CN112680105A - Environment-friendly anticorrosive paint, hyperbranched epoxy resin and preparation method thereof - Google Patents
Environment-friendly anticorrosive paint, hyperbranched epoxy resin and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an environment-friendly anticorrosive paint, hyperbranched epoxy resin and a preparation method thereof, wherein the environment-friendly anticorrosive paint comprises a component A and a component B, and the component A comprises: 70-80 parts of hyperbranched epoxy resin, 20-30 parts of bisphenol A epoxy resin, 30-120 parts of pigment and filler and 1-5 parts of auxiliary agent, wherein the total weight of the hyperbranched epoxy resin and the bisphenol A epoxy resin is 100 parts by weight, and the component B comprises: 30-100 parts of compound amine curing agent and 1-5 parts of auxiliary agent, wherein the weight ratio of A, B components is (1-10) to 1; also discloses hyperbranched epoxy resin and a preparation method thereof. The environment-friendly anticorrosive coating can be cured at normal temperature, has excellent performances, can be applied to protective coatings in various fields, and also prepares hyperbranched epoxy resin with a special macromolecular structure, so that the environment-friendly anticorrosive coating has the advantages of the epoxy resin, improves the flexibility of the epoxy resin, and reduces the production cost.
Description
Technical Field
The invention relates to the technical field of environment-friendly coatings, and further relates to an environment-friendly anticorrosive coating, hyperbranched epoxy resin and a preparation method thereof.
Background
The environment-friendly anticorrosive paint is anticorrosive paint with toxic Volatile Organic Compound (VOC) content less than 100, and mainly comprises water-based paint and solvent-free paint in the market at present. However, the corrosion resistance of the water-based paint is generally different from that of the traditional solvent-based corrosion-resistant paint, so that the solvent-free paint is the first choice of the environment-friendly corrosion-resistant paint. Water tanks of watering lorries, drinking water storage tanks, water delivery pipelines, industrial sewage pools and the like in daily life all need environment-friendly anticorrosive paint systems, scientific experiments prove that the epoxy resin paint has the characteristics of no toxicity, water resistance, good leakage resistance and the like, and is an ideal anticorrosive paint for water-involved products.
The common epoxy resin is epoxy resin with a bisphenol A structure, and as an anti-corrosion material, the common epoxy resin not only has the characteristics of compactness, water resistance, good leakage resistance, high strength and the like, but also has the advantages of no toxicity, strong adhesive force, normal-temperature operation, simple and convenient construction and other good manufacturability, low cost and the like, but also has the defects of large internal stress after curing, brittleness, fatigue resistance, aging resistance, heat resistance, impact resistance, cracking resistance and the like. Research shows that the liquid polysulfide prepolymer and the epoxy resin react to generate the block copolymer under the condition of an amine catalyst, so that the block copolymer has the excellent performance of the epoxy resin, and can effectively improve the internal stress and the flexibility of an epoxy coating. For example, patent documents CN200610014497.8 and CN01109499.0, the former needs heating to cure, and the latter has general salt spray resistance and cold-hot alternation resistance, which brings certain limitations to production, processing and application.
Disclosure of Invention
Aiming at the problems, the invention researches and designs an environment-friendly anticorrosive coating, hyperbranched epoxy resin and a preparation method thereof to solve the defects of brittle quality, easy damage and limited production of the traditional epoxy resin environment-friendly anticorrosive material. The technical means adopted by the invention are as follows:
an environment-friendly anticorrosive paint comprises a component A and a component B,
the component A comprises: bisphenol A epoxy resin, hyperbranched epoxy resin, pigment, filler and auxiliary agent;
based on the total weight of the hyperbranched epoxy resin and the bisphenol A epoxy resin as 100 parts by weight,
the component B comprises: compound amine curing agent and assistant;
30-100 parts of compound amine curing agent;
1-5 parts of an auxiliary agent;
A. the weight ratio of the component B is (1-10) to 1.
Preferably, component a comprises:
based on the total weight of the hyperbranched epoxy resin and the bisphenol A epoxy resin as 100 parts by weight,
the component B comprises:
40-90 parts of compound amine curing agent;
1-4 parts of an auxiliary agent;
A. the weight ratio of the component B is (2-8) to 1.
Preferably, the bisphenol A type epoxy resin can be bisphenol A type epoxy resin in the prior art, and preferably one of YD-128 of national chemical industry (Kunshan) Co., Ltd, NPEL-128 of epoxy resin factory of south Asia electronic materials (Kunshan) Co., Ltd, and WSR618 of Nantong Xinchen synthetic materials Co., Ltd.
