embodiment includes the following raw materials in parts by weight: 3.5 parts of nanocellulose, 2 parts of calcium carbonate, 5.5 parts of dopamine hydrochloride solution and 1.5 parts of silicon carbide.

[0105] The mass fraction of the dopamine hydrochloride solution in this embodiment is 3.5%.

[0106] Example 4

[0107] The coating and laminating process of this embodiment includes the following steps:

[0108] Step 1, preparation of film solution:

[0109] Add 6 parts of a crosslinking agent and 5 parts of a modified filler to 38 parts of an epoxy resin glue solution and stir until the stirring is complete to obtain a film solution;

[0110] Step 2: Use a polyimide (PI) film as the base film, and then apply the adhesive film liquid to the surface of the polyimide (PI) film with a coating thickness of 1 mm.

[0111] Preferably, the stirring speed of the stirring treatment is 360 r / min, the stirring time is 2 h, and the stirring temperature is 57° C.

[0112] The cross-linking agent in this embodiment is tricyclohexylphosphine; the epoxy resin glue is an epoxy resin diluent to keep the viscosity of the epoxy resin at 0.4 Pa.s.

[0113] The preparation method of the modified filler of this embodiment is:

[0114] S1: preheating nano-aluminum nitride at 56°C for 1 hour, and evenly mixing 5 parts of the preheated nano-aluminum nitride and 4 parts of kaolin solution to obtain a mixed modifier;

[0115] S2: stirring the carbon nanotubes in a modification solution that is three times the total amount of the carbon nanotubes for modification treatment. After stirring, filtering and drying to obtain modified carbon nanotubes;

[0116] The preparation method of the modified liquid is as follows:

[0117] 3 parts of sodium silicate solution, 4 parts of boron nitride and 1 part of yttrium nitrate solution were mixed evenly to prepare a modified solution;

[0118] S3: The modified carbon nanotubes, titanium oxide, and lanthanum oxide are mixed and sintered in a weight ratio of 6:3:3, and the sintering is completed to obtain a sintered body;

[0119] S4: The sintered body and the modified modifier are mixed in a weight ratio of 7:4 and ball-milled at a ball-milling speed of 1500 r / min for 2 h. After the ball-milling is completed, the mixture is filtered and dried to obtain a modified filler.

[0120] In the present embodiment, the stirring speed of the stirring modification treatment is 460 r / min, and the stirring is performed for 1 hour; the sintering temperature of the blending sintering treatment is 212° C., and the sintering is performed for 1 hour.

[0121] The mass fraction of the sodium silicate solution in this embodiment is 3%; the mass fraction of the yttrium nitrate solution is 5%.

[0122] The preparation method of the kaolin liquid of this embodiment is:

[0123] The kaolin is heat-treated at 145-155°C for 1 hour, then cooled to 55°C at a rate of 2-5°C / min, kept warm, and the kept warm kaolin is fully stirred in a treatment liquid that is 3-5 times the total amount of the kept warm kaolin to obtain a kaolin liquid.

[0124] The treatment solution of this embodiment includes the following raw materials in parts by weight: 3 parts of nanocellulose, 2 parts of calcium carbonate, 4 parts of dopamine hydrochloride solution and 1 part of silicon carbide.

[0125] The mass fraction of the dopamine hydrochloride solution in this embodiment is 3%.

[0126] Example 5

[0127] The coating and laminating process of this embodiment includes the following steps:

[0128] Step 1, preparation of film solution:

[0129] Add 9 parts of a cross-linking agent and 6 parts of a modified filler to 42 parts of an epoxy resin glue solution and stir until the stirring is complete to obtain a film solution;

[0130] Step 2: Use a polyimide (PI) film as the base film, and then apply the adhesive film liquid to the surface of the polyimide (PI) film with a coating thickness of 2 mm.

[0131] Preferably, the stirring speed of the stirring treatment is 390 r / min, the stirring time is 2 h, and the stirring temperature is 58° C.

