Preparation method of amino-functional bisphenol A epoxy resin

Abstract

The invention discloses a preparation method of an amino-functional bisphenol A epoxy resin. The method includes the steps of 1, weighting a certain amount of bisphenol A, adding a solvent under the protection of nitrogen, evenly stirring, adding thionyl chloride, evenly stirring, adjusting the temperature to 60-80 DEG C, stirring for 5-8 h, filtering to obtain a primary product, washing the primary product with deionized water until the primary product is neutral, and drying for use; 2, evenly mixing the primary product prepared in step 1 with an amine compound, flowing back at 80-100 DEG C for 6-10 h, filtering to obtain a secondary product, washing the secondary product until the secondary product is neutral, and drying for use; 3, adding the secondary product prepared in step 2 into a reaction vessel, adding epoxy chloropropane to react at 50-70 DEG C for 5-8 h, and filtering and washing to obtain a final product. The epoxy resin prepared by the preparation method includes not only an active epoxy group, but also an amino-functional group, and can react with different curing agents, which enlarges the application scope of the epoxy resin.

Description

technical field

[0001] The invention belongs to the field of epoxy resin preparation, and in particular relates to the preparation of amino functionalized bisphenol A epoxy resin. Background technique

[0002] Epoxy resin has the advantages of strong adhesion, high mechanical strength, insulation, and corrosion resistance, and is widely used in the field of coatings. The existing epoxy resins include glycidyl ether epoxy resins and glycidyl ester epoxy resins. , glycidyl amine epoxy resins, linear aliphatic epoxy resins, and alicyclic epoxy resins. These epoxy resins all have epoxy groups, and the reaction between epoxy groups and curing agents can further The coating is modified to make the coating have better properties. Commonly used epoxy resins include bisphenol A epoxy resin, bisphenol F epoxy resin, etc. Bisphenol epoxy resin passes phenolic hydroxyl and epichlorohydrin Reaction preparation, the obtained resin has epoxy active group, which can react with amine curing...

Examples

Embodiment 1

[0027] A kind of preparation of amino functionalized bisphenol A epoxy resin, concrete steps are as follows:

[0028] Step 1: Weigh 1kg of bisphenol A, under the protection of nitrogen, add 100L tetrahydrofuran, stir evenly, add 200L thionyl chloride, stir for 40min, adjust the temperature to 70°C, stir for 6h after the temperature is constant, and then filter to obtain The one-step product is washed with deionized water to neutrality and then dried for use;

[0029] Step 2: After mixing the one-step product prepared in step 1 and ammonia water according to the molar ratio of 1:2.2, reflux at 90°C for 7 hours and then filter to obtain the second-step product, which is washed to neutral and then dried for use;

[0030] Step 3: Take 100 mol of the second-step product prepared in step 2 and put it into the reaction vessel, then add 240 mol of epichlorohydrin into it, react at 60° C. for 7 hours, filter and wash to obtain the final product.

[0031] The prepared amino-functionali...

Embodiment 2

[0037] A kind of preparation of amino functionalized bisphenol A epoxy resin, concrete steps are as follows:

[0038] Step 1: Weigh 1kg of bisphenol A, add 80L of pyridine under nitrogen protection, stir evenly, add 150L of thionyl chloride, stir for 20min, adjust the temperature to 60°C, stir for 5h after the temperature is constant, and then filter to obtain The one-step product is washed with deionized water to neutrality and then dried for use;

[0039] Step 2: Mix the one-step product prepared in step 1 and ethylenediamine evenly according to the molar ratio of 1:2, reflux at 80°C for 6 hours, and then filter to obtain the second-step product, which is washed to neutral and then dried for use;

[0040] Step 3: Take 100 mol of the second-step product prepared in step 2 and put it into a reaction vessel, then add 200 mol of epichlorohydrin into it, react at 50°C for 8 hours, filter and wash to obtain the final product.

[0041] The prepared amino-functionalized bisphenol A...

