阅读说明：本技术 一种耐高温低黄变阻焊uv油墨用树脂及其制备方法 (Resin for high-temperature-resistant low-yellowing solder-resistant UV (ultraviolet) ink and preparation method thereof ) 是由 王国良 宋继瑞 邓煜东 于 2019-11-05 设计创作，主要内容包括：本发明公开了一种耐高温低黄变阻焊UV油墨用树脂及其制备方法,包括：将丙烯酸单体、引发剂、阻聚剂、抗氧剂、溶剂混合均匀后,在90～130℃下滴加到溶剂中,2～3小时滴完,然后控制温度在100～140℃内搅拌反应,直至酸值达到120～140mgKOH/g,从而得到丙烯酸预聚体；向所述丙烯酸预聚体内加入溶剂、环氧基树脂、催化剂、阻聚剂、抗氧剂,然后控制温度在90～110℃内搅拌反应,直至酸值达到25～35mgKOH/g,从而得到耐高温低黄变阻焊UV油墨用树脂。本发明不仅具有较高的硬度与光泽,而且具有良好的耐高温性能和耐黄变性能,可广泛应用于制作白墨、LED灯阻焊油墨、丝网印刷、PCB油墨、线路板UV油墨等诸多领域。(The invention discloses a resin for high-temperature-resistant low-yellowing solder-resistant UV (ultraviolet) ink and a preparation method thereof, wherein the resin comprises the following components: uniformly mixing an acrylic monomer, an initiator, a polymerization inhibitor, an antioxidant and a solvent, dripping the mixture into the solvent at the temperature of 90-130 ℃, finishing dripping within 2-3 hours, and then controlling the temperature to be within 100-140 ℃ to stir and react until the acid value reaches 120-140 mgKOH/g, thereby obtaining an acrylic prepolymer; and adding a solvent, epoxy resin, a catalyst, a polymerization inhibitor and an antioxidant into the acrylic prepolymer, and then controlling the temperature to be 90-110 ℃ and stirring for reaction until the acid value reaches 25-35 mgKOH/g, thereby obtaining the resin for the high-temperature-resistant low-yellowing-resistance UV ink. The invention not only has higher hardness and gloss, but also has good high temperature resistance and yellowing resistance, and can be widely applied to the fields of white ink manufacturing, LED lamp solder resist ink manufacturing, screen printing, PCB ink manufacturing, circuit board UV ink manufacturing and the like.)

1. A preparation method of resin for high-temperature-resistant low-yellowing solder resist UV ink is characterized by comprising the following steps:

step 1: uniformly mixing 15-25 parts by mass of an acrylic monomer, 0.1-0.4 part by mass of an initiator, 0.009-0.021 part by mass of a polymerization inhibitor, 0.06-0.14 part by mass of an antioxidant and 10-12 parts by mass of a solvent, dropwise adding the mixture into 10-12 parts by mass of the solvent at 90-130 ℃, completing dropwise adding for 2-3 hours, and then controlling the temperature to be within 100-140 ℃ and stirring for reaction until the acid value reaches 120-140 mgKOH/g, thereby obtaining an acrylic prepolymer;

step 2: and adding 20-24 parts of solvent, 20-30 parts of epoxy resin, 0.3-0.8 part of catalyst, 0.021-0.049 part of polymerization inhibitor and 0.24-0.56 part of antioxidant into the acrylic prepolymer, and then controlling the temperature to be within 90-110 ℃ and stirring for reaction until the acid value reaches 25-35 mgKOH/g, so as to obtain the resin for the high-temperature-resistant low-yellowing-resistance UV ink.

2. The preparation method of the resin for the high temperature resistant low yellowing solder mask UV ink, according to claim 1, is characterized in that the water contents of the acrylic monomer, the initiator, the polymerization inhibitor, the antioxidant, the solvent, the epoxy resin and the catalyst are all lower than 500 ppm.

3. The preparation method of the resin for the high temperature resistant low yellowing solder mask UV ink according to claim 1 or 2, wherein the acrylic monomer is at least one of acrylic acid, methacrylic acid, butyl acrylate, methyl methacrylate, styrene, hydroxyethyl acrylate and hydroxypropyl acrylate.

