Synthetic method of epoxy modified thermoplastic acrylic resin

文档序号:61879 发布日期:2021-10-01 浏览:28次 中文

阅读说明:本技术 一种环氧改性热塑性丙烯酸树脂的合成方法 (Synthetic method of epoxy modified thermoplastic acrylic resin ) 是由 雷挺 邹长源 陈俊 于 2021-07-27 设计创作,主要内容包括:本发明公开了一种环氧改性热塑性丙烯酸树脂的合成方法,涉及环氧面漆技术领域。本发明包括以下步骤:Step1,选用环氧树脂E20与甲基丙烯酸,在90-105℃先开环反应,降酸值小于3以下;Step2,用PMA、BAC溶剂开稀为60%,得到A料;Step3,选用五氧化二磷与丙烯酸羟丙酯,先酯化反应,反应时长为10-15min;Step4,基于上述反应,得到一种磷酸酯的B料;Step5,按丙烯酸树脂工艺合成树脂,包括如下步骤:步骤一:用无苯溶剂PMA、BAC作垫底回流溶剂,MMA、BA、MAA设计出TG在80,固含45%的材料;步骤二:添加A料8%至10%,B料0.5-1%。本发明环氧改性热塑性丙烯酸树脂附着力达到国标1级,并且光泽度保持80以上,耐候性佳,具备优异的使用效果。(The invention discloses a synthetic method of epoxy modified thermoplastic acrylic resin, and relates to the technical field of epoxy finish paint. The invention comprises the following steps: step1, epoxy resin E20 and methacrylic acid are selected to perform ring opening reaction at 90-105 ℃, and the deacidification value is less than 3; step2, diluting with PMA and BAC solvent to 60% to obtain material A; step3, firstly, carrying out esterification reaction on phosphorus pentoxide and hydroxypropyl acrylate for 10-15 min; step4, obtaining a phosphate B material based on the reaction; step5, synthesizing resin according to an acrylic resin process, comprising the following steps: the method comprises the following steps: using benzene-free solvents PMA and BAC as bedding reflux solvents, and designing materials with TG of 80 percent and solid content of 45 percent by using MMA, BA and MAA; step two: adding 8 to 10 percent of material A and 0.5 to 1 percent of material B. The epoxy modified thermoplastic acrylic resin has the advantages that the adhesive force reaches the national standard level 1, the glossiness is kept above 80, the weather resistance is good, and the using effect is excellent.)

1. A synthetic method of epoxy modified thermoplastic acrylic resin is characterized in that: the method comprises the following steps:

step1, epoxy resin E20 and methacrylic acid are selected to perform ring opening reaction at 90-105 ℃, and the deacidification value is less than 3;

step2, diluting with PMA and BAC solvent to 60% to obtain material A;

step3, firstly, carrying out esterification reaction on phosphorus pentoxide and hydroxypropyl acrylate for 10-15 min;

step4, obtaining a phosphate B material based on the reaction;

step5, synthesizing resin according to an acrylic resin process, comprising the following steps:

the method comprises the following steps: using benzene-free solvents PMA and BAC as bedding reflux solvents, and designing TG at 80 and solid content of material C at 45% by using MMA, BA and MAA;

step two: adding 8 to 10 percent of material A, 0.5 to 1 percent of material B and a proper amount of azodiisobutyronitrile;

step three: carrying out polymerization reaction at 90-95 ℃;

step four: based on the reaction steps, the epoxy modified thermoplastic acrylic resin with the solid content of 50 percent, the acid value of less than 5 and the viscosity of between 15000 and 25000 is obtained.

And Step6, completing the synthesis of the epoxy modified thermoplastic acrylic resin.

2. The method for synthesizing the epoxy modified thermoplastic acrylic resin as claimed in claim 1, wherein the molar ratio of the epoxy resin E20 to the methacrylic acid in Step1 is 1: 0.98.

3. The method for synthesizing the epoxy modified thermoplastic acrylic resin as claimed in claim 1, wherein the molar ratio of the phosphorus pentoxide to the hydroxypropyl acrylate in Step3 is 1: 5.

