Zinc-based imidazole type ion liquid for liquid sealing and preparation method thereof
An ionic liquid, zinc-based imidazole technology, applied in the field of zinc-based imidazole ionic liquids and their preparation, can solve the problems of low density, affect product quality, and are not suitable for high-density occasions, and achieve a wide range of applications and liquid ranges. wide effect
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Embodiment 1
[0045] A zinc-based imidazole ionic liquid for liquid sealing, which is obtained by compounding an ionic liquid intermediate and a zinc salt;
[0046] The structural formula of the ionic liquid intermediate is shown in formula (1):
[0047] Formula 1)
[0048] Among them, R 1 One of C2~C8 alkyl, allyl, aminopropyl, R 2 One of the C1-C4 alkyl groups, R 3 for H or CH 3 The anion X is one of the anions of ethyl sulfate, diethyl phosphate, bromide, and chloride; the zinc salt is zinc acetate, zinc bromide, zinc phosphate, zinc sulfate, zinc chloride, zinc fluoroborate, and iodine One of zinc chloride; the density of the ionic liquid intermediate is 1.05-1.20 g / mL, and the density of the ionic liquid is greater than 1.2 g / mL.
[0049] As mentioned above, the zinc-based imidazole ionic liquid used for liquid sealing is prepared through the following steps:
[0050] (1) Preparation of intermediate: mix the raw material containing the target cation with the raw material conta...
Embodiment 2
[0062] The device requiring a liquid seal is a U-shaped glass tube. The material requirements for the liquid seal are: no reaction with glass, stable to water and air below 200°C, non-volatile, and a density of 1.5g / mL or more. Choose 1-ethyl-3-methylimidazole ethyl sulfate salt as an intermediate, choose zinc chloride as a compound salt, and the structural formula of the ionic liquid is:
[0063]
[0064] Its preparation method is:
[0065] (1) Take 82.1g of N-methylimidazole, add 169.6g of diethyl sulfate, stir and react at 50°C for 24 hours, wash with ethyl acetate, and rotary steam at 80°C to obtain 220g of 1-ethyl-3-methylimidazole Ethyl sulfate salt, a light yellow liquid;
[0066] (2) Add 660g of zinc chloride to it, stir and react at 120°C for 12 hours, vacuum rotary evaporate at 100°C, and vacuum dry at 100°C for 24 hours to obtain 850g of light yellow product, [BMIM][EtSO 4 ]·xZnCl 2 , yield 96.6%. After inspection, the ionic liquid has a purity of 97.0% and a...
Embodiment 3
[0068] The device requiring a liquid seal is a vacuum pump, which is made of stainless steel. The material requirements for the liquid seal are: it does not react with 304 stainless steel, and is stable to water, air, and stainless steel below 200 ° C. It is not volatile, and the density requirement is 1.5 g / mL above. Choose 1-aminopropyl-3-butylimidazolium bromide as the intermediate, choose zinc bromide as the complex salt, and the structural formula of the ionic liquid is:
[0069]
[0070] Its preparation method is:
[0071] (1) Take 124.1g of N-butylimidazole, add 262.7g of 3-bromopropylamine hydrobromide, stir and react at 120°C for 24 hours, dry in vacuum at 120°C for 24 hours, wash with ethyl acetate, and rotary evaporate at 80°C to obtain 280g of 1-Aminopropyl--3-butylimidazolium bromide, a light yellow solid;
[0072] (2) Add 560g of zinc bromide to it, stir and react at 200°C for 12 hours, vacuum rotary evaporate at 100°C, and vacuum dry at 100°C for 24 hours t...
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