CN113388312B - High-performance ceramic-based epoxy modified organic silicon coating and preparation and application methods thereof - Google Patents
High-performance ceramic-based epoxy modified organic silicon coating and preparation and application methods thereof Download PDFInfo
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Abstract
The high-performance ceramic-based epoxy modified organic silicon coating selects boehmite modified epoxy resin, epoxy modified organic silicon resin and a curing agent as main components, and the ceramic-based resin is gradually formed in the resin curing and crosslinking process, so that the high hardness and the wear resistance of the epoxy modified organic silicon coating are realized, and the epoxy modified organic silicon coating has excellent oil resistance and high temperature resistance. In addition, the ceramic-based epoxy modified organosilicon coating has the advantages of simple construction, no need of complex equipment, good film forming property of the prepared material and higher adhesive force. The ceramic-based epoxy modified organic silicon coating can realize scratch-resistant protection and corrosion protection effects on equipment, and meanwhile, the coating can also be widely applied to high-temperature protection of chimney, heat pipeline and other facilities, and has higher economic benefit.
Description
Technical Field
The invention relates to the technical field of high-temperature-resistant coating materials, in particular to a high-performance ceramic-based epoxy modified organic silicon coating and preparation and application methods thereof.
Background
Currently, there are two main types of high temperature resistant coatings commonly used in the prior art: one type is ceramic coatings and the other type is silicone coatings. The ceramic coating can be suitable for the environment with the temperature of more than 1000 ℃ by utilizing the high temperature resistance of the inorganic material, but has large construction difficulty, is not suitable for large components and has poor maintenance performance, so the application range is narrower. The organic silicon coating is mostly used in the environment below 1000 ℃, and is often used for high-temperature chimneys by utilizing the excellent construction convenience and high temperature resistance. The chimney part is usually positioned in the atmospheric environment, which requires that the organic silicon high-temperature resistant coating has certain corrosion resistance. Epoxy resin is an accepted anti-corrosion material in the industry, but the anti-corrosion property of the epoxy resin is poor, so that the anti-corrosion property of the organic silicon resin is improved and the anti-corrosion property of the epoxy resin is solved by modifying organic silicon with the epoxy resin.
Chinese patent CN102559048A discloses an epoxy modified organic silicon insulating heat-conducting high-temperature-resistant coating prepared by utilizing synthesized epoxy modified organic silicon resin, the invention gives consideration to the insulating, heat-conducting and high-temperature-resistant performances of the coating, the adhesive force of the paint film is 1 grade, the hardness is 5H, the paint film has no obvious change after 24 hours at 250 ℃, and the coating can be widely applied to various industrial equipment and household appliances. However, it is known from the disclosure that the epoxy modified silicone resin prepared in this patent employs a 1:1 mass ratio of epoxy to silicone resin. It is known that epoxy silicone resins are difficult to achieve a hardness of 4H or more when cured by direct heating, and when cured with a curing agent, they exhibit yellowing when used at 250 ℃ for 24 hours, although the hardness can be achieved. Therefore, the paint film provided by the patent is liable to have yellowing and aging conditions after being cured at high temperature, and the corresponding application performance cannot be ensured.
Meanwhile, the high-temperature protective coating material adopted by the control system of the shipboard aircraft engine in China at present is a conventional epoxy modified organic silicon coating, the hardness of the coating is low, and the coating is prepared by the following steps in the processes of storage, transportation and installation: the surface is easy to scratch and knock and damage, and the battle effectiveness of the weapon equipment in China is severely limited by frequent maintenance work.
Therefore, how to design and develop a high-temperature resistant coating which is convenient to construct, strong in adhesive force, high-temperature resistant and corrosion-resistant, good in scratch resistance effect and excellent in comprehensive performance is necessary for high-temperature protection of service facilities in special service environments such as an engine control box, a chimney and a heat pipeline.
Disclosure of Invention
The technical purpose of the invention is as follows: the high-performance ceramic-based epoxy modified organic silicon coating is prepared by using the boehmite modified epoxy resin and the epoxy organic silicon resin as base materials to participate in a curing reaction, so that the high-performance ceramic-based epoxy modified organic silicon coating has the excellent performances of convenience in construction, high-temperature resistance, corrosion resistance, scratch resistance, long protection period, capability of effectively reducing the maintenance cost, beautifying the coating effect, prolonging the service life of equipment facilities and the like.