Preferably, the compound amine curing agent is prepared by mixing a modified aliphatic amine curing agent and a modified alicyclic amine curing agent. The modified aliphatic amine curing agent is preferably selected from one of R2251 and R2259 of Renzhe chemical engineering (Songzi) Limited, D3055 and D9040 of Shanghai Junjiang New Material marketing Limited, and JH-5988 and XH-454 of Shenzhen Jia Di Da New Material science and technology Limited. The modified alicyclic amine curing agent is preferably one selected from ANCAMINE1618 or ANCAMINE2143 of Yongchuang specialty Chemicals (Nanjing) Co.
Preferably, the environment-friendly anticorrosive paint selects pigments with anticorrosive function, such as iron oxide red, titanium dioxide, zinc phosphate, aluminum tripolyphosphate and the like, and fillers, such as functional pigment nano silica, precipitated barium sulfate, mica powder and the like, and can be selected and used in combination according to actual conditions.
The auxiliaries are conventional in the art, such as: one or a mixture of more of a defoaming agent, a flatting agent, a wetting dispersant, a rheological additive and a silane coupling agent. The defoaming agent can be one or more of Defom6800 and BYK-066N, BYK-054, the leveling agent can be one or more of BYK-322 and BYK-A530, the wetting dispersant can be one or more of BYK-P104S, BYK-354 and BYK-378, the rheological additive can be one or more of BYK410 and BENGEL828, and the silane coupling agent can be A187.
The preparation method of the hyperbranched epoxy resin comprises the step of carrying out graft synthesis on the epoxy resin and the amino polyether resin under the conditions of heating and the presence of a catalyst to prepare the hyperbranched epoxy resin.
Preferably, the epoxy resin is a bisphenol a type epoxy resin having the following structure:
wherein n is 1, 2 or 3;
the epoxy resin can adopt all epoxy resins which are in the prior art and meet the structure, and preferably one of bisphenol A epoxy resins 618, 6101 made in China.
Preferably, the aminopolyether resin comprises a difunctional and a trifunctional aminopolyether resin. The hyperbranched epoxy resin is synthesized by grafting epoxy resin and amino polyether resin with two functionality degrees and three functionality degrees after grafting the epoxy resin and the amino polyether resin with two functionality degrees and three functionality degrees in the presence of a catalyst.
The bifunctional aminopolyether resin is a polyether resin having the following structure:
wherein m is 10 to 1000;
the bifunctional aminopolyether resin of the present invention may be any aminopolyether resin according to the prior art, preferably one of D230, D400 and D1000 of Hounsfield, and EC301, EC302 and D1000 of Pasteur, all of which have the above-mentioned structure.
The trifunctional aminopolyether resin has the following structure:
in the formula m1Is 10 to 1000;
the trifunctional aminopolyether resin of the present invention may be any aminopolyether resin having the above structure, preferably one of U.S. Henschelman T403 and T3000, and Basff T403 and T3000 amino-containing aminopolyether resins.
Preferably, the catalyst is tert-butyl perbenzoate or isobutyl titanate and the heating temperature is 80-150 ℃.
Preferably, the preparation method of the hyperbranched epoxy resin comprises the steps of uniformly mixing the epoxy resin with the trifunctional amino polyether resin, adding a catalyst for reaction, wherein the reaction temperature is 80-120 ℃, and the reaction time is 4-6 hours; cooling to 40-45 ℃, adding the amino polyether resin with two functionalities, reacting at the temperature of 120-150 ℃ for 4-6 hours, cooling to 40-45 ℃, and discharging to obtain a low-viscosity solution, namely the hyperbranched epoxy resin.
