Synthesis method of imino butylated amino resin

Abstract

The invention discloses a synthesis method of imino butylated amino resin. The synthesis method comprises the following steps: adding butyl alcohol and tetramethylol melamine into a reaction kettle according to a certain ratio, adjusting the rotating speed of a stirrer of the reaction kettle to 50-120r / min, adding acid to adjust the pH value to 3.0-5.0, raising the temperature to 80-95 DEG C and reacting for 30-60min while preserving the heat; adding alkaline to adjust the pH value to 8.0-10.0, gradually raising the temperature to 90-120 DEG C, and dealcoholizing and dehydrating at normal pressure; starting a vacuum pump, dehydrating under a vacuum condition for 1-3h; and filtering to obtain a colorless thick liquid product. The method is applied to the industrial production of the imino butylated amino resin, is simple in process, capable of saving energy, simple and convenient in aftertreatment, low in production cost and little in discharged wastewater and conforms to the concepts of environment friendliness and resource saving.

Description

technical field

[0001] The invention belongs to the field of chemical synthesis, and in particular relates to the synthesis of iminobutyl etherified amino resins. Background technique

[0002] Iminobutyl etherified amino resin has excellent compatibility and fast low-temperature curing performance, and is an important crosslinking agent for coatings. At present, domestic production of butanol-based butanol resins is generally based on the reaction of methyl-etherified amine-based resins with butanol to obtain mixed-etherified amine-based resins. For example, the application number is 201210554152.7. The melamine resin adopts methyl etherified hexamethylol melamine resin as a raw material, and the reaction temperature is about 80-90°C. Its synthesis temperature is high, and the content of imino group in the synthesized resin is low, which limits its application range to some extent. If the iminobutyl etherified amino resin can be synthesized in one step, the synthesis proce...

Examples

Embodiment 1

[0018] A kind of method taking tetramethylol melamine as raw material synthetic imino butylated amino resin, concrete steps are as follows:

[0019] (1) Add metered n-butanol to the reaction kettle according to the tetramethylolmelamine: n-butanol molar ratio of 1:4, adjust the stirring speed of the reaction kettle to 70 rpm, add 36% hydrochloric acid aqueous solution to adjust the pH value is 3.0, add the tetramethylolmelamine measured above, keep the pH value at 3.0 with 36% hydrochloric acid aqueous solution, and heat up to 30°C to dissolve it;

[0020] (2) After complete dissolution, the temperature was raised to 40°C, and the temperature was kept for 30 minutes;

[0021] (3) Use 30% sodium hydroxide aqueous solution to neutralize the acidity in the system, adjust the pH value to 8.0, and gradually raise the temperature to 90°C for dehydration and dealcoholization under normal pressure;

[0022] (4) Start the vacuum pump, control the vacuum degree to 0.08MPa, and dehydrat...

Embodiment 2

[0025] A kind of method taking tetramethylol melamine as raw material synthetic imino butylated amino resin, its specific steps are the same as embodiment 1, wherein:

[0026] In step (1), add metered isobutanol to the reactor according to the tetramethylolmelamine: isobutanol molar ratio of 1:4, adjust the stirring speed of the reactor to 70 rpm, add 36% hydrochloric acid aqueous solution Adjust the pH to 3.5, add the above metered tetramethylol melamine, use 36% hydrochloric acid aqueous solution to keep the pH value at 3.5, and heat up to 30°C to dissolve it;

[0027] In step (2), heat up to 55°C for 50 minutes;

[0028] In step (3), adjust the pH value to 9.0;

[0029] In step (4), the vacuum degree is controlled to 0.07 MPa, and the temperature is 80° C. for dehydration for 2 hours.

[0030] In step (5), filter to obtain a colorless viscous liquid product with a conversion rate of 76% (calculated by tetramethylolmelamine).

