阅读说明：本技术 一种耐高温环氧改性丙烯酸树脂及其制备方法 (High-temperature-resistant epoxy modified acrylic resin and preparation method thereof ) 是由 殷鹏刚 于 2021-08-04 设计创作，主要内容包括：本发明专利涉及树脂技术领域,尤其为一种耐高温环氧改性丙烯酸树脂,由下列重量份的原料配制而成：丙烯酸(AA)10-20份、丙烯酸羟丙酯(HPA)20-25份、甲基丙烯酸甲酯(MMA)20-25份、丙烯酸丁酯(BA)20-25份、丙烯酸异辛酯(EHA)15-25份、过氧化苯甲酰(BPO)4～5份、正丁醇40～50份、乙酸丁酯4～5份、环已酮2～3份、丁酮40～50份、环氧树脂25～40份、纳米SiO-(2)1～2份；本发明专利将纳米SiO2与环氧丙烯酸树脂反应,不仅具有更好的防水性、耐候性、硬度、耐盐水腐蚀的性能,还降低了环氧丙烯酸树脂的玻璃化转变温度,且直接将有机、无机化合物同时置于同一体系进行反应,使得制备过程较传统纳米复合材料的工艺简单,缩短了生产周期。(The invention relates to the technical field of resin, in particular to high-temperature-resistant epoxy modified acrylic resin which is prepared from the following raw materials in parts by weight: 10-20 parts of Acrylic Acid (AA), 20-25 parts of hydroxypropyl acrylate (HPA), 20-25 parts of Methyl Methacrylate (MMA), 20-25 parts of Butyl Acrylate (BA), 15-25 parts of isooctyl acrylate (EHA), 4-5 parts of Benzoyl Peroxide (BPO), 40-50 parts of n-butyl alcohol, 4-5 parts of butyl acetate, 2-3 parts of cyclohexanone, 40-50 parts of butanone, 25-40 parts of epoxy resin, and nano SiO 2 1-2 parts; the invention makes the nano SiO2 react with the epoxy acrylic resin, not only has better performances of water resistance, weather resistance, hardness and salt water corrosion resistance, but also reduces the glass transition temperature of the epoxy acrylic resin, and directly places organic and inorganic compounds in the same system at the same timeThe reaction is carried out, so that the preparation process is simpler than the process of the traditional nano composite material, and the production period is shortened.)

1. A high-temperature-resistant epoxy modified acrylic resin is characterized in that: the paint is prepared from the following raw materials in parts by weight: 10-20 parts of Acrylic Acid (AA), 20-25 parts of hydroxypropyl acrylate (HPA), 20-25 parts of Methyl Methacrylate (MMA), 20-25 parts of Butyl Acrylate (BA), 15-25 parts of isooctyl acrylate (EHA), 4-5 parts of Benzoyl Peroxide (BPO), 40-50 parts of n-butyl alcohol, 4-5 parts of butyl acetate, 2-3 parts of cyclohexanone, 40-50 parts of butanone, 25-40 parts of epoxy resin, and nano SiO₂1-2 parts of curing agent and 1-2 parts of curing agent.

2. The high temperature resistant epoxy modified acrylic resin as claimed in claim 1, wherein: the butanone is analytically pure and is a product produced by the national medicine group.

3. The high temperature resistant epoxy modified acrylic resin as claimed in claim 1, wherein: the epoxy resin is of industrial grade.

4. The high temperature resistant epoxy modified acrylic resin as claimed in claim 1, wherein: the nano SiO₂Is a product produced by chemical industry in the four seas in Hubei province; the curing agent is IPDI trimer.

5. The high temperature resistant epoxy modified acrylic resin as claimed in claim 1, wherein: the Methyl Methacrylate (MMA) is a hard monomer, the Butyl Acrylate (BA) is a soft monomer, and the dosage ratio of the hard monomer to the soft monomer is 1: 1.