4. The method for synthesizing epoxy modified thermoplastic acrylic resin as claimed in claim 1, wherein the esterification reaction temperature of phosphorus pentoxide and hydroxypropyl acrylate in Step3 is 90-105 ℃.

5. The method for synthesizing the epoxy modified thermoplastic acrylic resin as claimed in claim 1, wherein in Step three of Step5, the polymerization reaction time of the material A, the material B and the material C with the azobisisobutyronitrile is 6-8 h.

Technical Field

The invention relates to the technical field of epoxy finish paint, in particular to a synthetic method of epoxy modified thermoplastic acrylic resin for repairing and finishing epoxy floor paint.

Background

The epoxy floor paint is a very beautiful and long-lasting floor paint, adopts an integral polymer surface layer, is called as epoxy floor paint, mainly comprises epoxy resin and a curing agent, can be divided into 2 types of solvent type and solvent-free type, and can discharge a certain amount of Volatile Organic Compounds (VOC) in the production, construction and curing processes of the solvent type epoxy floor paint, but has lower cost; and solvent-free epoxy floor paint accords with the environmental protection theory, and epoxy floor paint is used for functional floor from beginning: such as corrosion resistance, wear resistance and skid resistance, is developed into a general common industrial terrace, and has the decorative effect besides the functional requirement. On the basis of wide application of industrial terraces, along with the continuous improvement of living standard of people, the industrial terrace is popularized and applied in home decoration;

the epoxy floor paint is used in a large amount in parking lots, playgrounds, runways and large-scale rooms, the epoxy floor paint is usually low-price epoxy resin and is added with a large amount of powder fillers, so that the surface brightness is very low, the surface needs to be coated with light again, most of the epoxy floor paint needs to select thermoplastic acrylic acid with high gloss, weather resistance and moderate price as a finishing paint, the adhesive force is up to level 1, the salt spray resistance is up to 200 hours, the flexibility is good, the quick drying is high, and the like, but the current paint is difficult to reach the use standard; therefore, we propose a synthetic method of epoxy modified thermoplastic acrylic resin.

Disclosure of Invention

The present invention is directed to a method for synthesizing an epoxy-modified thermoplastic acrylic resin, which solves the problems set forth in the background above.

In order to solve the technical problems, the invention is realized by the following technical scheme:

the invention relates to a synthetic method of epoxy modified thermoplastic acrylic resin, which comprises the following steps:

step1, epoxy resin E20 and methacrylic acid are selected to perform ring opening reaction at 90-105 ℃, and the deacidification value is less than 3;

step2, diluting with PMA and BAC solvent to 60% to obtain material A;

step3, firstly, carrying out esterification reaction on phosphorus pentoxide and hydroxypropyl acrylate for 10-15 min;

step4, obtaining a phosphate B material based on the reaction;

step5, synthesizing resin according to an acrylic resin process, comprising the following steps:

the method comprises the following steps: using benzene-free solvents PMA and BAC as bedding reflux solvents, and designing TG at 80 and solid content of material C at 45% by using MMA, BA and MAA;

step two: adding 8 to 10 percent of material A, 0.5 to 1 percent of material B and a proper amount of azodiisobutyronitrile;

step three: carrying out polymerization reaction at 90-95 ℃;

step four: based on the reaction steps, the epoxy modified thermoplastic acrylic resin with the solid content of 50 percent, the acid value of less than 5 and the viscosity of between 15000 and 25000 is obtained.

And Step6, completing the synthesis of the epoxy modified thermoplastic acrylic resin.

Preferably, the molar ratio of the epoxy resin E20 to the methacrylic acid in Step1 is 1: 0.98.

Preferably, the molar ratio of the phosphorus pentoxide to the hydroxypropyl acrylate in Step3 is 1: 5.

Preferably, the esterification reaction temperature of phosphorus pentoxide and hydroxypropyl acrylate in Step3 is 90-105 ℃.

Preferably, in Step5, the polymerization reaction time of the material A, the material B and the material C and the azobisisobutyronitrile is 6 to 8 hours.

The invention has the following beneficial effects:

the epoxy modified thermoplastic acrylic resin for epoxy floor paint repair and finishing has the advantages that the adhesive force reaches the national standard level 1, the glossiness is kept above 80, the weather resistance is good, and the using effect is excellent.