Embodiment 3

[0032] A kind of new method that takes tetramethylol melamine as raw material synthetic imino butylated amino resin, its specific steps are the same as embodiment 1, wherein:

[0033] In step (1), press tetramethylol melamine: n-butanol mol ratio is 1: 6 feeds, adjust pH value with 30% sulfuric acid aqueous solution twice and be 4.0;

[0034] In step (2), heat up to 65°C for 60 minutes;

[0035] In step (3), the pH is adjusted to 9.5 with 30% sodium carbonate aqueous solution;

[0036] In step (4), the vacuum degree is controlled to 0.06MPa, and the temperature is 110°C for dealcoholization for 3h.

[0037] In step (5), filter to obtain a colorless viscous liquid product with a conversion rate of 82% (calculated by tetramethylolmelamine).

technical field

[0001] The invention belongs to the field of chemical synthesis, and in particular relates to the synthesis of iminobutyl etherified amino resins. Background technique

[0002] Iminobutyl etherified amino resin has excellent compatibility and fast low-temperature curing performance, and is an important crosslinking agent for coatings. At present, domestic production of butanol-based butanol resins is generally based on the reaction of methyl-etherified amine-based resins with butanol to obtain mixed-etherified amine-based resins. For example, the application number is 201210554152.7. The melamine resin adopts methyl etherified hexamethylol melamine resin as a raw material, and the reaction temperature is about 80-90°C. Its synthesis temperature is high, and the content of imino group in the synthesized resin is low, which limits its application range to some extent. If the iminobutyl etherified amino resin can be synthesized in one step, the synthesis proce...

Examples

Embodiment 1

[0018] A kind of method taking tetramethylol melamine as raw material synthetic imino butylated amino resin, concrete steps are as follows:

[0019] (1) Add metered n-butanol to the reaction kettle according to the tetramethylolmelamine: n-butanol molar ratio of 1:4, adjust the stirring speed of the reaction kettle to 70 rpm, add 36% hydrochloric acid aqueous solution to adjust the pH value is 3.0, add the tetramethylolmelamine measured above, keep the pH value at 3.0 with 36% hydrochloric acid aqueous solution, and heat up to 30°C to dissolve it;

[0020] (2) After complete dissolution, the temperature was raised to 40°C, and the temperature was kept for 30 minutes;

[0021] (3) Use 30% sodium hydroxide aqueous solution to neutralize the acidity in the system, adjust the pH value to 8.0, and gradually raise the temperature to 90°C for dehydration and dealcoholization under normal pressure;

[0022] (4) Start the vacuum pump, control the vacuum degree to 0.08MPa, and dehydrat...

Embodiment 2

[0025] A kind of method taking tetramethylol melamine as raw material synthetic imino butylated amino resin, its specific steps are the same as embodiment 1, wherein:

[0026] In step (1), add metered isobutanol to the reactor according to the tetramethylolmelamine: isobutanol molar ratio of 1:4, adjust the stirring speed of the reactor to 70 rpm, add 36% hydrochloric acid aqueous solution Adjust the pH to 3.5, add the above metered tetramethylol melamine, use 36% hydrochloric acid aqueous solution to keep the pH value at 3.5, and heat up to 30°C to dissolve it;

[0027] In step (2), heat up to 55°C for 50 minutes;

[0028] In step (3), adjust the pH value to 9.0;

[0029] In step (4), the vacuum degree is controlled to 0.07 MPa, and the temperature is 80° C. for dehydration for 2 hours.

[0030] In step (5), filter to obtain a colorless viscous liquid product with a conversion rate of 76% (calculated by tetramethylolmelamine).

Embodiment 3

[0032] A kind of new method that takes tetramethylol melamine as raw material synthetic imino butylated amino resin, its specific steps are the same as embodiment 1, wherein:

[0033] In step (1), press tetramethylol melamine: n-butanol mol ratio is 1: 6 feeds, adjust pH value with 30% sulfuric acid aqueous solution twice and be 4.0;

[0034] In step (2), heat up to 65°C for 60 minutes;

[0035] In step (3), the pH is adjusted to 9.5 with 30% sodium carbonate aqueous solution;

[0036] In step (4), the vacuum degree is controlled to 0.06MPa, and the temperature is 110°C for dealcoholization for 3h.

[0037] In step (5), filter to obtain a colorless viscous liquid product with a conversion rate of 82% (calculated by tetramethylolmelamine).