In order to solve the technical problems, the invention adopts the technical scheme that: the high-performance ceramic-based epoxy modified organic silicon coating comprises the following components in parts by weight: 15-50 parts of matrix resin mixture, 10-40 parts of solvent, 1-10 parts of pigment filler, 20-60 parts of functional filler, 0.1-3 parts of functional additive and 1-10 parts of curing agent; wherein the matrix resin mixture is prepared from (1-3) by mass: 1 and an epoxy-modified silicone resin.
Preferably, the boehmite modified epoxy resin is one or two of nano-boehmite modified E44 epoxy resin and nano-boehmite modified E20 epoxy resin.
Preferably, the mass percentage of the epoxy resin in the epoxy modified silicone resin is 60% or 30%.
Preferably, the solvent is one or two of xylene and toluene.
Preferably, the pigment and filler is at least one of copper chromium black and boron nitride.
Preferably, the functional filler is at least one of alumina, aluminum tripolyphosphate and nano silver.
Preferably, the functional auxiliary agent is at least two of BYK-110, BYK-320, fumed silica and organic bentonite.
Preferably, the curing agent is one or two of silane modified amine curing agent and terminal amino silane coupling agent.
The preparation method of the high-performance ceramic-based epoxy modified organic silicon coating comprises the following steps:
step one, preparation of boehmite-modified epoxy resin solution
(1) According to the proportion of 1 g/(1.5-3) ml, respectively and fully mixing epoxy resin and a xylene solvent which is dehydrated in advance to prepare an epoxy resin diluent for later use;
(2) according to the proportion of 1 mol/(16-25) g of isocyanate and epoxy resin, adding isocyanate into the epoxy resin diluent prepared in the step (1), carrying out polymerization reaction for 3-4 h in the environment of 110-;
(3) respectively mixing boehmite and a xylene solvent according to the proportion of 1 g/(8-15) ml, performing ultrasonic dispersion treatment to obtain boehmite emulsion, adding anhydrous calcium chloride into the boehmite emulsion, performing dehydration treatment at 70-100 ℃ for 1.5-2.5h, and then filtering to remove filter residues to obtain boehmite dispersion for later use;
(4) according to the mass ratio of (4-5): (25-30) respectively weighing the boehmite dispersion liquid prepared in the step (3) and the epoxy prepolymer prepared in the step (2), then placing the weighed epoxy prepolymer into a reactor, dropwise adding the boehmite dispersion liquid into the reactor, controlling the reactor to be heated to 120-150 ℃ under the condition of continuous stirring for reaction for 4-6 hours, naturally cooling to room temperature, washing the obtained reaction product for multiple times by using water and ethanol, and drying to prepare boehmite modified epoxy resin for later use;
(5) adding a xylene solvent into the boehmite modified epoxy resin prepared in the step (4) according to the addition amount of 1g/ml, heating to 110-130 ℃ under the condition of continuous stirring, performing homogenization treatment for 1.5-2.5h, and naturally cooling to room temperature to obtain a boehmite modified epoxy resin solution for later use;
step two, preparation of matrix resin mixture
The weight ratio of (1-3): 1, respectively mixing the boehmite modified epoxy resin solution prepared in the step one with epoxy modified organic silicon resin, and then performing dispersion treatment for 25-40min under the temperature environment below 50 ℃ and the stirring condition of 1300-1700r/min to prepare a matrix resin mixture for later use;
step three, preparation of resin base material
According to the parts by weight, firstly, uniformly mixing the matrix resin mixture prepared in the step two with a solvent, then, adding a functional auxiliary agent into the mixture, and fully and uniformly mixing the mixture again to prepare a resin base material for later use;
step four, preparation of the coating A component
Respectively adding the pigment filler and the functional filler into the resin base material prepared in the third step according to the parts by weight, and performing dispersion treatment for 3-8min under the temperature environment below 50 ℃ and the stirring condition of 1500r/min for 1000-;
step five, preparation of finished coating
And (4) adding a curing agent into the coating A component prepared in the fourth step according to the parts by weight, and fully stirring and uniformly mixing to obtain the finished ceramic-based epoxy modified organic silicon coating.
The application method of the high-performance ceramic-based epoxy modified organic silicon coating comprises the step of coating the finished ceramic-based epoxy modified organic silicon coating on the surface of a base material to be protected in a brushing, spraying or roller coating mode; drying and curing the coating at the temperature of 10-35 ℃ for 20-30 h; and carrying out 180-230 ℃ high-temperature hardness strength treatment on the cured coating for 1.5-2.5 h.