6. the high temperature resistant epoxy modified acrylic resin as claimed in claim 1, wherein: the dosage of the acrylic acid is 6-15% of the total amount of the soft and hard monomers, and the type of the epoxy resin is epoxy resin E-03.

7. A preparation method of high-temperature-resistant epoxy modified acrylic resin is characterized by comprising the following steps: the method comprises the following steps:

step 1: preparing materials: the following materials were prepared: 10-20 parts of Acrylic Acid (AA), 20-25 parts of hydroxypropyl acrylate (HPA), 20-25 parts of Methyl Methacrylate (MMA), 20-25 parts of Butyl Acrylate (BA), 15-25 parts of isooctyl acrylate (EHA), 4-5 parts of Benzoyl Peroxide (BPO), 40-50 parts of n-butyl alcohol, 4-5 parts of butyl acetate, 2-3 parts of cyclohexanone, 40-50 parts of butanone, 25-40 parts of epoxy resin, and nano SiO₂1-2 parts of curing agent and 1-2 parts of curing agent;

step 2: pouring into a reaction kettle: 10-20 parts of Acrylic Acid (AA), 20-25 parts of hydroxypropyl acrylate (HPA), 20-25 parts of Methyl Methacrylate (MMA), 20-25 parts of Butyl Acrylate (BA), 15-25 parts of isooctyl acrylate (EHA), 4-5 parts of Benzoyl Peroxide (BPO) and 40-50 parts of n-butyl alcohol are prepared and uniformly mixed for later use according to the proportion, then the prepared initiator and monomer mixed solution are taken out, one third of the initiator and monomer mixed solution is taken out and poured into a reaction kettle, and the reaction kettle is started for reaction;

and step 3: adding materials: starting the reaction kettle, heating the reaction kettle to 108 ℃ for reflux, heating and dissolving the initiator and the monomer mixed solution, stirring to fully mix the initiator and the monomer mixed solution, sticking the mixed solution of various raw materials for one hour, and then adding the nano SiO₂Mixing the dispersion liquid, the residual monomers and the initiator to form a mixed solution, and slowly dripping the mixed solution into the reaction kettle for two hours;

and 4, step 4: preparing resin: the reaction kettle begins to cool and mix, the temperature is reduced to about 100 ℃, then the heat preservation reaction is carried out for two hours, when the mixed liquid in the reaction kettle is cooled to 50 ℃, the epoxy resin mixed liquid is added into the reaction kettle, the reaction and the mixing are continued for half an hour, then the temperature is reduced, butyl acetate is added to dilute and mix the reaction, so that the light yellow transparent high temperature resistant epoxy modified acrylic resin is prepared, and finally the curing agent is poured into the high temperature resistant epoxy modified acrylic resin and is used after the mixing.

8. The preparation method of the high temperature resistant epoxy modified acrylic resin as claimed in claim 7, wherein the preparation method comprises the following steps: in the step 2, the initiator is one of benzoyl peroxide, potassium persulfate and ammonium persulfate, and the dosage of the initiator is 1.5-2.0% of the total amount of the soft and hard monomers.

9. The preparation method of the high temperature resistant epoxy modified acrylic resin as claimed in claim 7, wherein the preparation method comprises the following steps: in the step 3, the nano SiO₂The dispersion comprises SiO₂And cyclohexanone, reacting SiO₂Adding cyclohexanone to prepare dispersion liquid.

10. The preparation method of the high temperature resistant epoxy modified acrylic resin as claimed in claim 7, wherein the preparation method comprises the following steps: in the step 4, the epoxy resin mixed solution includes epoxy resin and butanone, and the epoxy resin is diluted with butanone in advance.

Technical Field

The invention relates to the technical field of resin, in particular to high-temperature-resistant epoxy modified acrylic resin and a preparation method thereof.

