CN111286268A - Toughening and hardening coating composition, preparation method and plastic treatment method - Google Patents

Toughening and hardening coating composition, preparation method and plastic treatment method Download PDF

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CN111286268A
CN111286268A CN202010221178.4A CN202010221178A CN111286268A CN 111286268 A CN111286268 A CN 111286268A CN 202010221178 A CN202010221178 A CN 202010221178A CN 111286268 A CN111286268 A CN 111286268A
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郭芳敏
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郭芳敏
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Abstract

The invention belongs to the technical field of coatings, and particularly relates to a toughening and hardening coating composition, a preparation method and a plastic treatment method, wherein the composition comprises, by weight, 30-50 parts of alkoxysilane hydrolysate, 10-20 parts of titanate hydrolysate, 7-12 parts of alkoxy modified silicone oil, 0.3-1.0 part of a curing agent, 0.1-0.4 part of a curing accelerator and 20-50 parts of absolute ethyl alcohol. After being degreased, cleaned and dried, the plastic to be treated is immersed in the wear-resistant hardened coating composition, lifted, aired and heated, so that a coating with higher hardness, better toughness and good adhesive force can be obtained on the surface of the plastic, and the purpose of protecting the surface of the plastic is achieved.

Description

Toughening and hardening coating composition, preparation method and plastic treatment method
Technical Field
The invention belongs to the technical field of coatings, and particularly relates to a toughening and hardening coating composition, a preparation method and a plastic treatment method.
Background
Optical plastic refers to plastic used as an optical medium material, and is mainly used in optical instruments with large batches for manufacturing optical substrates, lenses, contact lenses and the like. Polycarbonate is an important optical plastic, is called polycarbonate for short PC, is a thermoplastic resin with a molecular main chain containing a carbonate bond structure, has the advantages of high transparency, good impact resistance, heat resistance, cold resistance, stable size, high light transmittance and the like, and becomes an important optical material. However, PC materials have a low surface hardness (pencil hardness, 1kg force, 6B), poor abrasion resistance, and are prone to abrasion. Therefore, in the field of optical applications, it is necessary to apply a surface hardening treatment to increase the hardness and abrasion resistance, and the most common method is to apply an abrasion resistant hard coating layer, most of which is an abrasion resistant hard coating layer of a silicone system.
Publication No. CN1752165A discloses an organosilicon transparent wear-resistant hardening coating and a preparation method thereof, wherein a mixture consisting of tetraalkoxysilane, trialkoxysilane and dialkoxysilane is acidified and hydrolyzed, then a coupling agent is added, and a curing agent and a curing accelerator are added after curing, so that a transparent coating with the hardness of more than 3H can be obtained on the surface of PC.
Publication No. CN1834180A discloses an organosilicon abrasion-resistant transparent coating for optical plastic surface enhancement, which comprises a volume ratio of 83.3-86.7%: 13.3 to 16.7 percent of A, B, wherein the component A contains 25 to 31 percent of organic silicon monomer, 0.2 to 1 percent of flatting agent and 68 to 74.6 percent of solvent by volume ratio; the component B comprises, by weight, 6.2-9.9% of concentrated hydrochloric acid, 89.7-93.1% of water and 0.4-1.1% of a curing agent. The organic silicon monomer consists of ethyl orthosilicate, methyltrimethoxysilane, gamma-glycidoxypropyltrimethoxysilane and gamma-methacryloxypropyltrimethoxysilane.
However, the hardness and adhesion of the coating in the prior art methods can meet the requirements, but toughness is often problematic.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a toughening and hardening coating composition.
It is another object of the present invention to provide a method for preparing a toughened, hardened coating composition.
The invention also aims to provide a plastic treatment method which is simple, convenient and quick, and the treated plastic surface obtains a coating with high hardness, good adhesion, transparency and good toughness.
The invention adopts the following technical scheme:
the toughening and hardening coating composition consists of alkoxy silane hydrolysate 30-50 weight portions, titanate hydrolysate 10-20 weight portions, alkoxy modified silicone oil 7-12 weight portions, curing agent 0.3-1.0 weight portion, curing promoter 0.1-0.4 weight portion and anhydrous alcohol 20-50 weight portions.