The invention has the beneficial effects that:
1. according to the ceramic-based epoxy modified organic silicon coating provided by the invention, the boehmite modified epoxy resin and the epoxy modified organic silicon resin are used as base materials and matched with corresponding curing agents, the ceramic-based resin is gradually formed in the resin curing and crosslinking process, the high hardness and the wear resistance of the epoxy modified organic silicon coating are realized, and the epoxy modified organic silicon coating has excellent corrosion resistance and high temperature resistance and excellent comprehensive performance. In addition, the ceramic-based epoxy modified organosilicon coating has the advantages of simple construction, no need of complex equipment, good film forming property of the prepared material, higher adhesive force and the like. The ceramic-based epoxy modified organosilicon coating can obviously improve the scratch resistance of the surface of equipment, realize the scratch-resistant protection and corrosion protection effects on the equipment, save the construction and maintenance cost of the coating, improve the product performance, and meanwhile, the coating can also be widely applied to the high-temperature protection of chimney, heat pipeline and other facilities, thereby having higher economic benefit.
2. According to the ceramic-based epoxy modified organic silicon coating, in the selection of the raw material formula, the nano boehmite modified epoxy resin and the epoxy modified organic silicon resin are specifically selected for blending, in the curing and crosslinking processes of the two resins, one end of a molecular chain segment is provided with rigid particle alumina, the other end of the molecular chain segment is provided with organic silicon, and a ceramic organic film is gradually formed along with the mutual winding of the molecular chain segments and the increase of the rigid chain segment in the reaction process. The ceramic organic film inherits the excellent performances of high temperature resistance, high hardness and the like of a ceramic material, and gradually forms a ceramic-based high-temperature-resistant composite coating material with uniform texture and compact texture after the ceramic organic film is matched with the synergistic cooperation superposition protection effect of a pigment filler and a functional filler which are specific components, so that the finished coating material has ultrahigh hardness, good wear resistance and excellent high-temperature resistance, overcomes the defect of insufficient scratch resistance of the traditional epoxy modified organic silicon coating, can play a role in beautifying the coating effect and prolonging the service life of equipment facilities. The high-temperature protection device is particularly suitable for being used for high-temperature environment service equipment with high requirements on surface decoration, can realize maintenance-free equipment, achieves good anti-corrosion effect, can be widely applied to high-temperature protection of chimney, heat pipeline and other facilities, and has good practical effect.
3. The preparation process disclosed by the invention is simple in steps and convenient to operate, boehmite is introduced into the traditional epoxy resin for modification, so that boehmite is stably and reliably grafted on the surface of the epoxy resin, and after the prepared boehmite-modified epoxy resin, the epoxy-modified organic silicon resin and the curing agent are compounded, the finished ceramic-based epoxy-modified organic silicon coating has the properties of scratch resistance and wear resistance and can realize high-temperature resistance, so that the maintenance frequency is reduced. The finished paint has the advantages of simple construction, good film forming property, compact coating structure, good oil resistance and excellent adhesive force. The test shows that the coating adhesion is 1 grade; after an oil resistance test (RP-3 aviation kerosene 24 h; 4050 aviation lubricating oil resists oil for 24 h), the surface has no foaming, softening and damage phenomena; the high temperature resistance at 250 ℃ for 200h shows that the surface has no cracking, bubbling and falling off; the wear resistance (500 g/500 r) is only 8mg, which indicates that the coating can be applied to the high-temperature environment with higher requirement on the surface decoration of equipment, and has good anticorrosion effect and excellent comprehensive performance.
Drawings
FIG. 1 is a schematic structural view of a boehmite-modified epoxy resin prepared according to the present invention;
FIG. 2 is a photograph of the sample after painting and using the high performance ceramic based epoxy modified silicone coating of the present invention.
Detailed Description
The technical solution of the present invention is explained and explained in further detail below with reference to the accompanying drawings and specific embodiments:
the high-performance ceramic-based epoxy modified organic silicon coating comprises the following components in parts by weight: 15-50 parts of matrix resin mixture, 10-40 parts of solvent, 1-10 parts of pigment filler, 20-60 parts of functional filler, 0.1-3 parts of functional additive and 1-10 parts of curing agent; wherein the matrix resin mixture is prepared from (1-3) by mass: 1 and an epoxy-modified silicone resin, preferably (1-2): 1. the boehmite modified epoxy resin is one or two of nano-boehmite modified E44 epoxy resin and nano-boehmite modified E20 epoxy resin. The mass percentage of the epoxy resin in the epoxy modified organic silicon resin is 60% or 30%. The solvent is one or two of dimethylbenzene and methylbenzene. The pigment and filler is at least one of copper chromium black and boron nitride. The functional filler is at least one of alumina, aluminum tripolyphosphate and nano silver. The functional auxiliary agent is at least two of BYK-110, BYK-320, fumed silica and organic bentonite. The curing agent is one or two of silane modified amine curing agent and terminal amino silane coupling agent.
