CN115873492A - Laser-proof coating, preparation method and product - Google Patents
Laser-proof coating, preparation method and product Download PDFInfo
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Abstract
The invention discloses a laser-proof coating, a preparation method and a product, and relates to the technical field of coatings. The coating comprises the following raw materials in parts by weight: 1-10 parts of light-cured resin, 2-10 parts of active monomer, 0.1-1 part of photoinitiator, 80-100 parts of diluent, 0.5-4 parts of additive and 0.3-5 parts of auxiliary agent. The additive is prepared by loading molybdenum oxysulfide and tungsten oxysulfide nano materials on the surface of a carbon nano tube. The additive is added into the coating to improve the absorption efficiency of coating infrared light, and forms a better synergistic effect on the laser-proof performance, so that the optical density index of the material is improved. According to the application, the coating is coated on the substrate to obtain the product, the coating on the surface of the product has excellent wear resistance and antistatic performance, the adsorption of the material to dust can be reduced, and the application range of the laser-proof product is widened.
Description
Technical Field
The invention relates to the technical field of coatings, in particular to a laser-proof coating, a preparation method and a product.
Background
With the application and development of laser equipment in various fields, the laser protection performance of a laser equipment window is more and more concerned. The protective materials which are mature at present and applied to the laser protection window mainly comprise an absorption type, a reflection type and an absorption-reflection composite type, and the absorption type laser protection window is applied more at present. The absorption type laser protection window is usually formed by adding a nano absorbent having a strong absorption function for a specific spectrum into plastic or glass, so that the absorption type laser protection window has the characteristic of selectively absorbing laser with a specific wavelength.
The laser absorbing material may be classified into an inorganic type and an organic type, and may be classified into an ultraviolet absorber, a blue absorber, a green absorber, a near infrared absorber, a far infrared absorber, and the like according to an absorption band. The absorbent is added into a matrix such as plastic and the like, and a protective product with corresponding wavelength can be prepared. However, the plastic products usually need to be formed by extrusion, injection molding and other molding processes, and the processes are complex and the equipment is expensive. The absorption type protective coating is coated on the surface of the formed product, so that the production flexibility is greatly improved, and the product can be endowed with more performances such as scratch resistance, static resistance and the like through the coating. In recent years, absorption type infrared protective coatings are greatly developed, but the products are mainly applied to the field of heat insulation and cannot meet the requirement of high-power laser protection.
Therefore, a protective coating and a product applied to a window of a high-power laser device are urgently needed to be developed, and the protective coating and the product have the performances of scraping resistance, static electricity resistance and the like.
Disclosure of Invention
The invention aims to provide a laser-proof coating, a preparation method and a product, and solves the following technical problems:
the existing laser absorption material has poor laser protection performance.
The purpose of the invention can be realized by the following technical scheme:
the laser-proof coating composition comprises the following raw materials in parts by weight:
1-10 parts of light-cured resin, 2-10 parts of active monomer, 0.1-1 part of photoinitiator, 80-100 parts of diluent, 0.5-4 parts of additive and 0.3-5 parts of auxiliary agent.
As a further scheme of the invention: the light-cured resin is selected from any one of light-cured resin 6106, light-cured resin 7600B and light-cured resin 7605B, and the light-cured resin has good solubility in ethanol, isopropanol, n-propanol and butanol.
As a further scheme of the invention: the active monomer is one or more of tripropylene glycol diacrylate, dipentaerythritol hexaacrylate, hexanediol diacrylate, phthalic acid diethylene glycol diacrylate, neopentyl glycol diacrylate, pentaerythritol triacrylate, trimethylolpropane triacrylate and isoborneol acrylate which are mixed in any ratio.
As a further scheme of the invention: the preparation method of the additive comprises the following steps:
dissolving molybdenum pentachloride and tungsten hexachloride in carbon nano tube ethanol dispersion liquid, uniformly stirring, adding ammonia water to adjust the pH value of the solution to 8-9, adding polyvinylpyrrolidone and thiourea, heating to 180 ℃, and keeping the temperature for 12 hours to obtain the additive.
As a further scheme of the invention: the molybdenum pentachloride: tungsten hexachloride: carbon nanotube dispersion liquid: polyvinylpyrrolidone: the mass ratio of the thiourea is 0.5-30:0.1-1:20-50:3-8:1-4.
As a further scheme of the invention: the carbon nano tube ethanol dispersion liquid comprises the following raw materials in percentage by mass:
1-5 per mill of carbon nano tube
4 per mill to 2 percent of polymer dispersant
The balance of ethanol.
