Synthesis method of tackifying alkylphenol formaldehyde resin

Abstract

The invention provides a synthesis method of tackifying alkylphenol formaldehyde resin. The synthesis method comprises the following steps: firstly, adding alkylphenol and an acidic catalyst into a reaction still; secondly, slowly adding 65 to 80 percent of the total amount of formaldehyde aqueous solution after the temperature is raised to 50 to 60 DEG C; carrying out reflux reaction for 1 to 3 hours and steaming out all water, then stopping distillation, slowly adding the remaining formaldehyde aqueous solution and steaming out the water; thirdly, after the reaction time is ended, raising the temperature to 140 to 160 DEG C; distilling out residual water and unreacted alkylphenol in a vacuum state; fourthly, distilling out entrained water and the unreacted alkylphenol, and drying an organic phase by distilling; adding water into the reaction still for washing, separating out a water phase and drying the organic phase to obtain a product disclosed by the invention. According to the preparation method disclosed by the invention, acidic ionic liquid is used as a solvent and a catalyst and replaces the acidic catalyst and the solvent in the synthesis method of the traditional alkylphenol formaldehyd resin, so that the extensive use of organic solvents is effectively avoided.

Description

technical field

[0001] The invention relates to the technical field of phenolic tackifying resin, in particular to a synthesis method of green and high-efficiency tackifying alkylphenolic resin. Background technique

[0002] Lamination method is often used in the production of radial tires and bias tires. It is required that the surface of unvulcanized rubber must have a certain viscosity or initial adhesion. Therefore, self-adhesiveness is very important in the molding process, so it is also called molding viscosity. If there is a lack of viscosity between the rubber materials, especially for synthetic rubber compounds, the semi-finished rubber parts will not only creep to deform the dimensions, but also cause the adhesive parts of the rubber parts to come off due to the expansion during molding. In the product design of all-steel radial tires, thin films with good viscosity are used in many places such as the bead part and the belt layer. If there is no sticking phenomenon...

Examples

Embodiment 1

[0024] The synthesis of p-tert-butylphenol-formaldehyde resin, 1-methylimidazolium bisulfate as acidic catalyst and solvent, p-tert-butylphenol: formaldehyde (molar ratio)=1:0.85; Add formaldehyde aqueous solution (37% ).

[0025] Step 1: Add 46.5g (0.31mol) of p-tert-butylphenol and 3g of 1-methylimidazolium bisulfate to a 500ml four-necked round-bottomed reaction flask equipped with a mechanical stirrer, a thermometer, a reflux condenser and a dropping funnel ;

[0026] Step 2: The temperature of the reaction system was raised to 50°C, and 15.1 g of formaldehyde aqueous solution (37%) was slowly added through the dropping funnel. After the dropwise addition was completed, the temperature of the reaction system was raised to 90°C, and the reaction was refluxed. After 1.8 hours of reaction, the distillation was started. Continue to raise the temperature to 100-110°C, stop the distillation after distilling all the water out; slowly add the remaining formaldehyde aqueous soluti...

Embodiment 2

[0031] Synthesis of p-tert-butylphenol-formaldehyde resin, pyridine bisulfate as acidic catalyst and solvent, p-tert-butylphenol: formaldehyde (molar ratio) = 1:0.85; add formaldehyde aqueous solution (37%) twice.

[0032] Step 1: in the 500ml four-neck round-bottomed reaction flask that mechanical stirrer, thermometer, reflux condenser and dropping funnel are equipped with, add 46.5g (0.31mol) p-tert-butylphenol and 3g pyridine bisulfate;

[0033] Step 2: The temperature of the reaction system was raised to 50°C, and 15.1 g of formaldehyde aqueous solution (37%) was slowly added through the dropping funnel. After the dropwise addition was completed, the temperature of the reaction system was raised to 90°C, and the reaction was refluxed. After 1.8 hours of reaction, the distillation was started. Continue to raise the temperature to 100-110°C, stop the distillation after distilling all the water out; slowly add the remaining formaldehyde aqueous solution from the dropping funne...

Embodiment 3

[0038] Synthesis of tert-octylphenol-formaldehyde resin, pyridinium bisulfate as acidic catalyst and solvent, p-tert-butylphenol: formaldehyde (molar ratio) = 1:0.8; formaldehyde aqueous solution (37%) was added twice.