The preparation method of the high-performance ceramic-based epoxy modified organic silicon coating comprises the following steps:
step one, preparing a boehmite modified epoxy resin solution, wherein the preparation process comprises the steps of firstly, taking isocyanate as bridging to react with epoxy resin to prepare an epoxy prepolymer with an isocyanate group as a terminal group, and then removing hydroxyl in boehmite through a dehydration reaction to graft boehmite into an epoxy chain segment, and the preparation method specifically comprises the following steps:
(1) according to the proportion of 1 g/(1.5-3) ml, respectively placing epoxy resin and a xylene solvent which is subjected to dehydration treatment in advance into a reactor with magnetic stirring, and fully stirring and uniformly mixing to prepare an epoxy resin diluent for later use;
(2) at room temperature, according to the proportion that isocyanate and epoxy resin are 1 mol/(16-25) g, taking bridging reactant isocyanate to slowly add into the epoxy resin diluent prepared in the step (1), carrying out polymerization reaction for 3-4 h in the environment of 110-130 ℃ under the condition of continuous stirring, and then heating the obtained reaction product to 140 ℃ to remove xylene solvent to prepare an epoxy prepolymer for later use;
(3) respectively taking boehmite and a xylene solvent according to the proportion of 1 g/(8-15) ml, placing the boehmite and the xylene solvent in a reactor with mechanical stirring for mixing, preparing boehmite emulsion after ultrasonic dispersion treatment, then adding anhydrous calcium chloride into the boehmite emulsion, carrying out dehydration treatment for 1.5-2.5h at the temperature of 70-100 ℃, and then filtering to remove anhydrous calcium chloride filter residue to prepare boehmite dispersion for later use;
(4) according to the mass ratio of (4-5): (25-30) respectively weighing the boehmite dispersion liquid prepared in the step (3) and the epoxy prepolymer prepared in the step (2), then placing the weighed epoxy prepolymer into a reactor with mechanical stirring, slowly dropwise adding the boehmite dispersion liquid into the reactor, controlling the temperature of the reactor to be increased to 150 ℃ under the condition of continuous stirring, reacting for 4-6 hours at the temperature, naturally cooling to room temperature, washing the obtained reaction product for multiple times by using water and ethanol, and drying to prepare boehmite modified epoxy resin for later use;
(5) adding a xylene solvent into the boehmite modified epoxy resin prepared in the step (4) according to the addition amount of 1g/ml, heating to 110-130 ℃ under the condition of continuous stirring, carrying out homogenization treatment for 1.5-2.5h, and then naturally cooling to room temperature to obtain a boehmite modified epoxy resin solution with the mass fraction of 50% for later use;
step two, preparation of matrix resin mixture
The weight ratio of (1-3): 1, respectively mixing the boehmite modified epoxy resin solution prepared in the step one with epoxy modified organic silicon resin, then carrying out dispersion treatment for 25-40min under the stirring condition of 1300-;
step three, preparation of resin base material
According to the parts by weight, firstly, uniformly mixing the matrix resin mixture prepared in the step two with a solvent, then, adding a functional auxiliary agent into the mixture, and fully and uniformly mixing the mixture again to prepare a resin base material for later use;
step four, preparation of the coating A component
Respectively adding the pigment filler and the functional filler into the resin base material prepared in the third step according to the parts by weight, performing dispersion treatment for 3-8min under the stirring condition of 1000-1500r/min, and controlling the material temperature below 50 ℃ to prepare a coating A component for later use;
step five, preparation of finished coating
And C, adding the coating component B, namely the curing agent, into the coating component A prepared in the step four according to the parts by weight, and fully stirring and uniformly mixing to obtain the finished ceramic-based epoxy modified organic silicon coating.
The application method of the high-performance ceramic-based epoxy modified organic silicon coating comprises the step of coating the finished ceramic-based epoxy modified organic silicon coating on the surface of a base material to be protected in a brushing, spraying or roller coating mode; naturally placing the coating at the temperature of 10-35 ℃, drying and curing for 20-30 h; and the cured coating is subjected to hardness strength treatment for 1.5-2.5h under the high temperature condition of 180-230 ℃. Wherein the humidity at the time of the drying and curing treatment is preferably less than 85%.