The carbon nano tube is a single-wall carbon nano tube, the tube diameter is 0.8-1.2nm, and the length is 0.2-2um.
As a further scheme of the invention: the polymer dispersant is polyvinylpyrrolidone, polyethylene glycol, and polyvinyl alcohol
As a further scheme of the invention: the photoinitiator is a deep photoinitiator TPO.
As a further scheme of the invention: as a further scheme of the invention: the photoinitiator also includes any one of the photoinitiators 184, 1173.
As a further scheme of the invention: the diluent is one or more of methanol, ethanol, n-propanol and butanol which are mixed in any ratio.
As a further scheme of the invention: the diluent is obtained by mixing an alcohol ether diluent and an alcohol diluent, wherein the alcohol ether diluent is obtained by mixing one or more of ethylene glycol ethyl ether, ethylene glycol butyl ether and diethylene glycol ethyl ether in any ratio, and the alcohol diluent is obtained by mixing one or more of methanol, ethanol, n-propanol and butanol in any ratio.
As a further scheme of the invention: the auxiliary agent comprises an antioxidant vulcanizing agent and a leveling agent.
As a further scheme of the invention: the antioxidant vulcanizing agent is 2, 6-di-tert-butyl-p-cresol.
As a further scheme of the invention: the leveling agent is polyether modified polysiloxane BYK333.
A preparation method of a laser-proof coating composition comprises the following steps:
(1) Stirring and mixing the light-cured resin, the active monomer, the diluent, the photoinitiator and the auxiliary agent to obtain a mixture A;
(2) And uniformly stirring the mixture A and the additive to obtain the laser-proof coating.
The laser-proof product is coated with the coating on the surface.
As a further scheme of the invention: the laser-proof coating is coated on a base material by a coating process, and then is dried and photocured to obtain a laser-proof product.
As a further scheme of the invention: the coating process can be spraying, curtain coating, dip coating, roll coating and brush coating.
As a further scheme of the invention: the drying conditions were: thermally curing at 60-70 deg.c for 5-8 min.
As a further scheme of the invention: the drying conditions were: three sections of temperature of 60 ℃, 68 ℃ and 60 ℃ are used for thermal curing, the curing time of each section is the same, and the total curing time is 5-8 minutes.
As a further scheme of the invention: the conditions for photocuring were: the dried product enters a light source area at the speed of 2-4m/min, and the cumulative radiation is 500-800mJ/cm 2 。
As a further scheme of the invention: the base material is any one of a PVC plate, a PC plate and a PMMA plate.
The invention has the beneficial effects that:
the additive is added into the coating components, and the additive prepared by the method is prepared by loading molybdenum oxysulfide and tungsten oxysulfide nano materials on the surface of a carbon nano tube. The ultra-large specific surface area of the carbon nanotube material is utilized to ensure that the carbon nanotube material is mixed with (Mo) x W y ) 2 O 2 The S nano material is firmly combined through Van der Waals force, and the agglomeration of the tissues in the coating affects the performance. Meanwhile, the carbon nano tube improves the absorption efficiency of infrared light, forms a better synergistic effect with the molybdenum oxysulfide and tungsten oxysulfide nano materials on the laser resistance, and improves the optical density index of the materials. Meanwhile, the coating and the UV light-cured resin form a composition, so that the coating has excellent wear resistance. The optical density of the laser-proof product prepared by the invention is OD4-6, and the light transmittance is 15% -60%. The coating has excellent antistatic performance and surface resistance of 10 6 -10 8 Omega. The coating has the adhesion of 0 grade, and the optical density and the surface resistance are not attenuated and are very stable after QUV accelerated aging test. The coating prepared by the method has excellent antistatic performance, and can reduce the adsorption of materials to dust, so that the application range of the laser-proof product is greatly widened.
Detailed Description
The following will clearly and completely describe the technical solutions in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The preparation method of the laser-proof coating comprises the following steps:
(1) Weighing 1.2g of molybdenum pentachloride and 0.8g of tungsten hexachloride raw materials, dissolving the raw materials in 50g of single-walled carbon nanotube ethanol dispersion liquid (the content of the single-walled carbon nanotube is 2 per mill), uniformly stirring, adding 1g of ammonia water to adjust the pH value of the solution, adding 4g of polyvinylpyrrolidone and 2g of thiourea, placing the mixture in a reaction kettle, heating to 180 ℃, keeping the temperature for 12 hours, and cooling to room temperature after the reaction is finished to obtain a mixture A, wherein the mixture A contains 4% by mass of additives;
(2) Weighing 2g of light-cured resin 7600B, 4g of active monomer PETA, 40g of ethanol, 0.8g of deep photoinitiator TPO, 0.8g of photoinitiator 184 and 0.2g of flatting agent BYK333, and uniformly stirring to obtain a mixture B;
(3) And slowly adding the mixture B into the mixture A, and uniformly stirring to obtain the laser-proof coating.