[0132] The cross-linking agent in this embodiment is tricyclohexylphosphine; the epoxy resin glue is an epoxy resin diluent to maintain the viscosity of the epoxy resin at 0.3-0.7 Pa.s.

[0133] The preparation method of the modified filler of this embodiment is:

[0134] S1: Preheat nano-aluminum nitride at 58°C for 1 hour, and evenly blend 6 parts of the preheated nano-aluminum nitride and 4 parts of kaolin solution to obtain a mixed modifier;

[0135] S2: stirring the carbon nanotubes in a modification solution that is 4 times the total amount of the carbon nanotubes for modification treatment, filtering and drying after the stirring is completed to obtain modified carbon nanotubes;

[0136] The preparation method of the modified liquid is as follows:

[0137] 4 parts of sodium silicate solution, 4 parts of boron nitride solution and 2 parts of yttrium nitrate solution were mixed evenly to prepare a modified solution;

[0138] S3: The modified carbon nanotubes, titanium oxide, and lanthanum oxide are mixed and sintered in a weight ratio of 6:4:3, and the sintering is completed to obtain a sintered body;

[0139] S4: The sintered body and the modified modifier are mixed in a weight ratio of 7:5 and ball-milled at a ball-milling speed of 1500 r / min for 2 h. After the ball-milling is completed, the mixture is filtered and dried to obtain a modified filler.

[0140] In the present embodiment, the stirring speed of the stirring modification treatment is 490 r / min, and the stirring is performed for 1 hour; the sintering temperature of the blending sintering treatment is 215° C., and the sintering is performed for 1 hour.

[0141] The mass fraction of the sodium silicate solution in this embodiment is 4%; the mass fraction of the yttrium nitrate solution is 5%.

[0142] The preparation method of the kaolin liquid of this embodiment is:

[0143] The kaolin was heat treated at 152°C for 1 hour, then cooled to 55°C at a rate of 4°C / min and kept warm. The kept warm kaolin was fully stirred in a treatment liquid with a volume 4 times the total volume of the kept warm kaolin to obtain a kaolin liquid.

[0144] The treatment solution of this embodiment includes the following raw materials in parts by weight: 4 parts of nanocellulose, 2 parts of calcium carbonate, 6 parts of dopamine hydrochloride solution and 2 parts of silicon carbide.

[0145] The mass fraction of the dopamine hydrochloride solution in this embodiment is 4%.

[0146] Comparative Example 1.

[0147] The difference from Example 3 is that no modified filler is added.

[0148] Comparative Example 2.

[0149] The difference from Example 3 is that no sintered body is added in the preparation of the modified filler.

[0150] Comparative Example 3.

[0151] The difference from Example 3 is that no modified carbon nanotubes are added to the sintered body.

[0152] Comparative Example 4.

[0153] The difference from Example 3 is that the modified carbon nanotubes are not treated with a modifying liquid.

[0154] Comparative Example 5.

[0155] The difference from Example 3 is that no miscellaneous modifier is added in the preparation of the modified filler.

[0156] Comparative Example 6.

[0157] The difference from Example 3 is that no kaolin solution is added in the preparation of the mixed modifier.

[0158] The products of Examples 1-5 and Comparative Examples 1-6 were subjected to performance tests, and the performance measurement results are as follows:

[0159]

[0160]

[0161] From Examples 1-5 and Comparative Examples 1-6, it can be concluded that the product of Example 3 of the present invention has excellent insulation, inter-film peelability, and barrier properties, and the product can achieve coordinated improvement;

[0162] When no modified filler is added to the product, the performance of the product deteriorates significantly. When the modified filler is used for treatment, the performance effect of the product is most significant. When no sintered body is added in the preparation of the modified filler, no modified carbon nanotubes are added to the sintered body, the modified carbon nanotubes are not treated with a modifying liquid, no miscellaneous modifier is added in the preparation of the modified filler, and no kaolin liquid is added in the preparation of the miscellaneous modifier, the performance of the product tends to deteriorate to varying degrees. The product raw material obtained by the specific method of the present invention has the most significant performance effect. The effects of other methods are not as obvious as those of the present invention.