After the high-performance ceramic-based epoxy modified organic silicon coating prepared by the invention is coated and used, the high-performance ceramic-based epoxy modified organic silicon coating can play a role in high-temperature corrosion resistance and scratch resistance, and can be used for protecting equipment with scratch resistance and high-temperature requirements and supporting facilities thereof. The epoxy modified organic silicon coating is convenient and fast to construct, long in protection period, capable of effectively reducing maintenance cost, beautifying coating effect, prolonging service life of equipment facilities, making up for the defect of poor scratch resistance of the traditional epoxy modified organic silicon coating, and good in practical effect.
Example 1
The specific formula of the high-performance ceramic-based epoxy modified organosilicon coating is as follows:
table 1 ingredient table of example 1
The specific preparation method of the high-performance ceramic-based epoxy modified organosilicon coating provided by the embodiment comprises the following steps:
step one, preparation of boehmite-modified epoxy resin solution
(1) Placing 20g of epoxy resin and 40ml of xylene solvent which is dehydrated in advance in a reactor with magnetic stirring, fully and uniformly stirring to prepare epoxy resin diluent, then slowly adding 1mol of bridging reactant isocyanate into the epoxy resin diluent, carrying out polymerization reaction for 3.5 hours at the temperature of 120 ℃, and then heating the obtained reaction product to 140 ℃ to remove the xylene solvent to prepare an epoxy prepolymer for later use;
(2) putting 1g of boehmite and 10ml of xylene solvent into a reactor with mechanical stirring for mixing to prepare boehmite emulsion, then adding 10g of anhydrous calcium chloride into the boehmite emulsion, carrying out dehydration treatment at 80 ℃ for 2h, and then filtering to remove anhydrous calcium chloride filter residue to prepare boehmite dispersion for later use;
(3) placing 9g of the epoxy prepolymer prepared in the step (1) in a reactor with mechanical stirring, then weighing 60g of boehmite dispersion prepared in the step (2) and slowly dropwise adding the boehmite dispersion into the reactor, controlling the temperature of the reactor to rise to 140 ℃ under the condition of continuous stirring, reacting for 5 hours at the temperature, naturally cooling to room temperature, washing the obtained reaction product for multiple times by using water and ethanol, drying to obtain boehmite modified epoxy resin, adding a xylene solvent into the boehmite modified epoxy resin according to the addition amount of 1g/ml, heating to 120 ℃ under the condition of continuous stirring, homogenizing for 2 hours, and naturally cooling to room temperature to obtain boehmite modified epoxy resin solution for later use;
step two, preparation of matrix resin mixture
Taking 14g of nano boehmite modified E44 epoxy resin solution and 9g of epoxy modified organic silicon resin, carrying out dispersion treatment for 30min under the stirring condition of 1500r/min, and controlling the material temperature below 50 ℃ in the process to prepare a uniformly dispersed matrix resin mixture for later use;
step three, preparation of resin base material
Firstly weighing 35g of dimethylbenzene, placing the dimethylbenzene into the matrix resin mixture prepared in the second step, fully and uniformly mixing, then weighing 0.2g of BYK110 and 1g of fumed silica, placing the BYK110 and the fumed silica into the matrix resin mixture, and fully and uniformly mixing again to prepare a resin base material for later use;
step four, preparation of the coating A component
Weighing 4.6g of copper-chromium black, 3g of boron nitride, 31g of aluminum oxide, 4g of aluminum tripolyphosphate and 0.2g of nano silver, adding the materials into the resin base material prepared in the third step together, performing dispersion treatment for 5min under the stirring condition of 1300r/min, and controlling the material temperature below 50 ℃ in the process to prepare a coating A component for later use;
step five, preparation of finished coating
And 4g of silane modified amine curing agent is added into the coating component A prepared in the fourth step, and the ceramic-based epoxy modified organic silicon coating is obtained after the mixture is fully stirred and uniformly mixed.
When the ceramic-based epoxy modified organic silicon coating is used specifically, the ceramic-based epoxy modified organic silicon coating is coated on the surface of a substrate to be protected in a spraying mode, then the substrate needs to be placed in a room temperature condition of 25 ℃ for drying and curing for 24 hours, then the substrate is placed in a drying box of 200 ℃ in a transferring mode, the internal humidity is kept less than 85%, and hardness strengthening treatment is carried out for 2 hours.