Example 2
The preparation method of the laser-proof coating comprises the following steps:
(1) Weighing 1.2g of molybdenum pentachloride and 0.8g of tungsten hexachloride raw materials, dissolving the raw materials in 50g of single-walled carbon nanotube ethanol dispersion liquid (the content of the single-walled carbon nanotube is 2 per mill), uniformly stirring, adding 1g of ammonia water to adjust the pH value of the solution, adding 4g of polyvinylpyrrolidone and 2g of thiourea, placing the mixture in a reaction kettle, heating to 180 ℃, keeping the temperature for 12 hours, and cooling to room temperature after the reaction is finished to obtain a mixture A, wherein the mixture A contains 4% by mass of additives;
(2) Weighing 2g of photocuring resin 6106, 4g of active monomer HDDA, 40g of ethanol, 0.8g of deep layer photoinitiator TPO, 0.8g of photoinitiator 184 and 0.2g of flatting agent BYK333, and uniformly stirring to obtain a mixture B;
(3) Slowly adding the mixture B into the mixture A, and uniformly stirring to obtain the laser-proof coating;
example 3
The preparation method of the laser-proof coating comprises the following steps:
(1) Weighing 2.4g of molybdenum pentachloride and 1.6g of tungsten hexachloride raw materials, dissolving the raw materials in 50g of single-walled carbon nanotube ethanol dispersion liquid (the content of the single-walled carbon nanotube is 2 per mill), uniformly stirring, adding 2g of ammonia water to adjust the pH value of the solution, adding 5g of polyvinylpyrrolidone and 2.5g of thiourea, placing the mixture in a reaction kettle, heating the mixture to 180 ℃, keeping the temperature for 12 hours, and cooling the mixture to room temperature after the reaction is finished to obtain a mixture A, wherein the mixture A contains 4% by mass of additives;
(2) Weighing 2g of light-cured resin 7600B, 4g of active monomer PETA, 40g of ethanol, 0.8g of deep photoinitiator TPO, 0.8g of photoinitiator 184 and 0.2g of flatting agent BYK333, and uniformly stirring to obtain a mixture B;
(3) Slowly adding the mixture B into the mixture A, and uniformly stirring to obtain the laser-proof coating.
Example 4
The preparation method of the laser-proof coating comprises the following steps:
(1) Weighing 0.3g of molybdenum pentachloride and 0.2g of tungsten hexachloride as raw materials, dissolving the raw materials in 50g of single-walled carbon nanotube ethanol dispersion liquid (the content of single-walled carbon nanotubes is 2 per mill), uniformly stirring, adding 2g of ammonia water to adjust the pH value of the solution, adding 5g of polyvinylpyrrolidone and 2.5g of thiourea, placing the mixture in a reaction kettle, heating the mixture to 180 ℃, keeping the temperature for 12 hours, and cooling the mixture to room temperature after the reaction is finished to obtain a mixture A, wherein the mixture A contains 4 mass percent of additives;
(2) Weighing 2g of photocuring resin 7600B, 4g of active monomer PETA, 40g of ethanol, 0.8g of deep layer photoinitiator TPO, 0.8g of photoinitiator 184 and 0.2g of flatting agent BYK333, and uniformly stirring to obtain a mixture B;
(3) And slowly adding the mixture B into the mixture A, and uniformly stirring to obtain the laser-proof coating.
Example 5
The preparation method of the laser-proof product comprises the following steps:
(1) The PMMA plate is first cleaned, including purging and solvent cleaning.
(2) The cleaned PMMA plate is coated by spraying with the anti-laser coating prepared in the embodiment 1, and the thickness of the coating is 7 mu m; then, three-stage drying was carried out at 65 ℃ for 8 minutes, respectively, to obtain a preform.
(3) The prefabricated product enters the light source area at the speed of 2m/min, and the cumulative radiation is 600mJ/cm 2 And obtaining the antistatic PMMA board.
Example 6
Compared with the example 5, only the laser-proof paint prepared in the example 1 is replaced by the laser-proof paint prepared in the example 2, and the rest steps are completely consistent.
