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B/L dual acidic heteropolyacid ion hybrid and preparation method and applications thereof

A dual-acid, heteropolyacid technology, applied in the preparation of sulfonates, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of easy deliquescence of chlorides, pollution of the environment, corrosion of equipment, etc.

Active Publication Date: 2017-11-24
MINJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, chloride is very easy to deliquescence, which will corrode the equipment and pollute the environment.

Method used

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  • B/L dual acidic heteropolyacid ion hybrid and preparation method and applications thereof
  • B/L dual acidic heteropolyacid ion hybrid and preparation method and applications thereof
  • B/L dual acidic heteropolyacid ion hybrid and preparation method and applications thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0066] Ionic Hybrid [N 3 (SO 3 h) 2 ]Al 0.33 SiW 12 O 40 Synthesis

[0067] Step S101: In a reaction flask equipped with stirring, add 9.5 g of 1,4-butane sultone and 20 ml of acetonitrile in turn, stir at room temperature for 15 minutes, add dropwise 6.0 g of pentamethyldiethylenetriamine, and heat up after the addition The reaction was carried out at 45 °C for 24 h; the crude product was filtered with suction and rinsed with ether, and then dried under vacuum at 75 °C for 8 hours to obtain 14.5 g of the intermediate amphoteric salt L2 with a yield of 93.5%;

[0068] L2 is an off-white solid, m.p. 58°C. 1 HNMR (D 2 O, 400 MHz,), δ : 2.16~2.25(m, 8H, 2CH 2 ); 2.26(s, 3H, CH 3 ); 2.934~2.97(m, 8H, 4CH 2 ); 3.13 (s, 12H, 4CH 3 ); 3.47~3.52 (m, 8H, 4CH 2 ). 13 CNMR (D 2 O, 100 MHz), δ : 32.13 (CH 2 CH 2 N), 34.42 (CH 2 CH 2 CH 2 N), 43.35 (NCH 3 ), 48.14 (CH 2 SO 3 ), 51.85((NCH 3 ),, 57.64 (NCH 2 ), 63.67 (N + CH 2 ), 64.24 (CH 2 N + ).

[0069] ...

Embodiment 2

[0072] [N 3 (SO 3 h) 2 ]Ce 0.33 SiW 12 O 4 Synthesis

[0073] Step S101: For the preparation of the amphoteric salt L2, refer to step S101 of Example 1;

[0074] Step S102: the other operations are the same as those in Example 1, except that the aluminum nitrate is replaced by cerium nitrate, and the amount is 0.314 g. The target product 2.9 g was obtained with a yield of 93%.

[0075] Ionic Hybrid [N 3 (SO 3 h) 2 ]Ce 0.33 SiW 12 O 4 FT-IR(KBr), ν / cm －1 : 3422 (O-H stretching vibration), 2925 (saturated-CH stretching vibration), 1040 (Si-O stretching vibration), 972 (W-O stretching vibration), 921, 793 (W-O-W stretching vibration). Elemental analysis of hybrids, C 16 H 41 N 3 SiW 12 O 46 S 2 Ce 0.33 : Found value (calculated value), %: C 5.72 (5.70), H 1.23 (1.21), N 1.25 (1.22), S 1.91, (1.88). The hybrids appear characteristic peaks of Keggin-configuration heteropolyacids in the low-angle region (5°, 8°).

Embodiment 3

[0077] Ionic Hybrid [N 3 (SO 3 h) 2 ]Zn 0.5 SiW 12 O 40 Synthesis

[0078] Step S101: For the preparation of the amphoteric salt L2, refer to step S101 of Example 1;

[0079] Step S102: The other operations are the same as in Example 1, except that zinc chloride is used instead of aluminum nitrate, and the amount is 0.149 g. The target product 2.8 g was obtained with a yield of 90%.

[0080] Ionic Hybrid [N 3 (SO 3 h) 2 ]Zn 0.5 SiW 12 O 40 FT-IR(KBr), ν / cm －1 : 3446 (O-H stretching vibration), 2925 (saturated-CH stretching vibration), 1040 (Si-O stretching vibration), 972 (W-O stretching vibration), 921, 793 (W-O-W stretching vibration). Elemental analysis of hybrids, C 16 H 41 N 3 SiW 12 O 46 S 2 Zn 0.5: measured value (calculated value), %: C 5.75 (5.71), H1.24 (1.21), N 1.26 (1.22), S 1.92, (1.90). The characteristic peaks of heteropolyacids in Keggin configuration appear in the low-angle region (5°, 8°) of the hybrid.

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PUM

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Abstract

The invention belongs to the technical field of chemical products and preparation thereof, and specifically relates to a B / L dual acidic heteropolyacid ion hybrid and a preparation method and applications thereof. The B / L dual acidic heteropolyacid ion hybrid has organic positive ions with one bisulfonic acid functionalized long chain quaternary ammonium structure and transition metal positive ions at the same time. The matched heteropolyacid negative ion is Keggin type phosphotungstic acid or silicotungstic acid negative ions. The organic positive ions with one bisulfonic acid functionalized long chain quaternary ammonium structure and the transition metal positive ions are wrapped on the surface of the heteropolyacid negative ion through electrostatic force so as to form a core-shell structure. The B / L dual acidic heteropolyacid ion hybrid can be used as a heterogeneous catalyst to prepare five acetal (ketal) perfumes: series of benzaldehyde acetal, series of cyclohexanone ketal, fructone, fraistone, and [2-(1-ethoxyethoxy)ethyl]benzene. The heterogeneous catalyst has the characteristics of high catalytic activity, good selectivity, mild conditions, large operation elasticity, easy product separation, and high purity, and the catalyst system can be circularly used.

Description

technical field [0001] The invention belongs to the technical field of chemical products and preparation thereof, and particularly relates to a B / L biacid heteropolyacid ion hybrid and a preparation method and application thereof. Background technique [0002] Acetal (ketone) flavors are carbonyl flavors. In nature, carbonyl compounds mainly exist in the volatile flavors of fruits. The aroma of acetal (ketone) flavors is mild, round and long-lasting, which is superior to the floral, fruity and delicate fragrance of the parent aldehyde (ketone), and also makes up for the instability of the parent aldehyde (ketone) compound. A fast new type of spice. At present, acetal (ketone) flavors are mainly used in edible and daily flavors, which play the role of main flavoring agent or coordinating agent, and at the same time increase the natural feeling of flavoring. For example, apple ester has the aroma of fresh green apple and apple aroma, and can be used in fruit-flavored daily f...

Claims

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Application Information

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IPC IPC(8): B01J31/18B01J27/188C07C303/32C07C309/14C07D317/12C07D317/16C07D317/22C07D319/06C07D317/72C07D319/08C07D317/30C07C41/48C07C43/303
CPCB01J23/30B01J27/188B01J31/0279B01J31/0298C07C41/48C07C303/32C07C309/14C07D317/12C07D317/16C07D317/22C07D317/30C07D317/72C07D319/06C07D319/08C07C43/303
Inventor 李心忠
Owner MINJIANG UNIV
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