Preferably, the molar ratio of the epoxy resin to the bifunctional and trifunctional aminopolyether resin is 6:3:1, and the sum of the amounts of the epoxy resin and the bifunctional and trifunctional aminopolyether resin accounts for 98-99.9 wt% of the total charge amount; the dosage of the catalyst is 0.1-2 wt% of the total feeding amount;
wherein, the total material charge is the total weight of the epoxy resin, the amino polyether resin with two functionality and three functionality and the catalyst.
The hyperbranched epoxy resin has the following structural formula:
in the above formula, R has the following structural formula:
in the above formula, R1The structural formula of (A) is as follows:
in the above formula, n is 1, 2 or 3, m is 10-1000, m1Is 10-1000.
The preparation method of the environment-friendly anticorrosive paint comprises the following steps:
1) uniformly stirring hyperbranched epoxy resin, bisphenol A epoxy resin, pigment and filler and an auxiliary agent according to a corresponding proportion relation, then grinding to 40-70 mu m by using a sand mill or a three-roll mill, filtering by using a filter screen, metering and packaging, and preparing to obtain a component A;
2) mixing the compound amine curing agent and the auxiliary agent according to the corresponding proportion relationship to prepare a component B;
3) the component A, B is mixed according to the weight ratio to prepare the environment-friendly anticorrosive paint.
The coating method of the obtained coating can be a brush coating or spraying process, the thickness of the coating is controlled to be 80-150 mu m, and the effect is good.
The environment-friendly anticorrosive paint prepared by the invention has the following excellent comprehensive properties:
flexibility (mm): 1(GB/T1731-1993 paint film flexibility assay);
adhesion (grade): 1(GB/T9286-1998 cut-and-break test of paint and varnish films);
impact strength (kg. cm): 50 (GB/T1732-1993) paint film impact resistance determination method;
water resistance (60. + -. 1 ℃ C.): 1a no wrinkling, no bubbles, no peeling of the paint film (GB/T9274-1988 determination of the resistance of the paint and varnish to liquid media);
saline tolerance (60 ± 1 ℃): 1a no wrinkling, no bubbles, no peeling of the paint film (GB/T9274-1988 determination of the resistance of the paint and varnish to liquid media);
and (3) mould resistance: grade 0 (GJB150.10A-2009 mold test);
salt spray resistance: no foaming, no shedding and no discoloration after 8000 hours (GB/T1771-2007 determination of neutral salt spray resistance of colored paint and varnish).
Compared with the prior art, the environment-friendly anticorrosive paint, the hyperbranched epoxy resin and the preparation method thereof have the beneficial effects that: the environment-friendly anticorrosive coating can be cured at normal temperature, has excellent performance, can be applied to protective coatings in the fields of water storage tanks of watering lorries, drinking water storage tanks, water delivery pipelines, industrial sewage pools and the like, and can also be applied to non-toxic coatings in the fields of oil and sewage tanks of various ships, drinking water tanks, military affairs and the like which need long-term corrosion prevention. The hyperbranched epoxy resin with a special macromolecular structure is formed by modifying the epoxy resin with the chemically grafted multifunctional polyether chain segment, so that the hyperbranched epoxy resin has the performances of convenience in construction, strong binding power and the like caused by the normal-temperature curing and high crosslinking of the epoxy resin, improves the flexibility of the epoxy resin, reduces the production cost, and can be used for preparing the environment-friendly anticorrosive paint with excellent performance.
Detailed Description
The starting materials used in the examples are all commercial products.
Example 1: preparation of hyperbranched epoxy resin
60 parts of YD-128 (national chemical industry) epoxy resin and 9.5 parts of D230 (Hensman) amino polyether resin are mixed according to the parts by weight, and 0.5 part of tert-butyl perbenzoate is added. Reacting at 80 ℃ for 5 hours, cooling to 40 ℃, adding 30 parts of T403 (Hensman) amino polyether resin, reacting at 120 ℃ for 6 hours, cooling to 40 ℃, discharging to obtain 100 parts of transparent homogeneous low-viscosity solution, namely the hyperbranched epoxy resin. The epoxy value is tested by an epoxy value determination method (GB/T1677-2008 plasticizer epoxy value determination method B), the molecular weight of the synthesized product is tested by a liquid chromatography method, and the molecular weight reaches a theoretical value, so that the corresponding hyperbranched epoxy resin target product is obtained by the synthesis reaction.