Example 7
Compared with example 5, only the laser-proof paint prepared in example 1 is replaced by the laser-proof paint prepared in example 3, and the rest steps are completely consistent.
Example 8
Compared with the example 5, only the laser-proof paint prepared in the example 1 is replaced by the laser-proof paint prepared in the example 4, and the rest steps are completely consistent.
Comparative example 1
The preparation method of the laser-proof coating comprises the following steps:
(1) Weighing 1.2g of molybdenum pentachloride and 0.8g of tungsten hexachloride raw materials, dissolving the raw materials in 50g of ethanol, uniformly stirring, adding 1g of ammonia water to adjust the pH value of the solution, adding 4g of polyvinylpyrrolidone and 2g of thiourea, placing the mixture in a reaction kettle, heating the mixture to 180 ℃, keeping the temperature for 12 hours, and cooling the mixture to room temperature after the reaction is finished to obtain a laser absorbing material mixture A with the mass fraction of molybdenum oxysulfide and tungsten oxysulfide being about 4%;
(2) Weighing 2g of photocuring resin 7600B, 4g of active monomer PETA, 40g of ethanol, 0.8g of deep layer photoinitiator TPO, 0.8g of photoinitiator 184 and 0.2g of flatting agent BYK333, and uniformly stirring to obtain a mixture B;
(3) Slowly adding the mixture B into the mixture A, and uniformly stirring to obtain the laser-proof coating;
comparative example 2
The preparation method of the laser-proof coating comprises the following steps:
(1) Weighing 2.0g of tungsten hexachloride raw material, dissolving the raw material in 50g of ethanol, uniformly stirring, adding 1g of ammonia water to adjust the pH value of the solution, adding 4g of polyvinylpyrrolidone and 2g of thiourea, placing the mixture in a reaction kettle, heating to 180 ℃, keeping the temperature for 12 hours, and cooling to room temperature after the reaction is finished to obtain a laser absorbing material mixture A with the mass fraction of the carbon nano tube loaded with tungsten oxysulfide of about 4%;
(2) Weighing 2g of light-cured resin 7600B, 4g of active monomer PETA, 40g of ethanol, 0.8g of deep photoinitiator TPO, 0.8g of photoinitiator 184 and 0.2g of flatting agent BYK333, and uniformly stirring to obtain a mixture B;
(3) Slowly adding the mixture B into the mixture A, and uniformly stirring to obtain the laser-proof coating;
comparative example 3
The preparation method of the laser-proof coating comprises the following steps:
(1) Weighing 2.0g of molybdenum pentachloride raw material, dissolving the raw material in 50g of ethanol, uniformly stirring, adding 1g of ammonia water to adjust the pH value of the solution, adding 4g of polyvinylpyrrolidone and 2g of thiourea, placing the mixture into a reaction kettle, heating to 180 ℃, keeping the temperature for 12 hours, and cooling to room temperature after the reaction is finished to obtain a laser absorbing material mixture A with the mass fraction of molybdenum oxysulfide being about 4%;
(2) Weighing 2g of photocuring resin 7600B, 4g of active monomer PETA, 40g of ethanol, 0.8g of deep layer photoinitiator TPO, 0.8g of photoinitiator 184 and 0.2g of flatting agent BYK333, and uniformly stirring to obtain a mixture B;
(3) Slowly adding the mixture B into the mixture A, and uniformly stirring to obtain the laser-proof coating.
Comparative example 4
Compared with example 5, only the laser-proof paint prepared in example 1 was replaced with the laser-proof paint prepared in comparative example 1, and the rest steps were completely consistent.
Comparative example 5
Compared with example 5, only the laser-proof paint prepared in example 1 is replaced by the laser-proof paint prepared in comparative example 2, and the rest steps are completely consistent.
Comparative example 6
Compared with example 5, only the laser-proof paint prepared in example 1 was replaced with the laser-proof paint prepared in comparative example 3, and the remaining steps were completely consistent.