Background

The acrylic resin is a general name 1 of homopolymerization and copolymer of acrylic acid, methacrylic acid and esters or derivatives thereof, has low toxicity, light color, good film forming property and yellowing resistance, and the molecular structure of the epoxy resin contains active groups such as epoxy groups, hydroxyl groups, ether bonds and the like, has good adhesive force to a base material after crosslinking, has high film forming hardness and good sealing property, and is easy to process and form. However, the existing epoxy modified acrylic resin has limited performances such as waterproofness, weather resistance, hardness, salt water corrosion resistance and the like, high glass transition temperature, complex preparation process and long production period, and therefore, the high-temperature-resistant epoxy modified acrylic resin and the preparation method thereof are provided for solving the problems.

SUMMARY OF THE PATENT FOR INVENTION

The invention aims to provide a high-temperature-resistant epoxy modified acrylic resin and a preparation method thereof, and solves the problems of limited water resistance, weather resistance, hardness, salt water corrosion resistance and other properties, high glass transition temperature, complex preparation process and long production period of the conventional epoxy modified acrylic resin.

In order to achieve the purpose, the invention provides the following technical scheme: a high-temperature-resistant epoxy modified acrylic resin is prepared from the following raw materials in parts by weight: 10-20 parts of Acrylic Acid (AA), 20-25 parts of hydroxypropyl acrylate (HPA), 20-25 parts of Methyl Methacrylate (MMA), 20-25 parts of Butyl Acrylate (BA), 15-25 parts of isooctyl acrylate (EHA), 4-5 parts of Benzoyl Peroxide (BPO), 40-50 parts of n-butyl alcohol, 4-5 parts of butyl acetate, 2-3 parts of cyclohexanone, 40-50 parts of butanone, 25-40 parts of epoxy resin, and nano SiO₂1-2 parts of curing agent and 1-2 parts of curing agent.

Preferably, the butanone is analytically pure and is a product produced by the national medicine group.

Preferably, the epoxy resin is of industrial grade.

Preferably, the nano SiO₂Is a product produced by chemical industry in the four seas in Hubei province; the curing agent is IPDI trimer.

Preferably, the Methyl Methacrylate (MMA) is a hard monomer, and the Butyl Acrylate (BA) is a soft monomer, wherein the ratio of the hard monomer to the soft monomer is 1: 1.

preferably, the dosage of the acrylic acid is 6-15% of the total amount of the soft and hard monomers, and the type of the epoxy resin is epoxy resin E-03.

A preparation method of high-temperature-resistant epoxy modified acrylic resin comprises the following steps:

step 1: preparing materials: the following materials were prepared: 10-20 parts of Acrylic Acid (AA), 20-25 parts of hydroxypropyl acrylate (HPA), 20-25 parts of Methyl Methacrylate (MMA), 20-25 parts of Butyl Acrylate (BA), 15-25 parts of isooctyl acrylate (EHA), 4-5 parts of Benzoyl Peroxide (BPO), 40-50 parts of n-butyl alcohol, 4-5 parts of butyl acetate, 2-3 parts of cyclohexanone, 40-50 parts of butanone, 25-40 parts of epoxy resin, and nano SiO₂1-2 parts of curing agent and 1-2 parts of curing agent;

step 2: pouring into a reaction kettle: 10-20 parts of Acrylic Acid (AA), 20-25 parts of hydroxypropyl acrylate (HPA), 20-25 parts of Methyl Methacrylate (MMA), 20-25 parts of Butyl Acrylate (BA), 15-25 parts of isooctyl acrylate (EHA), 4-5 parts of Benzoyl Peroxide (BPO) and 40-50 parts of n-butyl alcohol are prepared and uniformly mixed for later use according to the proportion, then the prepared initiator and monomer mixed solution are taken out, one third of the initiator and monomer mixed solution is taken out and poured into a reaction kettle, and the reaction kettle is started for reaction;