4. The method for preparing the resin for the high temperature resistant low yellowing solder mask UV ink according to claim 1 or 2, wherein the solvent is at least one of dipropylene glycol methyl ether, ethylene glycol butyl ether, diethylene glycol butyl ether, propylene glycol methyl ether, propylene glycol butyl ether and n-butanol.

5. The method for preparing the resin for the high temperature and low yellowing resistance welding resistant UV ink according to claim 1 or 2, wherein the epoxy resin is at least one of 3, 4-epoxycyclohexylmethyl, bis ((3, 4-epoxycyclohexyl) methyl) adipate, 1, 2-epoxy-4-vinylcyclohexane, tetrahydrophthalic acid bisglycidyl ester, glycidyl methacrylate and 3, 4-epoxycyclohexylmethyl methacrylate.

6. The method for preparing the resin for the high temperature resistant low yellowing solder mask UV ink according to claim 1 or 2, wherein the initiator is at least one of di-tert-butyl peroxide, di-tert-amyl peroxide, tert-butyl peroxybenzoate, benzoyl peroxide, azobisisobutyronitrile and azobisisoheptonitrile.

7. The preparation method of the resin for the high temperature resistant low yellowing solder mask UV ink according to claim 1 or 2, wherein the catalyst is at least one of triphenylphosphine, N-dimethylbenzylamine, triethylamine, sodium borohydride and sodium hydroxide.

8. The preparation method of the resin for the high temperature resistant low yellowing solder mask UV ink according to claim 1 or 2, wherein the polymerization inhibitor is at least one of p-hydroxyanisole, hydroquinone and 2, 5-dimethyl hydroquinone.

9. The preparation method of the resin for the high temperature resistant and low yellowing solder mask UV ink according to claim 1 or 2, wherein the antioxidant is at least one of phenothiazine, 2, 6-di-tert-butyl-4-methylphenol, triphenyl phosphite and hypophosphorous acid.

10. The resin for the high-temperature-resistant low-yellowing solder mask UV ink is characterized by being prepared by the preparation method of the resin for the high-temperature-resistant low-yellowing solder mask UV ink according to any one of claims 1 to 9.

Technical Field

The invention relates to the technical field of UV (ultraviolet) photocureable resin for ink, in particular to high-temperature-resistant low-yellowing-resistance UV-resistant ink resin and a preparation method thereof.

Background

With the development of socioeconomic and the improvement of environmental awareness, people put forward higher and higher requirements on the development of the ink. The application field of the traditional ink is narrow, and the problems of solvent volatilization, environmental pollution and the like exist, so that the traditional ink is increasingly limited. Modern ink is developed towards the direction of integrating multiple functions such as high performance, high efficiency, high environmental protection, high decoration, wide application field and the like.

The resin for UV light-curable ink (i.e. UV ink) is a photosensitive resin with relatively low molecular weight, has groups (such as various unsaturated double bonds) capable of undergoing a light-curing reaction, and can be completely cured under the irradiation of ultraviolet light. In the light-cured final product, the resin for the UV light-cured ink is a main material, and the performance of the resin basically determines the main performance of the light-cured final product, so the resin for the UV light-cured ink is undoubtedly an important link for designing the light-cured product.

Among resin systems for UV ink, epoxy-based UV resins have advantages of high hardness, high gloss, good chemical resistance, relatively low price, and the like, and thus have relatively wide applications. However, the epoxy UV resin has poor wettability and leveling property, and the epoxy UV resin has low molecular weight, so that the epoxy UV resin has poor high-temperature resistance and is easy to yellow. Particularly, when the epoxy UV resin is applied to the fields of white ink, LED lamp solder resist ink, silk screen printing and the like, the high temperature resistance and yellowing resistance of the epoxy UV resin are poorer.

Disclosure of Invention

Aiming at the defects in the prior art, the resin for the high-temperature-resistant low-yellowing-resistance UV ink and the preparation method thereof provided by the invention have the advantages of higher hardness and gloss, good high-temperature-resistant performance and yellowing-resistant performance, and can be widely applied to the fields of manufacturing white ink, LED lamp resistance-welding ink, silk-screen printing, PCB ink, circuit board UV ink and the like.