Preferably, the alkoxysilane hydrolysate is hydrolyzed from tetraalkoxysilane and trialkoxysilane or from tetraalkoxysilane, trialkoxysilane and dialkoxysilane in the presence of an acidic catalyst in water and an organic solvent. The film layer obtained by hydrolyzing the tetraalkoxysilane and the trialkoxysilane under the acidic condition after drying the hydrolysate has higher hardness but lower toughness; the dried film layer of the hydrolyzate obtained by hydrolyzing tetraalkoxysilane, trialkoxysilane and dialkoxysilane under acidic conditions will have a slightly lower hardness, but a somewhat better toughness. The tetraalkoxysilane may be selected from methyl orthosilicate or ethyl orthosilicate; the chemical general formula of the trialkoxysilane is R4Si(OM1)3Wherein R is4Can be independently selected from one of methyl, vinyl, n-propyl, 3,3, 3-trifluoropropyl, phenyl, n-octyl, n-hexyl, isobutyl, isooctyl, 3- (2, 3-epoxypropyl) propyl, 2- (3, 4-epoxycyclohexyl) ethyl, 3- (methacryloyloxy) propyl and 3-mercaptopropyl, M1May be independently selected from one of methyl, ethyl, isopropyl and acetyl; the chemical formula of the dialkoxysilane is R5MeSi(OM2)2Wherein R is5Can be independently selected from one of methyl, vinyl, n-propyl, 3,3, 3-trifluoropropyl, phenyl, n-octyl, n-hexyl, isobutyl, isooctyl, 3- (2, 3-epoxypropyl) propyl, 2- (3, 4-epoxycyclohexyl) ethyl, 3- (methacryloyloxy) propyl and 3-mercaptopropyl, M2Can be independently selected from one of methyl, ethyl, isopropyl and acetyl, and Me is methyl.
Preferably, the titanate is selected from at least one of methyl titanate, tetraethyl titanate, n-propyl titanate, tetraisopropyl titanate, tetra-n-butyl titanate, tetra-t-butyl titanate, diisopropyl di (acetylacetonate) titanate, diisopropyl di (triethanolamine) titanate, isopropyl triisostearate, isopropyltrioleate acyloxy titanate, isopropyltri (dioctylphosphonoyl) titanate and isopropyldioleate acyloxy (dioctylphosphonoyl) titanate.
Preferably, the chemical general formula of the alkoxy modified silicone oil is shown as a formula (1),
Figure BDA0002426109860000021
wherein R is1Independently selected from one of methyl, phenyl, ethyl, propyl, isobutyl, 3,3, 3-trifluoropropyl, 2- (3, 4-epoxycyclohexyl) ethyl and gamma- (2, 3-epoxypropoxy) propyl, R2Independently selected from-CH2CH2-,-CH2CH2SCH2-、-CH2CH2SCH2CH2-and-CH2CH2SCH2CH2CH2One of (A), (B), (C) and (C), R3At least one of methyl, ethyl, isopropyl and acetyl, a is more than or equal to 0 and less than or equal to 20, b is more than or equal to 50 and less than or equal to 200, and c is more than or equal to 5 and less than or equal to 25.
When R is2is-CH2CH2When the silane coupling agent is used, the silane coupling agent is obtained by performing hydrosilylation reaction on vinyl silicone oil and a corresponding hydrogen-containing silane coupling agent; when R is2is-CH2CH2SCH2-、-CH2CH2SCH2CH2-or-CH2CH2SCH2CH2CH2And when the coupling agent is-prepared, vinyl silicone oil and a corresponding mercaptosilane coupling agent are subjected to a mercapto-alkene click chemical reaction.
Preferably, the curing agent is at least one selected from the group consisting of tetramethylammonium hydroxide, tetrabutylammonium hydroxide, tetramethylammonium chloride, tetrabutylammonium chloride, tetramethylammonium acetate and tetrabutylammonium acetate.
Preferably, the curing accelerator is selected from at least one of acrylamide, caprolactam, N-dimethylformamide, and boron trifluoride.
According to the preparation method of the toughening and hardening coating composition of any embodiment, the raw materials are accurately weighed according to the formula, and the alkoxy silane hydrolysate, the titanate hydrolysate, the alkoxy modified silicone oil and the absolute ethyl alcohol are uniformly mixed and filtered to obtain a premix; and adding the curing agent and the curing accelerator into the premix before use, and uniformly stirring and mixing for later use.
A plastic treating method includes such steps as immersing the plastic to be treated in the composition, lifting, drying in air, and heating for drying.
Preferably, the plastic is an optical plastic selected from Polycarbonate (PC), Polystyrene (PS), styrene acrylonitrile copolymer (SAN), styrene methyl methacrylate copolymer (PS-PMMA), Polyamide (PA), poly 4-methyl-1-pentene or organic glass (PMMA).
The invention has the beneficial effects that:
(1) the toughening hardening coating composition has wide raw material sources and lower cost.
(2) The equipment used in the preparation method of the toughening and hardening coating composition is simpler, the whole process flow is basically consistent with that in the prior art, and the preparation method can be directly replaced into the prior art.