Example 2: preparation of hyperbranched epoxy resin
60 parts by weight of NPEL-128 (southern Asia electronic) epoxy resin and 9 parts by weight of EC302 (basf) aminopolyether resin were mixed, and 2 parts by weight of isobutyl titanate was added. Reacting at 90 ℃ for 5 hours, cooling to 40 ℃, adding 29 parts of T3000 (basf) amino polyether resin, reacting at 130 ℃ for 6 hours, cooling to 40 ℃, discharging to obtain 100 parts of transparent homogeneous low-viscosity solution, namely the hyperbranched epoxy resin. The epoxy value is tested by an epoxy value determination method (GB/T1677-2008 plasticizer epoxy value determination method B), the molecular weight of the synthesized product is tested by a liquid chromatography method, and the molecular weight reaches a theoretical value, so that the corresponding hyperbranched epoxy resin target product is obtained by the synthesis reaction.
Example 3: preparation of hyperbranched epoxy resin
60 parts by weight of WSR618 (Nantong star) epoxy resin and 9 parts by weight of D1000 (Hensman) aminopolyether resin are mixed, and 1.2 parts by weight of isobutyl titanate is added. Reacting for 5 hours at 110 ℃, cooling to 40 ℃, adding 29.8 parts of T3000 (basf) amino polyether resin, reacting for 6 hours at 150 ℃, cooling to 40 ℃, discharging to obtain 100 parts of transparent homogeneous low-viscosity solution, namely the hyperbranched epoxy resin. The epoxy value is tested by an epoxy value determination method (GB/T1677-2008 plasticizer epoxy value determination method B), the molecular weight of the synthesized product is tested by a liquid chromatography method, and the molecular weight reaches a theoretical value, so that the corresponding hyperbranched epoxy resin target product is obtained by the synthesis reaction.
Example 4: preparation of environment-friendly anticorrosive paint
Weighing 70 parts by weight of the hyperbranched epoxy resin prepared in the example 1 and 30 parts by weight of bisphenol A type epoxy resin (DOC YD-128), putting the mixture into a stainless steel tank, stirring the mixture by using a high-speed stirrer, adding 0.3 part by weight of a defoaming agent BYK066N, 0.5 part by weight of a leveling agent BYK322 and BYKA530, 0.5 part by weight of a wetting dispersant BYK-P104S, 0.5 part by weight of a rheological additive BYK410 and 0.2 part by weight of a silane coupling agent A187, uniformly stirring the mixture, adding 20 parts by weight of titanium dioxide, 10 parts by weight of zinc phosphate, 5 parts by weight of precipitated barium sulfate, 2 parts by weight of nano-silica and 3 parts by weight of mica powder, uniformly stirring the mixture, grinding the mixture by using a sand mill or a three-roll mill to a standard fineness, filtering and packaging the mixture to obtain a coating A.
30 parts by weight of an aliphatic modified amine curing agent R2251 (Ruiqi chemical industry), 10 parts by weight of D3055 (Shanghai Junjiang) and 30 parts by weight of ANCAMINE1618 (Yinhuang specialty Chemicals) are weighed, 0.5 part by weight of BYK410 serving as a rheological additive is added, and the mixture is uniformly stirred to form a component B of the coating.
When in use, A, B is prepared from two components according to the weight ratio of 2: 1, mixing and spraying to form a film.
Example 5: preparation of environment-friendly anticorrosive paint
75 parts by weight of the hyperbranched epoxy resin prepared in example 2 and 25 parts by weight of bisphenol A type epoxy resin (south Asia electronic NPEL-128) are weighed and put into a stainless steel tank to be stirred by a high-speed stirrer, 1.5 parts by weight of defoamer Defom6800, 0.8 part by weight of flatting agent BYK322, 0.7 part by weight of wetting dispersant BYK354 and 0.5 part by weight of rheological additive BYK410 are added, 0.5 part by weight of silane coupling agent A187 can be added, after stirring uniformly, 30 parts by weight of iron oxide red, 10 parts by weight of aluminum tripolyphosphate, 3 parts by weight of precipitated barium sulfate, 2 parts by weight of nano silica and 25 parts by weight of mica powder are added, stirring uniformly, then grinding to a standard fineness by a sand mill or a three-roll grinder is carried out, and the mixture is filtered and packaged into a coating A component.