and step 3: adding materials: starting the reaction kettle, heating the reaction kettle to 108 ℃ for reflux, heating and dissolving the initiator and the monomer mixed solution, stirring to fully mix the initiator and the monomer mixed solution, sticking the mixed solution of various raw materials for one hour, and then adding the nano SiO₂Mixing the dispersion liquid, the residual monomers and the initiator to form a mixed solution, and slowly dripping the mixed solution into the reaction kettle for two hours;

and 4, step 4: preparing resin: the reaction kettle begins to cool and mix, the temperature is reduced to about 100 ℃, then the heat preservation reaction is carried out for two hours, when the mixed liquid in the reaction kettle is cooled to 50 ℃, the epoxy resin mixed liquid is added into the reaction kettle, the reaction and the mixing are continued for half an hour, then the temperature is reduced, butyl acetate is added to dilute and mix the reaction, so that the light yellow transparent high temperature resistant epoxy modified acrylic resin is prepared, and finally the curing agent is poured into the high temperature resistant epoxy modified acrylic resin and is used after the mixing.

Preferably, in step 2, the initiator is one of benzoyl peroxide, potassium persulfate and ammonium persulfate, and the amount of the initiator is 1.5-2.0% of the total amount of the soft and hard monomers.

Preferably, theIn step 3, nano SiO₂The dispersion comprises SiO₂And cyclohexanone, reacting SiO₂Adding cyclohexanone to prepare dispersion liquid.

Preferably, in step 4, the epoxy resin mixed solution includes epoxy resin and butanone, and the epoxy resin is diluted with butanone in advance.

Compared with the prior art, the invention has the following beneficial effects:

the invention discloses nano SiO₂The epoxy acrylic resin modified by the nano silicon oxide takes epoxy acrylate macromolecules as a main chain and takes hydroxyl or unsaturated residual bonds on a side chain, and experimental results show that the epoxy acrylic resin modified by the nano silicon oxide takes the epoxy acrylate macromolecules as a modified material of a main film forming material, has better performances of water resistance, weather resistance, hardness and salt water corrosion resistance, reduces the glass transition temperature of the epoxy acrylic resin, and directly places organic and inorganic compounds in the same system for reaction at the same time, so that the preparation process is simpler than that of the traditional nano composite material, and the production period is shortened.

Drawings

FIG. 1 is a schematic view of the present invention.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings 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, not all of the embodiments. All other embodiments obtained by a person skilled in the art based on the embodiments in the patent of the invention without any inventive work belong to the protection scope of the patent of the invention.

Referring to fig. 1, a high temperature resistant epoxy modified acrylic resin is prepared from the following raw materials in parts by weight: 10-20 parts of Acrylic Acid (AA), 20-25 parts of hydroxypropyl acrylate (HPA), 20-25 parts of Methyl Methacrylate (MMA), 20-25 parts of Butyl Acrylate (BA), 15-25 parts of isooctyl acrylate (EHA), 4-5 parts of Benzoyl Peroxide (BPO), 40-50 parts of n-butyl alcohol, 4-5 parts of butyl acetate, 2-3 parts of cyclohexanone, and butyl40-50 parts of ketone, 25-40 parts of epoxy resin and nano SiO₂1-2 parts of curing agent and 1-2 parts of nano SiO₂The epoxy acrylic resin modified by the nano silicon oxide takes epoxy acrylate macromolecules as a main chain and takes hydroxyl or unsaturated residual bonds on a side chain, and experimental results show that the epoxy acrylic resin modified by the nano silicon oxide takes the epoxy acrylate macromolecules as a modified material of a main film forming material, has better performances of water resistance, weather resistance, hardness and salt water corrosion resistance, reduces the glass transition temperature of the epoxy acrylic resin, and directly places organic and inorganic compounds in the same system for reaction at the same time, so that the preparation process is simpler than that of the traditional nano composite material, and the production period is shortened.

In the embodiment, the butanone is analytically pure, is a product produced by the national medicine group, and provides preparation for subsequent processing.