Embodiment 3

[0047] A kind of preparation of amino functionalized bisphenol A epoxy resin, concrete steps are as follows:

[0048] Step 1: Weigh 1kg of bisphenol A, add 150L of pyridine under nitrogen protection, stir evenly, add 250L of thionyl chloride, stir for 50min, adjust the temperature to 80°C, stir for 8h after the temperature is constant, and then filter to obtain The one-step product is washed with deionized water to neutrality and then dried for use;

[0049] Step 2: Mix the one-step product prepared in step 1 and ethylenediamine evenly according to the molar ratio of 1:2.5, reflux at 110°C for 10 hours, and then filter to obtain the second-step product, which is washed to neutral and then dried for use;

[0050] Step 3: Take 100 mol of the second-step product prepared in step 2 and put it into the reaction vessel, then add 270 mol of epichlorohydrin into it, react at 70° C. for 8 hours, filter and wash to obtain the final product.

[0051] The prepared amino-functionalized bi...

technical field

[0001] The invention belongs to the field of epoxy resin preparation, and in particular relates to the preparation of amino functionalized bisphenol A epoxy resin. Background technique

[0002] Epoxy resin has the advantages of strong adhesion, high mechanical strength, insulation, and corrosion resistance, and is widely used in the field of coatings. The existing epoxy resins include glycidyl ether epoxy resins and glycidyl ester epoxy resins. , glycidyl amine epoxy resins, linear aliphatic epoxy resins, and alicyclic epoxy resins. These epoxy resins all have epoxy groups, and the reaction between epoxy groups and curing agents can further The coating is modified to make the coating have better properties. Commonly used epoxy resins include bisphenol A epoxy resin, bisphenol F epoxy resin, etc. Bisphenol epoxy resin passes phenolic hydroxyl and epichlorohydrin Reaction preparation, the obtained resin has epoxy active group, which can react with amine curing...

Examples

Embodiment 1

[0027] A kind of preparation of amino functionalized bisphenol A epoxy resin, concrete steps are as follows:

[0028] Step 1: Weigh 1kg of bisphenol A, under the protection of nitrogen, add 100L tetrahydrofuran, stir evenly, add 200L thionyl chloride, stir for 40min, adjust the temperature to 70°C, stir for 6h after the temperature is constant, and then filter to obtain The one-step product is washed with deionized water to neutrality and then dried for use;

[0029] Step 2: After mixing the one-step product prepared in step 1 and ammonia water according to the molar ratio of 1:2.2, reflux at 90°C for 7 hours and then filter to obtain the second-step product, which is washed to neutral and then dried for use;

[0030] Step 3: Take 100 mol of the second-step product prepared in step 2 and put it into the reaction vessel, then add 240 mol of epichlorohydrin into it, react at 60° C. for 7 hours, filter and wash to obtain the final product.

[0031] The prepared amino-functionali...

Embodiment 2

[0037] A kind of preparation of amino functionalized bisphenol A epoxy resin, concrete steps are as follows:

[0038] Step 1: Weigh 1kg of bisphenol A, add 80L of pyridine under nitrogen protection, stir evenly, add 150L of thionyl chloride, stir for 20min, adjust the temperature to 60°C, stir for 5h after the temperature is constant, and then filter to obtain The one-step product is washed with deionized water to neutrality and then dried for use;

[0039] Step 2: Mix the one-step product prepared in step 1 and ethylenediamine evenly according to the molar ratio of 1:2, reflux at 80°C for 6 hours, and then filter to obtain the second-step product, which is washed to neutral and then dried for use;

[0040] Step 3: Take 100 mol of the second-step product prepared in step 2 and put it into a reaction vessel, then add 200 mol of epichlorohydrin into it, react at 50°C for 8 hours, filter and wash to obtain the final product.

[0041] The prepared amino-functionalized bisphenol A...

Embodiment 3

[0047] A kind of preparation of amino functionalized bisphenol A epoxy resin, concrete steps are as follows:

[0048] Step 1: Weigh 1kg of bisphenol A, add 150L of pyridine under nitrogen protection, stir evenly, add 250L of thionyl chloride, stir for 50min, adjust the temperature to 80°C, stir for 8h after the temperature is constant, and then filter to obtain The one-step product is washed with deionized water to neutrality and then dried for use;

[0049] Step 2: Mix the one-step product prepared in step 1 and ethylenediamine evenly according to the molar ratio of 1:2.5, reflux at 110°C for 10 hours, and then filter to obtain the second-step product, which is washed to neutral and then dried for use;

[0050] Step 3: Take 100 mol of the second-step product prepared in step 2 and put it into the reaction vessel, then add 270 mol of epichlorohydrin into it, react at 70° C. for 8 hours, filter and wash to obtain the final product.

[0051] The prepared amino-functionalized bi...