[0163] The above is a detailed introduction to a solid waste-based, high-volume ultrafine fly ash antifreeze concrete and its preparation method provided by the present application. Specific examples are used herein to illustrate the principles and implementation methods of the present application. The description of the above embodiments is only used to help understand the method and core idea of ​​the present application. At the same time, for those skilled in the art, based on the ideas of the present application, other different forms of changes can be made on the basis of the above description. In summary, the content of this specification should not be understood as a limitation on the present application.

Claims

1. Coating composite process, characterized in that, The following steps are involved: Step 1, preparation of film solution: Add 5-10 parts of a crosslinking agent and 4-7 parts of a modified filler to 35-45 parts of an epoxy resin glue solution, stirring the mixture until the stirring is complete to obtain a film solution; Step 2: Use a polyimide (PI) film as the base film, and then apply the adhesive film liquid to the surface of the polyimide (PI) film with a coating thickness of 1-2 mm.

2. The coating composite process according to claim 1, characterized in that: The stirring speed of the stirring treatment is 350-400 r / min, the stirring time is 2 hours, and the stirring temperature is 55-60°C.

3. The coating composite process according to claim 1, characterized in that: The cross-linking agent is tricyclohexylphosphine; the epoxy resin glue is an epoxy resin diluent to maintain the viscosity of the epoxy resin at 0.3-0.7 Pa.s.

4. The coating composite process according to claim 1, characterized in that: The preparation method of the modified filler is as follows: S1: preheating nano-aluminum nitride at 55-60°C for 1 hour, and evenly mixing 4-7 parts of the preheated nano-aluminum nitride and 3-5 parts of kaolin solution to obtain a mixed modifier; S2: stirring the carbon nanotubes in a modification solution that is 3-5 times the total amount of the carbon nanotubes for modification treatment, filtering and drying after the stirring is completed to obtain modified carbon nanotubes; The preparation method of the modified liquid is as follows: 2-5 parts of sodium silicate solution, 3-5 parts of boron nitride and 1-3 parts of yttrium nitrate solution are uniformly mixed to prepare a modified solution; S3: The modified carbon nanotubes, titanium oxide and lanthanum oxide are mixed and sintered in a weight ratio of (5-8): (3-5): 3, and the sintering is completed to obtain a sintered body; S4: The sintered body and the modified modifier are mixed in a weight ratio of 7:(3-5) and ball-milled at a ball-milling speed of 1500 r / min for 2 h. After the ball-milling is completed, the mixture is filtered and dried to obtain a modified filler.

5. The coating composite process according to claim 4, characterized in that: The stirring speed of the stirring modification treatment is 450-500 r / min, and the stirring is 1 hour; the sintering temperature of the blending sintering treatment is 210-220° C., and the sintering is 1 hour.

6. The coating composite process according to claim 4, characterized in that: The mass fraction of the sodium silicate solution is 2-5%; the mass fraction of the yttrium nitrate solution is 4-7%.

7. The coating composite process according to claim 1, characterized in that: The preparation method of kaolin liquid is: The kaolin is heat-treated at 145-155°C for 1 hour, then cooled to 55°C at a rate of 2-5°C / min, kept warm, and the kept warm kaolin is fully stirred in a treatment liquid that is 3-5 times the total amount of the kept warm kaolin to obtain a kaolin liquid.

8. The coating composite process according to claim 7, characterized in that: The treatment liquid comprises the following raw materials in parts by weight: 2-5 parts of nanocellulose, 1-3 parts of calcium carbonate, 4-7 parts of dopamine hydrochloride solution and 1-2 parts of silicon carbide.

9. The coating composite process according to claim 8, characterized in that: The mass fraction of the dopamine hydrochloride solution is 2-5%.

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