In this embodiment, the epoxy resin is of an industrial grade, which facilitates subsequent processing.

In this example, nano SiO₂Is a product produced by chemical industry in the four seas in Hubei province; the curing agent is IPDI tripolymer, and is convenient to cure.

In this example, Methyl Methacrylate (MMA) was used as the hard monomer, and Butyl Acrylate (BA) was used as the soft monomer, wherein the ratio of the hard monomer to the soft monomer was 1: 1, preparing for subsequent processing.

In the embodiment, the amount of the acrylic acid is 6-15% of the total amount of the soft and hard monomers, and the type of the epoxy resin is epoxy resin E-03, so that the processing is convenient.

A preparation method of high-temperature-resistant epoxy modified acrylic resin comprises the following steps:

step 1: preparing materials: the following materials were prepared: 10-20 parts of Acrylic Acid (AA), 20-25 parts of hydroxypropyl acrylate (HPA), 20-25 parts of Methyl Methacrylate (MMA), 20-25 parts of Butyl Acrylate (BA), 15-25 parts of isooctyl acrylate (EHA), 4-5 parts of Benzoyl Peroxide (BPO), 40-50 parts of n-butyl alcohol, 4-5 parts of butyl acetate, 2-3 parts of cyclohexanone, 40-50 parts of butanone, 25-40 parts of epoxy resin, and nano SiO₂1-2 parts of curing agent and 1-2 parts of curing agent;

step 2: pouring into a reaction kettle: 10-20 parts of Acrylic Acid (AA), 20-25 parts of hydroxypropyl acrylate (HPA), 20-25 parts of Methyl Methacrylate (MMA), 20-25 parts of Butyl Acrylate (BA), 15-25 parts of isooctyl acrylate (EHA), 4-5 parts of Benzoyl Peroxide (BPO) and 40-50 parts of n-butyl alcohol are prepared and uniformly mixed for later use according to the proportion, then the prepared initiator and monomer mixed solution are taken out, one third of the initiator and monomer mixed solution is taken out and poured into a reaction kettle, and the reaction kettle is started for reaction;

and step 3: adding materials: starting the reaction kettle, heating the reaction kettle to 108 ℃ for reflux, heating and dissolving the initiator and the monomer mixed solution, stirring to fully mix the initiator and the monomer mixed solution, sticking the mixed solution of various raw materials for one hour, and then adding the nano SiO₂Mixing the dispersion liquid, the residual monomers and the initiator to form a mixed solution, and slowly dripping the mixed solution into the reaction kettle for two hours;

and 4, step 4: preparing resin: the reaction kettle begins to cool and mix, the temperature is reduced to about 100 ℃, then the heat preservation reaction is carried out for two hours, when the mixed liquid in the reaction kettle is cooled to 50 ℃, the epoxy resin mixed liquid is added into the reaction kettle, the reaction and the mixing are continued for half an hour, then the temperature is reduced, butyl acetate is added to dilute and mix the reaction, so that the light yellow transparent high temperature resistant epoxy modified acrylic resin is prepared, and finally the curing agent is poured into the high temperature resistant epoxy modified acrylic resin and is used after the mixing.

In this embodiment, in step 2, the initiator is one of benzoyl peroxide, potassium persulfate, and ammonium persulfate, and the amount of the initiator is 1.5% to 2.0% of the total amount of the soft and hard monomers, so as to facilitate the reaction of the mixed solution.

In this embodiment, in step 3, nano SiO₂The dispersion comprises SiO₂And cyclohexanone, reacting SiO₂Adding cyclohexanone to prepare dispersion liquid, so that the silicon dioxide is conveniently blended into the mixed liquid.

In this embodiment, in step 4, the epoxy resin mixed solution includes epoxy resin and butanone, and the epoxy resin is diluted with butanone in advance.

Although embodiments of the present patent have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the present patent, the scope of which is defined in the appended claims and their equivalents.