A kind of polyether amine compound and preparation method and application
A compound, polyetheramine technology, applied in the field of polyetheramine compound and preparation, can solve the problem, can only temporarily stabilize the clay, easy to not compound, high cost, and achieve the effect of good clay anti-swelling rate
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Embodiment 1
[0032] The synthetic route of polyetheramine compound is as follows:
[0033] Step 1, propylene glycol and epichlorohydrin are polymerized in the presence of a base and a catalyst to obtain an intermediate product A chlorinated polyether compound:
[0034]
[0035] Step 2, catalyzed amination of chlorinated polyether and amine to obtain the target product B polyether amine compound:
[0036] .
[0037] The reactions of step 1 and step 2 belong to catalytic polymerization reaction and multifunctional group conversion reaction respectively. The reaction ratio of reactants depends entirely on the final degree of polymerization and functional group conversion rate, not the amount added. Therefore, in order not to cause misunderstanding, in the above synthesis The molar ratio of the reactants is not given in the route, but the specific synthesis conditions are illustrated through the following examples to clarify the addition amount of each substance mass.
[0038] Synthesis...
Embodiment 2
[0045] Synthesis of Intermediate A:
[0046] With the propylene glycol of 6.08g, 0.272g sodium carbonate and 0.100g catalyst IPh 3 C + M(OC 6 f 5 ) 6 -Add a 100mL two-necked flask, install a condenser tube and a constant pressure dropping funnel, and add 55g of pre-dried epichlorohydrin into the constant pressure dropping funnel, under magnetic stirring, use the SCHLENK method to remove the oxygen in the device system, and Continuous nitrogen protection. After deoxygenation is completed, stir and heat in an oil bath at 85°C. At this temperature, drip epichlorohydrin into the flask. After the dropwise addition, continue to heat up to 115°C. After 6 hours of reaction, cool with liquid nitrogen to stop the reaction. The catalyst was removed by filtration, and the obtained pale yellow reaction product was evaporated under reduced pressure to remove incompletely reacted raw materials; finally, 12 g of bright yellow liquid product was obtained, which was intermediate product A...
Embodiment 3
[0051] Synthesis of Intermediate A:
[0052] With the propylene glycol of 7.6g, 0.353g potassium carbonate and 0.120g catalyst IY (OTf) 3 Add a 100mL two-necked flask, install a condenser tube and a constant pressure dropping funnel, and add 78g of pre-dried epichlorohydrin into the constant pressure dropping funnel, under magnetic stirring, use the SCHLENK method to remove the oxygen in the device system, and Continuous nitrogen protection. After deoxygenation is completed, stir and heat in an oil bath at 100°C. At this temperature, drip epichlorohydrin into the flask. After the dropwise addition, continue to heat up to 150°C. After reacting for 5 hours, cool with liquid nitrogen to stop the reaction. The catalyst was removed by filtration, and the obtained pale yellow reaction product was evaporated under reduced pressure to remove incompletely reacted raw materials; finally, 65 g of bright yellow liquid product was obtained, which was intermediate product A.
[0053] Cata...
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