Example 2
The specific formula of the high-performance ceramic-based epoxy modified organosilicon coating is as follows:
table 2 ingredient table of example 2
The specific preparation method of the high-performance ceramic-based epoxy modified organosilicon coating of the embodiment comprises the following steps:
step one, preparation of boehmite-modified epoxy resin solution
(1) Placing 20g of epoxy resin and 30ml of xylene solvent which is dehydrated in advance in a reactor with magnetic stirring, fully and uniformly stirring to prepare epoxy resin diluent, then slowly adding 1.25mol of bridging reactant isocyanate into the epoxy resin diluent, carrying out polymerization reaction for 3 hours at the temperature of 130 ℃, then heating the obtained reaction product to 140 ℃ to remove the xylene solvent to prepare an epoxy prepolymer for later use;
(2) putting 1g of boehmite and 8ml of xylene solvent into a reactor with mechanical stirring for mixing to prepare boehmite emulsion, then adding 9g of anhydrous calcium chloride into the boehmite emulsion, carrying out dehydration treatment at 70 ℃ for 2.5h, and then filtering to remove anhydrous calcium chloride filter residue to prepare boehmite dispersion for later use;
(3) placing 10g of the epoxy prepolymer prepared in the step (1) in a reactor with mechanical stirring, then weighing 50g of boehmite dispersion prepared in the step (2) and slowly dropwise adding the boehmite dispersion into the reactor, controlling the temperature of the reactor to rise to 120 ℃ under the condition of continuous stirring, reacting for 4 hours at the temperature, naturally cooling to room temperature, washing the obtained reaction product for multiple times by using water and ethanol, drying to obtain boehmite modified epoxy resin, adding a xylene solvent into the boehmite modified epoxy resin according to the addition amount of 1g/ml, heating to 110 ℃ under the condition of continuous stirring, homogenizing for 2.5 hours, and naturally cooling to room temperature to obtain a boehmite modified epoxy resin solution for later use;
step two, preparation of matrix resin mixture
Taking 18g of nano boehmite modified E44 epoxy resin solution and 16g of epoxy modified organic silicon resin, carrying out dispersion treatment for 25min under the stirring condition of 1700r/min, and controlling the material temperature below 50 ℃ in the process to prepare a uniformly dispersed matrix resin mixture for later use;
step three, preparation of resin base material
Firstly weighing 25g of xylene and 13g of toluene, placing the xylene and the toluene in the matrix resin mixture prepared in the second step, fully and uniformly mixing, then weighing 0.5g of BYK110 and 2g of fumed silica, placing the mixture in the matrix resin mixture, fully and uniformly mixing again to prepare a resin base material for later use;
step four, preparation of the coating A component
Weighing 4g of copper-chromium black, 3.5g of boron nitride, 35g of aluminum oxide and 0.3g of nano silver, adding the copper-chromium black, the boron nitride, the aluminum oxide and the nano silver into the resin base material prepared in the third step together, performing dispersion treatment for 8min under the stirring condition of 1000r/min, and controlling the material temperature below 50 ℃ in the process to prepare a coating A component for later use;
step five, preparation of finished coating
And (4) adding 8g of terminal aminosilane coupling agent into the coating A component prepared in the fourth step, and fully stirring and uniformly mixing to obtain the finished ceramic-based epoxy modified organic silicon coating.
When the ceramic-based epoxy modified organic silicon coating is used specifically, the coating is coated on the surface of a substrate to be protected in a brushing mode, then the substrate needs to be placed at 35 ℃ and room temperature for drying and curing for 20 hours, then the substrate is placed in a drying box at 180 ℃, the internal humidity is kept less than 85%, and the hardness strengthening treatment is carried out for 2.5 hours.
