Preparation method for pentadiene petroleum resin

Abstract

The invention relates to a preparation method for pentadiene petroleum resin. The method comprises the following step of: synthesizing pentadiene petroleum resin by taking a pentadiene concentrate as a raw material and taking a boron trifluoride complex as a catalyst, wherein the catalyst consists of boron trifluoride and a complexing agent; the complexing agent consists of C1-C10 alcohol and benzene alkyl ether C6H5-OR; in the formula, R is methyl, ethyl or butyl; the molar ratio of the C1-C10 alcohol to the benzene alkyl ether is 2-8; the molar ratio of the boron triflouride to the complexing agent is 0.5-0.8; and a preparation method for the boron triflouride complex serving as the catalyst comprises the following steps of: adding the C1-C10 alcohol and the benzene alkyl ether into a reactor; cooling the materials in the reactor to 0 DEG C to 30 DEG C below zero while stirring; introducing boron triflouride gas into a container within 2-6 hours; and controlling the reaction temperature at -15+ / -5 DEG C. The color phase (Fe-Co) of the pentadiene petroleum resin produced with the method is less than or equal to 5, and the softening point is 89 DEG C.

Description

technical field

[0001] The present invention relates to a kind of preparation method of piperylene petroleum resin with higher softening point, especially boron trifluoride (BF 3 ) complex is the method for catalyst synthesis piperylene petroleum resin. Background technique

[0002] Piperylene petroleum resin is generally prepared by cationic polymerization, usually using Lewis acid catalysts such as metal or non-metal halides. Among these Lewis acids, the most widely used is AlCl 3 , because the single-component Lewis acid catalyst itself has certain limitations in the control of the reaction during the polymerization process. At this time, the polymerization reaction is a heterogeneous reaction, which makes the polymerization reaction difficult to control and the product quality is unstable. Therefore, in the reaction system The introduction of a composite catalyst can regulate the polymerization reaction and improve the performance of the resin.

[0003] Patent US441950...

Examples

Embodiment 1

[0020] Add solvent and boron trifluoride complex catalyst in proportion in reactor, then slowly drop piperylene concentrate (composition is shown in Table 1), catalyst and piperylene consumption ratio (weight) are 0.6, Control the rate of addition so that the reaction temperature is within 20°C. After the dropwise addition, the temperature was raised slowly, the reaction temperature was controlled at 20° C., and the reaction time was 10 h. After the reaction, deactivate with water, filter and use air stripping method to obtain the product piperylene petroleum resin, the resin yield reaches 82%, the hue (Fe—Co) can be obtained≤5, and the softening point is 89°C.

Embodiment 2

[0022] The experimental process and raw materials are the same as in Example 1, the catalyst to piperylene dosage ratio (weight) is 0.8, the reaction temperature is changed to 40° C., and the reaction time is 5 hours. After the reaction, unpolymer and solvent are flashed off to obtain the product piperylene petroleum resin with a resin yield of 84%, a hue (Fe-Co)≤4, and a softening point of 95°C.

Embodiment 3

[0024] The experimental process and raw materials are the same as in Example 1, the catalyst to piperylene dosage ratio (weight) is 0.5, the reaction temperature is changed to 50° C., and the reaction time is 6 hours. After the reaction is finished, unpolymer and solvent are flashed off to obtain the product piperylene petroleum resin with a resin yield of 88%, a hue (Fe-Co)≤4, and a softening point of 100°C.

technical field

[0001] The present invention relates to a kind of preparation method of piperylene petroleum resin with higher softening point, especially boron trifluoride (BF 3 ) complex is the method for catalyst synthesis piperylene petroleum resin. Background technique

[0002] Piperylene petroleum resin is generally prepared by cationic polymerization, usually using Lewis acid catalysts such as metal or non-metal halides. Among these Lewis acids, the most widely used is AlCl 3 , because the single-component Lewis acid catalyst itself has certain limitations in the control of the reaction during the polymerization process. At this time, the polymerization reaction is a heterogeneous reaction, which makes the polymerization reaction difficult to control and the product quality is unstable. Therefore, in the reaction system The introduction of a composite catalyst can regulate the polymerization reaction and improve the performance of the resin.

[0003] Patent US441950...

Examples

Embodiment 1

[0020] Add solvent and boron trifluoride complex catalyst in proportion in reactor, then slowly drop piperylene concentrate (composition is shown in Table 1), catalyst and piperylene consumption ratio (weight) are 0.6, Control the rate of addition so that the reaction temperature is within 20°C. After the dropwise addition, the temperature was raised slowly, the reaction temperature was controlled at 20° C., and the reaction time was 10 h. After the reaction, deactivate with water, filter and use air stripping method to obtain the product piperylene petroleum resin, the resin yield reaches 82%, the hue (Fe—Co) can be obtained≤5, and the softening point is 89°C.

Embodiment 2

[0022] The experimental process and raw materials are the same as in Example 1, the catalyst to piperylene dosage ratio (weight) is 0.8, the reaction temperature is changed to 40° C., and the reaction time is 5 hours. After the reaction, unpolymer and solvent are flashed off to obtain the product piperylene petroleum resin with a resin yield of 84%, a hue (Fe-Co)≤4, and a softening point of 95°C.

Embodiment 3

[0024] The experimental process and raw materials are the same as in Example 1, the catalyst to piperylene dosage ratio (weight) is 0.5, the reaction temperature is changed to 50° C., and the reaction time is 6 hours. After the reaction is finished, unpolymer and solvent are flashed off to obtain the product piperylene petroleum resin with a resin yield of 88%, a hue (Fe-Co)≤4, and a softening point of 100°C.

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