Detecting content
(1) Optical density: testing according to related specifications in a GJB 2408-95 laser protection glasses protection performance test method, wherein the test results are shown in Table 1;
(2) Surface resistance: testing according to relevant specifications in 'general specification for antistatic detection of electronic product manufacturing and application systems' SJ/T10694-2006, wherein the detection results are shown in a table 1;
(3) Light transmittance: the test is carried out according to the relevant specifications in GB/T2410-2008 'determination of transparent plastic light transmittance and haze', and the detection results are shown in Table 1;
(4) Surface hardness: the test is carried out according to the relevant specifications in GB/T6739-2006 paint film hardness determination by a color paint and varnish pencil method, and the test results are shown in Table 1;
table 1: tables of data for testing PMMA plates of examples 5 to 8 and comparative examples 4 to 6
As can be seen from Table 1, examples 5 to 8 produced PMMA plates having antistatic, abrasion resistant and laser protective functions (optical density 4-6 +). Example 6 using more 2-functional monomer resulted in lower hardness and wear resistance, and example 7 increased the amount of molybdenum oxysulfide and tungsten oxysulfide, which decreased the light transmittance to 12%, but increased the optical density to 6.2, indicating a significant increase in laser protection. Example 8 the light transmittance increased to 45% with reduced amounts of molybdenum oxysulfide and tungsten oxysulfide, but the optical density also decreased from 5.1 to 4.1.
In comparison with example 5, comparative example 4, in which the molybdenum oxysulfide and tungsten oxysulfide nanomaterials are not supported by using carbon nanotubes, has an optical density significantly lower than that of example 5, and thus it can be seen that the carbon nanotubes form a significant synergistic effect with the molybdenum oxysulfide and tungsten oxysulfide nanomaterials, and in addition, comparative example 4 has a surface resistance > 10 12 Omega, no antistatic effect. In comparative examples 5 and 6, only one of tungsten oxysulfide and molybdenum oxysulfide nano materials is used, and the laser protection performance is obviously reduced.
The embodiments of the present invention have been described in detail, but the description is only for the preferred embodiments of the present invention and should not be construed as limiting the scope of the present invention. All equivalent changes and modifications made within the scope of the present invention shall fall within the scope of the present invention.
Claims (10)
1. The laser-proof coating is characterized by comprising the following raw materials in parts by weight:
1-10 parts of light-cured resin, 2-10 parts of active monomer, 0.1-1 part of photoinitiator, 80-100 parts of diluent, 0.5-4 parts of additive and 0.3-5 parts of auxiliary agent.
2. The laser-proof paint according to claim 1, wherein the photocurable resin is one of photocurable resin 6106, photocurable resin 7600B and photocurable resin 7605B.
3. The laser-proof paint as claimed in claim 1, wherein the reactive monomer is one or more selected from the group consisting of tripropylene glycol diacrylate, dipentaerythritol hexaacrylate, hexanediol diacrylate, diethylene glycol diacrylate phthalate, neopentyl glycol diacrylate, pentaerythritol triacrylate, trimethylolpropane triacrylate, and isoborneol acrylate, which are mixed in an arbitrary ratio.
4. The laser-proof paint according to claim 1, wherein the preparation method of the additive comprises the following steps:
dissolving molybdenum pentachloride and tungsten hexachloride in carbon nano tube ethanol dispersion liquid, uniformly stirring, adding ammonia water to adjust the pH value of the solution, adding polyvinylpyrrolidone and thiourea, heating to 180 ℃, and keeping the temperature for 12 hours to obtain the additive.
5. The laser-resistant coating of claim 4, wherein the molybdenum pentachloride: tungsten hexachloride: carbon nanotube dispersion liquid: polyvinylpyrrolidone: the mass ratio of the thiourea is 0.5-30:0.1-1:20-50:3-8:1-4.
6. The laser-proof paint according to claim 4, wherein the carbon nanotube ethanol dispersion is prepared by mixing a polymer dispersant, carbon nanotubes and ethanol.
7. The laser-proof paint as claimed in claim 1, wherein the diluent is one or more of methanol, ethanol, n-propanol and butanol mixed in any ratio.
8. The laser-proof coating as claimed in claim 1, wherein the diluent is obtained by mixing an alcohol ether diluent and an alcohol diluent, the alcohol ether diluent is obtained by mixing one or more of ethylene glycol ethyl ether, ethylene glycol butyl ether and diethylene glycol ethyl ether in any ratio, and the alcohol diluent is obtained by mixing one or more of methanol, ethanol, n-propanol and butanol in any ratio.
9. The preparation method of the laser-proof coating is characterized by comprising the following preparation steps:
(1) Stirring and mixing the light-cured resin, the active monomer, the diluent, the photoinitiator and the auxiliary agent to obtain a mixture A;
(2) And uniformly stirring the mixture A and the additive to obtain the laser-proof coating.
10. A laser protection article made of a laser protection coating according to any one of claims 1 to 8, wherein the surface of the article is coated with a laser protection coating.
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