Example 3
The specific formula of the high-performance ceramic-based epoxy modified organosilicon coating is as follows:
table 3 ingredient table of example 3
The specific preparation method of the high-performance ceramic-based epoxy modified organosilicon coating provided by the embodiment comprises the following steps:
step one, preparation of boehmite-modified epoxy resin solution
(1) Placing 20g of epoxy resin and 60ml of xylene solvent which is dehydrated in advance in a reactor with magnetic stirring, fully and uniformly stirring to prepare epoxy resin diluent, then slowly adding 0.8mol of bridging reactant isocyanate into the epoxy resin diluent, carrying out polymerization reaction for 4 hours at the temperature of 110 ℃, then heating the obtained reaction product to 140 ℃ to remove the xylene solvent to prepare an epoxy prepolymer for later use;
(2) putting 1g of boehmite and 15ml of a xylene solvent into a reactor with mechanical stirring for mixing to prepare boehmite emulsion, then adding 15g of anhydrous calcium chloride into the boehmite emulsion, dehydrating for 1.5 hours at the temperature of 100 ℃, and then filtering to remove anhydrous calcium chloride filter residues to prepare boehmite dispersion for later use;
(3) putting 8g of the epoxy prepolymer prepared in the step (1) into a reactor with mechanical stirring, then weighing 60g of boehmite dispersion prepared in the step (2), slowly dropwise adding into the reactor, controlling the temperature of the reactor to rise to 150 ℃ under the condition of continuous stirring, reacting for 6 hours at the temperature, naturally cooling to room temperature, washing the obtained reaction product for multiple times by using water and ethanol, drying to obtain boehmite modified epoxy resin, adding a xylene solvent into the boehmite modified epoxy resin according to the addition amount of 1g/ml, heating to 130 ℃ under the condition of continuous stirring, homogenizing for 1.5 hours, and naturally cooling to room temperature to obtain a boehmite modified epoxy resin solution for later use;
step two, preparation of matrix resin mixture
Taking 20g of nano boehmite modified E20 epoxy resin solution and 20g of epoxy modified organic silicon resin, carrying out dispersion treatment for 40min under the stirring condition of 1300r/min, and controlling the material temperature below 50 ℃ in the process to prepare a uniformly dispersed matrix resin mixture for later use;
step three, preparation of resin base material
Weighing 30g of toluene, placing the toluene in the matrix resin mixture prepared in the second step, fully and uniformly mixing, weighing 0.5g of BYK110 and 3g of fumed silica, placing the BYK110 and the fumed silica in the matrix resin mixture, and fully and uniformly mixing again to prepare a resin base material for later use;
step four, preparation of the coating A component
Weighing 5g of copper-chromium black, 4g of boron nitride, 40g of aluminum oxide and 0.4g of nano silver, adding the materials into the resin base material prepared in the third step together, performing dispersion treatment for 3min under the stirring condition of 1500r/min, and controlling the material temperature below 50 ℃ in the process to prepare a coating A component for later use;
step five, preparation of finished coating
And (4) adding 3g of silane modified amine curing agent into the coating component A prepared in the step four, and fully stirring and uniformly mixing to obtain the finished ceramic-based epoxy modified organic silicon coating.
When the ceramic-based epoxy modified organic silicon coating is used specifically, the ceramic-based epoxy modified organic silicon coating is coated on the surface of a substrate to be protected in a roller coating mode, then the substrate needs to be placed at 10 ℃ and room temperature for drying and curing for 30 hours, then the substrate is placed in a drying box at 230 ℃ and kept with the internal humidity less than 85%, and then the hardness strengthening treatment is carried out for 1.5 hours.
Example 4
The specific formula of the high-performance ceramic-based epoxy modified organosilicon coating is as follows:
table 4 ingredient table of example 4
The preparation process of the ceramic-based epoxy modified silicone coating of this example is the same as example 1. Only the specific materials and contents of the components are modified correspondingly.
Example 5
The specific formula of the high-performance ceramic-based epoxy modified organosilicon coating is as follows:
table 5 ingredient table of example 5
The preparation process of the ceramic-based epoxy modified organosilicon coating of the embodiment is the same as that of the embodiment 1, and only the specific materials and contents of the components are modified correspondingly.
The paint of each example of the invention was tested for performance and the results are shown in the following table:
table 6 results of performance testing
The results of the performance index test in table 6 show that:
the result of the adhesion test of the high-performance ceramic-based epoxy modified organic silicon coating prepared by the invention is grade 1; the loss of abrasion resistance is less than or equal to 8 mg; after the paint film is soaked for 24 hours in oil resistance, the paint film has no foaming, softening and breakage phenomena; after the high temperature test of 250 ℃ and 200h, the surface of the coating has no phenomena of cracking, bubbling and falling off, and the paint film only slightly changes color or does not change color; the pencil hardness of the paint film reaches more than 8H, and the coating does not have bubbling, falling and rusting after a salt spray resistance test is carried out for 1000H, and has excellent comprehensive performance.
The above examples are provided for clarity of illustration only and are not intended to limit the invention to the particular embodiments described. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And obvious variations or modifications can be made without departing from the scope of the invention as claimed.