(3) The obtained coating has the characteristics of high hardness, good toughness, good adhesive force and transparency, the hardness (1 Kg force) reaches more than H, and the coating has the advantages of good toughness, high adhesive force, good water boiling resistance and high light transmittance.
Detailed Description
The technical solution of the present invention is further illustrated and described by the following detailed description.
Unless otherwise specified, the parts described in the embodiments in the following embodiments are all parts by weight.
The toughening hardening coating composition comprises the following raw material components:
(A) the alkoxy-modified silicone oil is selected from the following,
(A-1)R1is methyl, R2is-CH2CH2SCH2CH2CH2-,a=10.7,b=95.3,c=10.1;
(A-2)R1Is 2- (3, 4-epoxycyclohexyl) ethyl, R2is-CH2CH2-,a=12.6,b=105.5,c=16.3;
(A-3)R1Is gamma- (2, 3-epoxypropoxy) propyl, R2is-CH2CH2-,a=15.3,b=74.7,c=24.5;
(A-4)R1Is phenyl, R2is-CH2CH2SCH2CH2CH2-,a=5.8,b=133.8,c=19.7;
(B) The alkoxysilane hydrolyzate is selected from the group consisting of,
(B-1) hydrolysate of ethyl orthosilicate and 3- (2, 3-epoxypropyl) propyltrimethoxysilane in a molar ratio of 1: 3;
(B-2) hydrolysates of ethyl orthosilicate, methyltriethoxysilane and 3- (2, 3-epoxypropyl) propylmethyldiethoxysilane in a molar ratio of 1:1: 1.5;
(B-3) hydrolysates of ethyl orthosilicate, isobutyltriethoxysilane, and methylphenyldiethoxysilane in a molar ratio of 1:2: 2;
(C) the titanate ester hydrolysate is selected from the group consisting of,
(C-1) a hydrolysate of methyl titanate;
(C-2) a hydrolysate of tetraethyl titanate;
(D) the curing agent is selected from the group consisting of,
(D-1) tetramethylammonium hydroxide;
(D-2) tetramethylammonium acetate;
(E) the curing accelerator is selected from the group consisting of,
(E-1) boron trifluoride;
(E-2) caprolactam;
the formulations of the specific examples are shown in table 1.
TABLE 1
Figure BDA0002426109860000041
Figure BDA0002426109860000051
The preparation method of each embodiment and comparative example of the toughened and hardened coating composition comprises the following steps: accurately weighing each raw material component according to the formula of table 1, uniformly mixing the alkoxy silane hydrolysate, the titanate hydrolysate, the alkoxy modified silicone oil and the absolute ethyl alcohol, and filtering to obtain a premix; adding a curing agent and a curing accelerator into the premix before use, and uniformly stirring and mixing to obtain the toughening and hardening coating composition.
The plastic treatment method comprises the steps of soaking the to-be-treated plastic which is cleaned and dried after oil removal into the toughening and hardening coating composition obtained in each embodiment and comparative example for 10-25 seconds, lifting, airing, and heating and drying at the temperature of 100-120 ℃ for 2-3 hours.
Performance testing
Viscosity: the toughened, hardened coating compositions of each example and comparative example were left to stand at 25 ℃ for 24 hours and then tested for viscosity at 25 ℃ using a rotational viscometer. The results are shown in Table 2.
Film thickness: tested according to GB 1767-1979. The results are shown in Table 2.
Hardness: pencil hardness was tested according to GB/T6739-2006, 1Kg force. The results are shown in Table 2.
Adhesion force: tested according to GB/T9286-1998. The best is grade 0 and the worst is grade 5. The results are shown in Table 2.
Light transmittance: the test was carried out according to GB/T2410-2008 using an ultraviolet-spectrophotometer at 800nm wavelength. The results are shown in Table 2.
Boiling resistance: and (3) placing the sample plate coated with the film layer in deionized water at 80 ℃, soaking for 1h, taking out, airing, and observing the change of the film layer. The results are shown in Table 2.
Toughness: impact resistance was tested according to GB/T1732-1993 at 50cm, 1 Kg. The results are shown in Table 2.
TABLE 2
Figure BDA0002426109860000052
Figure BDA0002426109860000061
From the results in table 2, it is clear that the hardness of the film layer obtained from the plastic surface treated with the toughening and hardening coating composition of the present invention is H or more, and the film layer has good adhesion, good boiling resistance, high light transmittance, and high toughness.
The foregoing has shown and described the fundamental principles, major features and advantages of the invention. It should be understood by those skilled in the art that the present invention is not limited by the foregoing embodiments, which are merely preferred embodiments of the present invention, and the scope of the present invention should not be limited thereby, and that equivalent changes and modifications made within the scope of the present invention and the specification should be covered thereby. The scope of the invention is defined by the appended claims and equivalents thereof.