The purpose of the invention is realized by the following technical scheme:

a preparation method of resin for high-temperature-resistant low-yellowing solder-resistant UV (ultraviolet) ink comprises the following steps:

step 1: uniformly mixing 15-25 parts by mass of an acrylic monomer, 0.1-0.4 part by mass of an initiator, 0.009-0.021 part by mass of a polymerization inhibitor, 0.06-0.14 part by mass of an antioxidant and 10-12 parts by mass of a solvent, dropwise adding the mixture into 10-12 parts by mass of the solvent at 90-130 ℃, completing dropwise adding for 2-3 hours, and then controlling the temperature to be within 100-140 ℃ and stirring for reaction until the acid value reaches 120-140 mgKOH/g, thereby obtaining an acrylic prepolymer;

step 2: and adding 20-24 parts of solvent, 20-30 parts of epoxy resin, 0.3-0.8 part of catalyst, 0.021-0.049 part of polymerization inhibitor and 0.24-0.56 part of antioxidant into the acrylic prepolymer, and then controlling the temperature to be within 90-110 ℃ and stirring for reaction until the acid value reaches 25-35 mgKOH/g, so as to obtain the resin for the high-temperature-resistant low-yellowing-resistance UV ink.

Preferably, the water content of the acrylic monomer, the initiator, the polymerization inhibitor, the antioxidant, the solvent, the epoxy resin and the catalyst is less than 500 ppm.

Preferably, the acrylic monomer is at least one of acrylic acid, methacrylic acid, butyl acrylate, methyl methacrylate, styrene, hydroxyethyl acrylate and hydroxypropyl acrylate.

Preferably, the solvent is at least one of dipropylene glycol methyl ether, ethylene glycol butyl ether, diethylene glycol butyl ether, propylene glycol methyl ether, propylene glycol butyl ether and n-butanol.

Preferably, the epoxy resin is at least one of 3, 4-epoxycyclohexylmethyl, bis ((3, 4-epoxycyclohexyl) methyl) adipate, 1, 2-epoxy-4-vinylcyclohexane, tetrahydrophthalic acid bisglycidyl ester, glycidyl methacrylate, and 3, 4-epoxycyclohexylmethyl methacrylate.

Preferably, the initiator is at least one of di-tert-butyl peroxide, di-tert-amyl peroxide, tert-butyl peroxybenzoate, benzoyl peroxide, azobisisobutyronitrile and azobisisoheptonitrile.

Preferably, the catalyst is at least one of triphenylphosphine, N-dimethylbenzylamine, triethylamine, sodium borohydride and sodium hydroxide.

Preferably, the polymerization inhibitor is at least one of p-hydroxyanisole, hydroquinone and 2, 5-dimethyl hydroquinone.

Preferably, the antioxidant is at least one of phenothiazine, 2, 6-di-tert-butyl-4-methylphenol, triphenyl phosphite and hypophosphorous acid.

The resin for the high-temperature-resistant low-yellowing solder-resistant UV ink is prepared by adopting the preparation method of the resin for the high-temperature-resistant low-yellowing solder-resistant UV ink.

According to the technical scheme provided by the invention, the preparation method of the resin for the high-temperature-resistant low-yellowing solder-resistant UV ink takes the acrylic monomer, the initiator, the polymerization inhibitor, the antioxidant, the solvent, the epoxy resin and the catalyst in a specific ratio as main raw materials, the main raw materials are divided into two steps for reaction, the reaction temperature of each step is controlled, and the reaction time and the reaction end point of each step are determined by detecting the acid value of each step, so that the resin for the high-temperature-resistant low-yellowing solder-resistant UV ink is finally prepared. The invention controls the production process of resin synthesis according to the reaction temperature and the acid value of the product, synthesizes the resin for the high-temperature-resistant low-yellowing-resistance UV ink, has higher hardness and luster, and better high-temperature resistance and yellowing resistance, and can be widely applied to the fields of manufacturing white ink, LED lamp resistance welding ink, screen printing, PCB ink, circuit board UV ink and the like.

Detailed Description

In the following, technical solutions in the embodiments of the present invention are clearly and completely described, 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 of the present invention without making any creative effort, shall fall within the protection scope of the present invention.

The resin for the high temperature resistant low yellowing solder mask UV ink and the preparation method thereof provided by the invention are described in detail below. Details which are not described in detail in the embodiments of the invention belong to the prior art which is known to the person skilled in the art.