Claims (9)
1. The high-performance ceramic-based epoxy modified organosilicon coating is characterized by comprising the following components in parts by weight: 15-50 parts of matrix resin mixture, 10-40 parts of solvent, 1-10 parts of pigment filler, 20-60 parts of functional filler, 0.1-3 parts of functional additive and 1-10 parts of curing agent; wherein the matrix resin mixture is prepared from (1-3) by mass: 1, wherein the mass percentage of the epoxy resin in the epoxy modified organic silicon resin is 60% or 30%;
the preparation method of the boehmite modified epoxy resin solution comprises the following steps:
(1) according to the proportion of 1 g/(1.5-3) ml, respectively and fully mixing epoxy resin and a xylene solvent which is dehydrated in advance to prepare an epoxy resin diluent for later use;
(2) according to the proportion of 1 mol/(16-25) g of isocyanate and epoxy resin, adding isocyanate into the epoxy resin diluent prepared in the step (1), carrying out polymerization reaction for 3-4 h in the environment of 110-;
(3) respectively mixing boehmite and a xylene solvent according to the proportion of 1 g/(8-15) ml, performing ultrasonic dispersion treatment to obtain boehmite emulsion, adding anhydrous calcium chloride into the boehmite emulsion, performing dehydration treatment at 70-100 ℃ for 1.5-2.5h, and then filtering to remove filter residues to obtain boehmite dispersion for later use;
(4) according to the mass ratio of (4-5): (25-30) respectively weighing the boehmite dispersion liquid prepared in the step (3) and the epoxy prepolymer prepared in the step (2), then placing the weighed epoxy prepolymer into a reactor, dropwise adding the boehmite dispersion liquid into the reactor, controlling the reactor to be heated to 120-150 ℃ under the condition of continuous stirring for reaction for 4-6 hours, naturally cooling to room temperature, washing the obtained reaction product for multiple times by using water and ethanol, and drying to prepare boehmite modified epoxy resin for later use;
(5) and (3) adding a xylene solvent into the boehmite modified epoxy resin prepared in the step (4) according to the addition amount of 1g/ml, heating to 110-130 ℃ under the condition of continuous stirring, carrying out homogenization treatment for 1.5-2.5h, and then naturally cooling to room temperature to obtain the boehmite modified epoxy resin solution.
2. The high performance ceramic based epoxy modified silicone coating of claim 1, characterized in that: the boehmite modified epoxy resin is one or two of nano-boehmite modified E44 epoxy resin and nano-boehmite modified E20 epoxy resin.
3. The high performance ceramic based epoxy modified silicone coating of claim 1, characterized in that: the solvent is one or two of dimethylbenzene and methylbenzene.
4. The high performance ceramic based epoxy modified silicone coating of claim 1, characterized in that: the pigment and filler is at least one of copper chromium black and boron nitride.
5. The high performance ceramic based epoxy modified silicone coating of claim 1, characterized in that: the functional filler is at least one of alumina, aluminum tripolyphosphate and nano silver.
6. The high performance ceramic based epoxy modified silicone coating of claim 1, characterized in that: the functional auxiliary agent is at least two of BYK-110, BYK-320, fumed silica and organic bentonite.
7. The high performance ceramic based epoxy modified silicone coating of claim 1, characterized in that: the curing agent is one or two of silane modified amine curing agent and terminal amino silane coupling agent.
8. The preparation method of the high-performance ceramic-based epoxy modified silicone coating according to claim 1, comprising the steps of:
step one, preparation of boehmite-modified epoxy resin solution
Preparing a boehmite modified epoxy resin solution according to the operation for later use;
step two, preparation of matrix resin mixture
The weight ratio of (1-3): 1, respectively mixing the boehmite modified epoxy resin solution prepared in the step one with epoxy modified organic silicon resin, and then performing dispersion treatment for 25-40min under the temperature environment below 50 ℃ and the stirring condition of 1300-1700r/min to prepare a matrix resin mixture for later use;
step three, preparation of resin base material
According to the parts by weight, firstly, uniformly mixing the matrix resin mixture prepared in the step two with a solvent, then, adding a functional auxiliary agent into the mixture, and fully and uniformly mixing the mixture again to prepare a resin base material for later use;
step four, preparation of the coating A component
Respectively adding the pigment filler and the functional filler into the resin base material prepared in the third step according to the parts by weight, and performing dispersion treatment for 3-8min under the temperature environment below 50 ℃ and the stirring condition of 1500r/min for 1000-;
step five, preparation of finished coating
And (4) adding a curing agent into the coating A component prepared in the fourth step according to the parts by weight, and fully stirring and uniformly mixing to obtain the finished ceramic-based epoxy modified organic silicon coating.
9. The method of applying a high performance ceramic based epoxy modified silicone coating of claim 1, wherein: coating the finished ceramic-based epoxy modified organic silicon coating on the surface of a base material to be protected in a brushing, spraying or roller coating mode; drying and curing the coating at the temperature of 10-35 ℃ for 20-30 h; and the cured coating is subjected to hardness strength treatment for 1.5-2.5h under the high temperature condition of 180-230 ℃.
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