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Polysulfo-functionalized heteropolyacid ionic hybrid with multiple heteropolyacid negative ions as well as preparation method and application thereof

A heteropolyacid anion, polysulfonic acid functional technology, applied in the preparation of carboxylate, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of easy deactivation, low catalytic activity, and complicated catalyst preparation process. , to achieve good amphipathic effect

Active Publication Date: 2017-05-31
MINJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there are still problems such as cumbersome catalyst preparation process, easy deactivation, high cost, low catalytic activity, low equipment utilization rate, and difficulty in product separation and purification.

Method used

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  • Polysulfo-functionalized heteropolyacid ionic hybrid with multiple heteropolyacid negative ions as well as preparation method and application thereof
  • Polysulfo-functionalized heteropolyacid ionic hybrid with multiple heteropolyacid negative ions as well as preparation method and application thereof
  • Polysulfo-functionalized heteropolyacid ionic hybrid with multiple heteropolyacid negative ions as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] ionic hybrid 4[N 3 (SO 3 h) 2 ]3SiW 12 o 40 Synthesis

[0051] Step S101: Add 9.5 g of 1,4-butane sultone and 20 ml of acetonitrile in sequence in a reaction flask equipped with stirring, stir at room temperature for 15 minutes, add 6.0 g of pentamethyldiethylenetriamine dropwise, and heat up after the addition Reaction at 45°C for 24 h; the crude product was vacuum-dried at 75°C for 8 hours after suction filtration and diethyl ether rinse to obtain 14.5 g of the intermediate amphoteric salt L2 with a yield of 93.7%;

[0052] L2 is an off-white solid, yield 96%, 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 + ).

[0053] Step S102: After fully di...

Embodiment 2

[0056] Ionic hybrid 3[N 2 (SO 3 h) 2 ]2PW 12 o 40 Synthesis

[0057] S101: Add 4.8g of 1,4-butane sultone and 20ml of acetonitrile in turn to a reaction flask equipped with stirring, stir at room temperature for 15 minutes, add 2.0g of tetramethylethylenediamine dropwise, and raise the temperature to 50°C after adding Reacted for 24 h; the crude product was suction-filtered, rinsed with ether, and vacuum-dried at 75°C for 8 hours to obtain 5.8 g of the intermediate amphoteric salt L1 with a yield of 86.7%;

[0058] L1 is an off-white solid in 95% yield, m.p. 66 °C. 1 HNMR (D 2 O, 400 MHz), δ : 2.26~2.47 (m, 8H, 4CH 2 ); 2.99~3.03 (t, 4H, 2CH 2 ); 3.27(s, 12H); 3.59~3.64 (t, 4H, 2CH 2 ); 3.98(t,4H,2CH 2 ). 13 CNMR (D 2 O, 100 MHz), δ : 31.85 (CH 2 CH 2 N), 35.36 (CH 2 CH 2 CH 2 N), 47.86 (CH 2 SO 3 ), 50.81 (NCH 3 ), 63.33 (NCH 2 ), 64.17 (CH 2 N).

[0059] S102: After fully dissolving 1.0 g of amphoteric salt in 15 ml of deionized water, slowly add d...

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Abstract

The invention discloses a polysulfo-functionalized heteropolyacid ionic hybrid with multiple heteropolyacid negative ions as well as a preparation method and an application thereof. Two ionic hybrids with novel structures are built by taking aliphatic polyamine, 1,4-butanesultone, phosphotungstic acid and silicotungstic acid as starting materials and carrying out two steps of atomic economic reaction through quaternization and acidification. Positive ions of the ionic hybrid comprise four or three bissulfo-functionalized long-chain quaternary ammonium positive ions; negative ions matched with the positive ions comprise three Keggin configuration silicotungstic acid negative ions or two Keggin configuration phosphotungstic acid negative ions; the prepared ionic hybrid can be used for preparing cyclohexyl carboxylate. The ionic hybrid has high acid strength and high acid content; the ionic hybrid also shows high amphipathy, so the reaction between substrate cyclohexene and organic carboxylic acid is facilitated; the ionic hybrid has the characteristics of atom economy, mild reaction condition, no backflow water diversion, high separation probability of products and high purity.

Description

technical field [0001] The invention belongs to the technical field of chemical products and their preparation, and in particular relates to polysulfonic acid functionalized polyheteropolyacid anion heteropolyacid ion hybrids and their preparation methods and applications. Background technique [0002] Heteropolyacids not only have strong acidity and mild redox catalytic activity, but also have structural designability at the molecular level. They are one of the "green" catalysts with the most research value and development prospects after molecular sieves. The thermal stability, solubility, and acidity of heteropolyacids are closely related to their counterions, so the physical and chemical properties and catalytic activity of heteropolyacids can be adjusted by changing the counterions. Based on this idea, heteropolyacids with organic cations as counterions Multi-acid ion hybrids came into being. In 2001, Xi et al. reported the first quaternary ammonium heteropolyacid ion ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C309/14B01J31/18B01J31/16C07C69/14C07C67/04C07C69/06C07C69/24
CPCC07C67/04C07C309/14B01J31/0239B01J31/0271B01J31/34B01J35/396C07C69/14C07C69/06C07C69/24
Inventor 李心忠
Owner MINJIANG UNIV
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