A preparation method of resin for high-temperature-resistant low-yellowing solder-resistant UV (ultraviolet) ink specifically comprises the following steps:

step 1: uniformly mixing 15-25 parts by mass of an acrylic monomer, 0.1-0.4 part by mass of an initiator, 0.009-0.021 part by mass of a polymerization inhibitor, 0.06-0.14 part by mass of an antioxidant and 10-12 parts by mass of a solvent, dropwise adding the mixture into 10-12 parts by mass of the solvent at 90-130 ℃, finishing dropwise adding for 2-3 hours, and then stirring and reacting at 100-140 ℃ until the acid value reaches 120-140 mgKOH/g, thereby obtaining the acrylic prepolymer.

Step 2: and adding 20-24 parts of solvent, 20-30 parts of epoxy resin, 0.3-0.8 part of catalyst, 0.021-0.049 part of polymerization inhibitor and 0.24-0.56 part of antioxidant into the acrylic prepolymer, and then controlling the temperature to be within 90-110 ℃ and stirring for reaction until the acid value reaches 25-35 mgKOH/g, so as to obtain the resin for the high-temperature-resistant low-yellowing-resistance UV ink.

The resin for the high-temperature-resistant low-yellowing-resistance UV-resistant ink can comprise the following embodiments:

(1) the water contents of the acrylic monomer, the initiator, the polymerization inhibitor, the antioxidant, the solvent, the epoxy resin and the catalyst are all lower than 500 ppm.

(2) The acrylic monomer is at least one of acrylic acid, methacrylic acid, butyl acrylate, methyl methacrylate, styrene, hydroxyethyl acrylate and hydroxypropyl acrylate.

(3) The solvent is at least one of dipropylene glycol methyl ether, ethylene glycol butyl ether, diethylene glycol butyl ether, propylene glycol methyl ether, propylene glycol butyl ether and n-butyl alcohol.

(4) The epoxy resin is at least one of 3, 4-epoxycyclohexylmethyl, bis ((3, 4-epoxycyclohexyl) methyl) adipate, 1, 2-epoxy-4-vinylcyclohexane, tetrahydrophthalic acid bisglycidyl ester, glycidyl methacrylate and 3, 4-epoxycyclohexyl methacrylate.

(5) The initiator is at least one of di-tert-butyl peroxide, di-tert-amyl peroxide, tert-butyl peroxybenzoate, benzoyl peroxide, azobisisobutyronitrile and azobisisoheptonitrile.

(6) The catalyst is at least one of triphenylphosphine, N-dimethylbenzylamine, triethylamine, sodium borohydride and sodium hydroxide.

(7) The polymerization inhibitor is at least one of p-hydroxyanisole, hydroquinone and 2, 5-dimethyl hydroquinone.

(8) The antioxidant is at least one of phenothiazine, 2, 6-di-tert-butyl-4-methylphenol, triphenyl phosphite and hypophosphorous acid.

Specifically, the preparation method of the resin for the high-temperature-resistant low-yellowing solder-resistant UV ink provided by the invention takes an acrylic monomer, an initiator, a polymerization inhibitor, an antioxidant, a solvent, an epoxy resin and a catalyst in a specific ratio as main raw materials, and is divided into two steps for reaction, the reaction temperature of each step is controlled, and the reaction time and the reaction end point of each step are determined by detecting the acid value of each step, so that the resin for the high-temperature-resistant low-yellowing solder-resistant UV ink is finally prepared. The invention controls the production process of resin synthesis according to the reaction temperature and the acid value of the product, synthesizes the resin for the high-temperature-resistant low-yellowing-resistance UV ink, has higher hardness and luster, and better high-temperature resistance and yellowing resistance, and can be widely applied to the fields of manufacturing white ink, LED lamp resistance welding ink, screen printing, PCB ink, circuit board UV ink and the like.

In conclusion, the embodiment of the invention has high hardness and gloss, good high temperature resistance and yellowing resistance, and can be widely applied to the fields of white ink, LED lamp solder resist ink, screen printing, PCB ink, circuit board UV ink and the like.

In order to more clearly show the technical scheme and the technical effects provided by the present invention, the resin for high temperature resistant low yellowing solder mask UV ink and the preparation method thereof provided by the present invention are described in detail with specific examples below.