8 parts by weight of aliphatic modified amine curing agent R2259 (Redgkin chemical), 8 parts by weight of JH-5988 (Jia Di Da) and 4 parts by weight of ANCAMINE1618 (YinA Special chemistry) are weighed, and 3 parts by weight of BYK410 serving as rheological additive are added and uniformly stirred to obtain a component B of the coating.
When in use, A, B is prepared from two components according to the weight ratio of 8: 1, mixing and spraying to form a film.
Example 6: preparation of environment-friendly anticorrosive paint
80 parts by weight of the hyperbranched epoxy resin prepared in example 3 and 20 parts by weight of bisphenol A type epoxy resin (Nantong star WSR618) are weighed and put into a stainless steel tank to be stirred by a high-speed stirrer, 0.5 part by weight of defoaming agent BYK054, 0.3 part by weight of leveling agent BYKA530, 0.8 part by weight of wetting dispersant BYK378 and 0.5 part by weight of rheological additive BYK410 are added, 0.2 part by weight of silane coupling agent A187 can be added into the mixture, 10 parts by weight of iron oxide red, 10 parts by weight of titanium dioxide, 10 parts by weight of zinc phosphate, 10 parts by weight of precipitated barium sulfate, 5 parts by weight of nano-silica and 25 parts by weight of mica powder are added into the mixture after uniform stirring, the mixture is uniformly stirred and then ground by a sand mill or a three-roll grinder to a standard fineness degree, and the mixture is filtered and packaged into a.
Weighing 15 parts by weight of aliphatic modified amine curing agent D9040 (Shanghai Junjiang), 10 parts by weight of XH-454 (Jia Di Da) and 15 parts by weight of ANCAMINE2143 (Yinhuang specialty Chemicals), adding 1 part by weight of BYK410 as a rheological additive, and uniformly stirring to obtain a component B of the coating.
When in use, A, B is prepared from two components according to the weight ratio of 4: 1, mixing and spraying to form a film.
Example 7: preparation of environment-friendly anticorrosive paint
75 parts by weight of the hyperbranched epoxy resin prepared in example 3 and 25 parts by weight of bisphenol A type epoxy resin (Nantong star WSR618) are weighed and put into a stainless steel tank to be stirred by a high-speed stirrer, 1.3 parts by weight of defoamer Defom6800, 0.7 part by weight of leveling agent BYKA530, 1 part by weight of wetting dispersant BYK354 and 0.4 part by weight of rheological additive BYK410 are added, 0.3 part by weight of silane coupling agent A187 can be added into the mixture, after the mixture is uniformly stirred, 20 parts by weight of titanium dioxide, 8 parts by weight of aluminum tripolyphosphate, 12 parts by weight of zinc phosphate, 5 parts by weight of precipitated barium sulfate, 5 parts by weight of nano-silica and 15 parts by weight of mica powder are added into the mixture to be uniformly stirred, and then the mixture is ground to a standard fineness by a sand mill or a three-roll mill and is filtered and packaged into a coating.
11 parts by weight of aliphatic modified amine curing agent (R2259 in Ruiqi chemical engineering), 11 parts by weight of XH-454 (Jia Di Da) and 5 parts by weight of ANCAMINE2143 (Yinhuang specialty chemical) are weighed, 1 part by weight of BYK410 serving as rheological additive is added, and the mixture is uniformly stirred to form a component B of the coating.
When in use, A, B is prepared from two components according to the weight ratio of 6: 1, mixing and spraying to form a film.
The performance indexes of the coating obtained by spraying the coating obtained in the embodiments 4 to 7 into a film can meet the following requirements:
flexibility (mm): 1;
adhesion (grade): 1;
impact strength (kg. cm): 50;
water resistance (60. + -. 1 ℃ C.): 1a, a paint film has no wrinkles, no bubbles and no shedding;
saline tolerance (60 ± 1 ℃): 1a, a paint film has no wrinkles, no bubbles and no shedding;
and (3) mould resistance: level 0;
salt spray resistance: no bubbling, no shedding and no discoloration within 8000 hours.