Claims (9)

1. A toughened and hardened coating composition is characterized in that: the adhesive comprises, by weight, 30-50 parts of alkoxysilane hydrolysate, 10-20 parts of titanate hydrolysate, 7-12 parts of alkoxy modified silicone oil, 0.3-1.0 part of curing agent, 0.1-0.4 part of curing accelerator and 20-50 parts of absolute ethyl alcohol.
2. The toughened, hardened coating composition of claim 1, wherein: the alkoxy silane hydrolysate is hydrolyzed by tetraalkoxysilane and trialkoxysilane or by tetraalkoxysilane, trialkoxysilane and dialkoxysilane in the presence of an acidic catalyst, water and an organic solvent.
3. The toughened, hardened coating composition of claim 1, wherein: the titanate is selected from at least one of methyl titanate, tetraethyl titanate, n-propyl titanate, tetraisopropyl titanate, tetra-n-butyl titanate, tetra-tert-butyl titanate, diisopropyl di (acetylacetonate) titanate, diisopropyl di (triethanolamine) titanate, isopropyl triisostearate, isopropyltrioleate acyloxy titanate, isopropyltri (dioctylphosphonoyl) titanate and isopropyldioleate acyloxy (dioctylphosphonoyl) titanate.
4. The toughened, hardened coating composition of claim 1, wherein: the chemical general formula of the alkoxy modified silicone oil is shown as a formula (1),
Figure FDA0002426109850000011
wherein R is1Independently selected from one of methyl, phenyl, ethyl, propyl, isobutyl, 3,3, 3-trifluoropropyl, 2- (3, 4-epoxycyclohexyl) ethyl and gamma- (2, 3-epoxypropoxy) propyl, R2Independently selected from-CH2CH2-,-CH2CH2SCH2-、-CH2CH2SCH2CH2-and-CH2CH2SCH2CH2CH2One of (A), (B), (C) and (C), R3At least one of methyl, ethyl, isopropyl and acetyl, a is more than or equal to 0 and less than or equal to 20, b is more than or equal to 50 and less than or equal to 200, and c is more than or equal to 5 and less than or equal to 25.
5. The toughened, hardened coating composition of claim 1, wherein: the curing agent is at least one selected from tetramethylammonium hydroxide, tetrabutylammonium hydroxide, tetramethylammonium chloride, tetrabutylammonium chloride, tetramethylammonium acetate and tetrabutylammonium acetate.
6. The toughened, hardened coating composition of claim 1, wherein: the curing accelerator is at least one selected from acrylamide, caprolactam, N-dimethylformamide and boron trifluoride.
7. A method for preparing the toughened and hardened coating composition as claimed in any one of claims 1 to 6, characterized in that: accurately weighing the raw materials according to a formula, uniformly mixing the alkoxysilane hydrolysate, the titanate hydrolysate, the alkoxy modified silicone oil and the absolute ethyl alcohol, and filtering to obtain a premix; and adding the curing agent and the curing accelerator into the premix before use, and uniformly stirring and mixing for later use.
8. A plastic processing method, characterized in that: degreasing, cleaning and drying the plastic to be treated, soaking the plastic in the toughening and hardening coating composition of any one of claims 1 to 6, lifting, airing, and heating and drying.
9. A plastic material processing method according to claim 8, characterized in that: the plastic is optical plastic and is selected from polycarbonate, polystyrene, styrene acrylonitrile copolymer, styrene methyl methacrylate copolymer, polyamide, poly-4-methyl-1-pentene or organic glass.
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