The epoxy modified thermoplastic acrylic resin for epoxy floor paint repair and finishing passes a salt spray test for 200 hours, has good flexibility, can pass a 2mm bend, and has good film forming property, good quick-drying effect, strong use adaptability and high popularization value.

Of course, it is not necessary for any product in which the invention is practiced to achieve all of the above-described advantages at the same time.

Drawings

In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.

FIG. 1 is a flow chart of a synthetic method of epoxy modified thermoplastic acrylic resin 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, and not all of the 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 one

Please refer to fig. 1: the invention relates to a synthetic method of epoxy modified thermoplastic acrylic resin, which comprises the following steps:

step1, epoxy resin E20 and methacrylic acid are selected to perform ring opening reaction at 90-105 ℃, and the deacidification value is less than 3;

step2, diluting with PMA and BAC solvent to 60% to obtain material A;

step3, firstly, carrying out esterification reaction on phosphorus pentoxide and hydroxypropyl acrylate for 10-15 min;

step4, obtaining a phosphate B material based on the reaction;

step5, synthesizing resin according to an acrylic resin process, comprising the following steps:

the method comprises the following steps: using benzene-free solvents PMA and BAC as bedding reflux solvents, and designing TG at 80 and solid content of material C at 45% by using MMA, BA and MAA;

step two: adding 8 to 10 percent of material A, 0.5 to 1 percent of material B and a proper amount of azodiisobutyronitrile;

step three: carrying out polymerization reaction at 90-95 ℃;

step four: based on the reaction steps, the epoxy modified thermoplastic acrylic resin with the solid content of 50 percent, the acid value of less than 5 and the viscosity of between 15000 and 25000 is obtained.

And Step6, completing the synthesis of the epoxy modified thermoplastic acrylic resin.

Wherein, the molar ratio of the epoxy resin E20 to the methacrylic acid in Step1 is 1: 0.98.

Wherein, the molar ratio of the phosphorus pentoxide to the hydroxypropyl acrylate in Step3 is 1: 5.

Wherein the esterification reaction temperature of phosphorus pentoxide and hydroxypropyl acrylate in Step3 is 90-105 ℃.

Wherein, in the third Step of Step5, the polymerization reaction time of the material A, the material B and the material C and the azobisisobutyronitrile is 6 to 8 hours.

The epoxy paint is coated with finish paint, and the greatest difficulty is the problem of adhesion; in order to solve the adhesion problem, the acrylic resin is modified by the epoxy resin with epoxy groups, which is the same as the primer, so as to achieve the effect of good adhesion between layers with similar groups, and because the epoxy resin has higher hardness after being cured, the adhesion of the epoxy modified acrylic resin cannot achieve better effect, a self-made phosphate modified polymer adhesive force functional monomer is introduced in the scheme, and the phosphate modified polymer adhesive force functional monomer is polymerized with an acrylate monomer to form high molecular resin, so that the adhesion on the epoxy primer is effectively improved, and the salt spray resistance improves the vitrification temperature of the resin and the molecular weight of the resin.

Example two

Aiming at the effect test of the modified thermoplastic acrylic resin, the modified thermoplastic acrylic resin prepared by the method is selected and expressed as group D, 4 groups of commercial common paint coatings are selected and expressed as A, B and group C respectively, under the same observation environment and observation time, the adhesion, the glossiness, the flexibility and the salt spray resistance of 5 groups of coatings are tested, and the test results are shown in the following table;

table one is the test comparison effect of 5 groups of coatings:

group of Adhesion (grade) Glossiness (60 degree) Flexibility (mm) Salt spray resistance (200h)
A ≤3 74 ≤3 Severe rust and slight discoloration
B ≤1 83 ≤8 No rust and no color change
C ≤2 79 ≤1 No rust and slight discoloration
D ≤1 91 ≤2 No rust and no color change

As can be seen from the above table, compared with the common paint coatings sold in the market, the modified thermoplastic acrylic resin has stronger advantages in the aspects of adhesion performance, glossiness, flexibility, salt spray resistance and the like, and has better use effect and higher popularization value.

In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.

The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.

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