[0039] Step 1: in the 500ml four-neck round-bottomed reaction flask that mechanical stirrer, thermometer, reflux condenser and dropping funnel are housed, add 63.8g (0.31mol) p-tertoctylphenol and 6g pyridine bisulfate;

[0040] Step 2: The temperature of the reaction system was raised to 50°C, and 17.0g of formaldehyde aqueous solution (37%) was slowly added from the dropping funnel. After the dropwise addition was completed, the temperature of the reaction system was raised to 95°C, and the reaction was refluxed. After 2.5 hours of reaction, the distillation was started. Continue to raise the temperature to 100-110°C, stop the distillation after all the water is distilled; slowly add the remaining formaldehyde solution from the dropping funnel, continue the r...

technical field

[0001] The invention relates to the technical field of phenolic tackifying resin, in particular to a synthesis method of green and high-efficiency tackifying alkylphenolic resin. Background technique

[0002] Lamination method is often used in the production of radial tires and bias tires. It is required that the surface of unvulcanized rubber must have a certain viscosity or initial adhesion. Therefore, self-adhesiveness is very important in the molding process, so it is also called molding viscosity. If there is a lack of viscosity between the rubber materials, especially for synthetic rubber compounds, the semi-finished rubber parts will not only creep to deform the dimensions, but also cause the adhesive parts of the rubber parts to come off due to the expansion during molding. In the product design of all-steel radial tires, thin films with good viscosity are used in many places such as the bead part and the belt layer. If there is no sticking phenomenon...

Examples

Embodiment 1

[0024] The synthesis of p-tert-butylphenol-formaldehyde resin, 1-methylimidazolium bisulfate as acidic catalyst and solvent, p-tert-butylphenol: formaldehyde (molar ratio)=1:0.85; Add formaldehyde aqueous solution (37% ).

[0025] Step 1: Add 46.5g (0.31mol) of p-tert-butylphenol and 3g of 1-methylimidazolium bisulfate to a 500ml four-necked round-bottomed reaction flask equipped with a mechanical stirrer, a thermometer, a reflux condenser and a dropping funnel ;

[0026] Step 2: The temperature of the reaction system was raised to 50°C, and 15.1 g of formaldehyde aqueous solution (37%) was slowly added through the dropping funnel. After the dropwise addition was completed, the temperature of the reaction system was raised to 90°C, and the reaction was refluxed. After 1.8 hours of reaction, the distillation was started. Continue to raise the temperature to 100-110°C, stop the distillation after distilling all the water out; slowly add the remaining formaldehyde aqueous soluti...

Embodiment 2

[0031] Synthesis of p-tert-butylphenol-formaldehyde resin, pyridine bisulfate as acidic catalyst and solvent, p-tert-butylphenol: formaldehyde (molar ratio) = 1:0.85; add formaldehyde aqueous solution (37%) twice.

[0032] Step 1: in the 500ml four-neck round-bottomed reaction flask that mechanical stirrer, thermometer, reflux condenser and dropping funnel are equipped with, add 46.5g (0.31mol) p-tert-butylphenol and 3g pyridine bisulfate;

[0033] Step 2: The temperature of the reaction system was raised to 50°C, and 15.1 g of formaldehyde aqueous solution (37%) was slowly added through the dropping funnel. After the dropwise addition was completed, the temperature of the reaction system was raised to 90°C, and the reaction was refluxed. After 1.8 hours of reaction, the distillation was started. Continue to raise the temperature to 100-110°C, stop the distillation after distilling all the water out; slowly add the remaining formaldehyde aqueous solution from the dropping funne...

Embodiment 3

[0038] Synthesis of tert-octylphenol-formaldehyde resin, pyridinium bisulfate as acidic catalyst and solvent, p-tert-butylphenol: formaldehyde (molar ratio) = 1:0.8; formaldehyde aqueous solution (37%) was added twice.

[0039] Step 1: in the 500ml four-neck round-bottomed reaction flask that mechanical stirrer, thermometer, reflux condenser and dropping funnel are housed, add 63.8g (0.31mol) p-tertoctylphenol and 6g pyridine bisulfate;

[0040] Step 2: The temperature of the reaction system was raised to 50°C, and 17.0g of formaldehyde aqueous solution (37%) was slowly added from the dropping funnel. After the dropwise addition was completed, the temperature of the reaction system was raised to 95°C, and the reaction was refluxed. After 2.5 hours of reaction, the distillation was started. Continue to raise the temperature to 100-110°C, stop the distillation after all the water is distilled; slowly add the remaining formaldehyde solution from the dropping funnel, continue the r...

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