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Preparation of hydroxyl/sulfo bifunctional vanadium-doped heteropolyacid ionic hybrid and application thereof

A sulfonic acid-based bifunctional, heteropolyacid anion technology, applied in the preparation of organic compounds, catalytic reactions, catalysts for physical/chemical processes, etc., can solve problems such as increasing the difficulty of phenol purification and reducing the selectivity of catalytic systems.

Active Publication Date: 2018-03-06
MINJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main problem of this process is that the generated phenol is easily further oxidized to hydroquinone and quinone, and one-step polymerization produces tar-like by-products, which not only reduces the selectivity of the catalytic system, but also increases the difficulty of phenol purification

Method used

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  • Preparation of hydroxyl/sulfo bifunctional vanadium-doped heteropolyacid ionic hybrid and application thereof
  • Preparation of hydroxyl/sulfo bifunctional vanadium-doped heteropolyacid ionic hybrid and application thereof
  • Preparation of hydroxyl/sulfo bifunctional vanadium-doped heteropolyacid ionic hybrid and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Embodiment 1: the synthesis of quaternary ammonium salt

[0035]Step S101: In a reaction flask equipped with nitrogen protection and magnetic stirring, add 16.6g of sodium bisulfite and appropriate amount of distilled water, stir until completely dissolved, slowly add 9.3g of epichlorohydrin dropwise, and react at room temperature for 4 hours. The crude product was obtained by filtration, and the crude product was recrystallized with a mixed solvent of ethanol / water (V / V=3:1) to obtain 16.5 g of the product 3-chloro-2-hydroxypropanesulfonate sodium, with a yield of 85.4%.

[0036] FT-IR(KBr), ν / cm -1 : 3359 (-OH stretching vibration), 2923 (saturated -CH stretching vibration), 1422 (in-plane bending vibration of -OH), 1178.79, 1051.56 (-SO 3 stretching vibration), 728.28 (-ch 2 -Cl stretching vibration).

[0037] Step S102: In a reaction flask equipped with nitrogen protection and stirring, add 4.9 g of 3-chloro-2-hydroxypropanesulfonate sodium, 25 ml of ion-free, s...

Embodiment 2

[0040] Example 2 [C 17 h 38 N + o 4 S] 7 [P 2 Mo 17 VO 62 -7 ](HVSM-1) synthesis

[0041] Step S101: Add 7.71H to the reactor equipped with magnetic stirring 7 [P 2 Mo 17 VO 62 ], after dissolving completely with minimum amount of deionized water, slowly drip the aqueous solution of 7.0g quaternary ammonium salt that embodiment 1 obtains, add and react 8 hours under the reflux reaction state. h 7 [P 2 Mo 17 VO 62 ]: quaternary ammonium salt = 1:7 (molar ratio).

[0042] Step S102: Suction filter or centrifuge the reaction mixture obtained in Step S101, wash the collected solids with deionized water, and vacuum-dry them at 60° C. to constant weight. The yield of the target compound is 90%.

[0043] FT-IR(KBr), ν / cm －1 : 3421 (O-H stretching vibration), 2924 (saturation-CH stretching vibration), 1160 (S=O stretching vibration), 1063 (P-O stretching vibration), 960 (V-O asymmetric stretching vibration), 868, 782 (Mo-O -Mo stretching vibration).

[0044] Hybrid...

Embodiment 3

[0047] Ionic hybrid [C 17 h 38 N + o 4 S] 8 [P 2 Mo 16 V 2 o 62 -8 ]Synthesis

[0048] Step S101: the preparation of the amphoteric salt is the same as the synthesis of the quaternary ammonium salt in Example 1;

[0049] Step S102: divide H 8 [P 2 Mo 16 V 2 o 62 ] Except that the dosage is 8.9 g, the other operations are the same as above. The target product yield is 90%.

[0050] Ion hybrid FT-IR (KBr), ν / cm －1 : 3446 (O-H stretching vibration), 2925 (saturation-CH stretching vibration), 1040 (Si-O stretching vibration), 972 (W-O stretching vibration), 921, 793 (W-O-W stretching vibration). [C 17 h 38 N + o 4 S] 8 [P 2 Mo 16 V 2 o 62 -8 ]

[0051] Hybrid Elemental Analysis, C 136 h 304 N 8 P 2 Mo 16 o 94 S 8 V 2 : Measured value (calculated value), %: C 29.64 (29. 62); H 5.56 (5. 51); N 2.03 (2. 00); S 4.65 (4. 63). The hybrid XRD does not appear H 7 [P 2 Mo 17 VO 62 ] The characteristic peaks of heteropolyacids indicate that the hybr...

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Abstract

The invention discloses preparation of a hydroxyl / sulfo bifunctional vanadium-doped heteropolyacid ionic hybrid and application thereof. In the structure of the hydroxyl / sulfo bifunctional vanadium-doped heteropolyacid ionic hybrid, a long-chain quaternary ammonium structure cation simultaneously has hydroxyl / sulfo bifunctional groups, and the matched heteropolyacid anions are respectively [P2Mo17VO62]-7, [P2Mo16V2O62]-8 and [P2Mo15V3O62]-9; and 7 or 8 or 9 bifunctional organic cations are coated on the surface of nano-scale polyoxoanions due to electrostatic interaction so as to present a core-shell structure. The prepared ionic hybrid serving as a heterogeneous catalyst is applied to a phenol cleaning preparation method. The phenol preparation method provided by the invention has the characteristics of being high in reaction activity of the catalytic system, excellent in selectivity, mild in reaction conditions, high in operating flexibility, easily separable in products, high in purity, recyclable in catalytic system and the like.

Description

technical field [0001] The invention belongs to the technical field of chemical products and their preparation, and specifically relates to the design and synthesis of three hydroxyl / sulfonate-based vanadium-doped heteropolyacid ion hybrids; the synthesized ionic liquid is used as a heterogeneous catalytic system, and industrial-grade peroxidation Hydrogen is a green oxidant, and benzene can be oxidized and hydroxylated to phenol in one step under solvent-free reaction conditions. Background technique [0002] Phenol is an important organic chemical raw material, widely used in industrial fields such as synthetic fibers, synthetic rubber, synthetic plastics, medicine, pesticides, spices, dyes, and paints. In 2012, the global phenol consumption exceeded 10 million tons. At present, my country's phenol self-sufficiency rate is about 65%, and there is a large market gap. The preparation methods of phenol can be divided into two types: multi-step synthesis method and one-step s...

Claims

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Application Information

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IPC IPC(8): B01J31/18C07C37/58C07C39/04
CPCC07C37/58B01J27/199B01J31/0279B01J31/0298B01J2231/70B01J35/398C07C39/04Y02P20/52
Inventor 李心忠
Owner MINJIANG UNIV
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