When the paint is constructed, firstly, the sprayed surface is treated to meet relevant requirements, A, B two components are uniformly mixed and then sprayed, and after the paint is cured for seven days at normal temperature, the protective coating applied to the fields of water storage tanks of watering lorries, drinking water storage tanks, water pipelines, industrial sewage pools and the like can be obtained, and the paint can also be applied to non-toxic coatings of various ship oil and sewage tanks, drinking water tanks, military affairs and other fields needing long-term corrosion resistance.
The above-mentioned embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solution of the present invention by those skilled in the art should fall within the protection scope defined by the claims of the present invention without departing from the spirit of the present invention.
Claims (10)
1. An environment-friendly anticorrosive paint is characterized in that: comprises a component A and a component B,
the component A comprises:
wherein the total weight of the hyperbranched epoxy resin and the bisphenol A epoxy resin is 100 parts by weight;
the component B comprises:
30-100 parts of compound amine curing agent;
1-5 parts of an auxiliary agent;
A. the weight ratio of the component B is (1-10) to 1.
2. The environment-friendly anticorrosive paint as claimed in claim 1, characterized in that:
the component A comprises:
wherein the total weight of the hyperbranched epoxy resin and the bisphenol A epoxy resin is 100 parts by weight;
the component B comprises:
40-90 parts of compound amine curing agent;
1-4 parts of an auxiliary agent;
A. the weight ratio of the component B is (2-8) to 1.
3. The environment-friendly anticorrosive paint according to claim 1 or 2, characterized in that: the compound amine curing agent comprises a modified aliphatic amine curing agent and a modified alicyclic amine curing agent.
4. A method for preparing the hyperbranched epoxy resin of any one of claims 1 to 3, wherein: heating epoxy resin and amino polyether resin in the presence of a catalyst for grafting synthesis to obtain the hyperbranched epoxy resin.
5. The method for preparing hyperbranched epoxy resin according to claim 4, wherein the method comprises the following steps: the epoxy resin is bisphenol A type epoxy resin.
6. The method for preparing hyperbranched epoxy resin according to claim 4, wherein the method comprises the following steps: the aminopolyether resins include difunctional and trifunctional aminopolyether resins.
7. The method for preparing hyperbranched epoxy resin according to claim 4, wherein the method comprises the following steps: the catalyst is tert-butyl perbenzoate or isobutyl titanate, and the heating temperature is 80-150 ℃.
8. The method for preparing hyperbranched epoxy resin according to claim 6, wherein the hyperbranched epoxy resin comprises: the method comprises the following steps: mixing epoxy resin with trifunctional amino polyether resin, adding a catalyst, reacting at 80-120 ℃ for 4-6 hours, cooling to 40-45 ℃ after reaction, adding bifunctional amino polyether resin, reacting at 120-150 ℃ for 4-6 hours, cooling to 40-45 ℃ and discharging to obtain the hyperbranched epoxy resin.
9. The method for preparing hyperbranched epoxy resin according to claim 8, wherein the hyperbranched epoxy resin comprises: the molar ratio of the epoxy resin to the bifunctional and trifunctional amino polyether resins is 6:3:1, the sum of the epoxy resin and the bifunctional and trifunctional amino polyether resins accounts for 98-99.9 wt% of the total charge, and the catalyst accounts for 0.1-2 wt% of the total charge;
wherein, the total material charge is the total weight of the epoxy resin, the amino polyether resin with two functionality and three functionality and the catalyst.
10. A hyperbranched epoxy resin according to any one of claims 1 to 9 wherein: the structural formula is as follows:
in the above formula, R has the following structural formula:
in the above formula, R1The structural formula of (A) is as follows:
in the above formula, n is 1, 2 or 3, m is 10-1000, m1Is 10-1000.
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| CN114774046A (en) * | 2022-04-28 | 2022-07-22 | 固德电材***（苏州）股份有限公司 | Normal-temperature curing adhesive and using method thereof |
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| CN115651483A (en) * | 2022-11-06 | 2023-01-31 | 中远关西涂料（上海）有限公司 | Solvent-free ultrahigh-solid epoxy paint for containers and preparation method thereof |
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