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Preparation and application of a cationic polyquaternium vanadium-doped heteropolyacid supramolecular system

A cationic poly-heteropolyacid anion technology, which is applied in the field of preparation of cationic polyquaternary ammonium vanadium-doped heteropolyacid supramolecular systems, can solve problems such as single structure, serious equipment corrosion, and limited types of heteropolyacids

Active Publication Date: 2020-07-31
MINJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Disadvantages of this route: 1) The process route is long; 2) The conversion rate of cyclohexane is low, the equipment is corroded seriously, and the energy consumption is high; 3) A large amount of nitrogen oxides and waste acid are produced, causing serious environmental pollution
This route expands the source of raw materials, but the two-step reaction of hydrogenation and hydration has obvious shortcomings such as unstable catalytic system and low conversion rate, and the use of nitric acid as the oxidation system is seriously polluted
[0006] 3) Butadiene method: The synthesis uses cheap C4 as raw material, which not only effectively reduces the production cost, but also eliminates the environmental pollution problems existing in the traditional process, but there are disadvantages such as complex process, harsh reaction conditions and many by-products
[0014] In summary, heteropolyacids and heteropolyacid complexes have been successfully used as catalytic systems in the clean oxidation of cyclic ketones, but there are still many improvements in the reported catalytic systems, such as limited selection of heteropolyacids. , The structure is relatively simple; the structure of the heteropoly acid complex is relatively complex, the cost is high, and the recycling is inconvenient, etc.

Method used

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  • Preparation and application of a cationic polyquaternium vanadium-doped heteropolyacid supramolecular system
  • Preparation and application of a cationic polyquaternium vanadium-doped heteropolyacid supramolecular system
  • Preparation and application of a cationic polyquaternium vanadium-doped heteropolyacid supramolecular system

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Embodiment 1: the synthesis of cationic polyquaternary ammonium salt

[0048] Step S101: Under nitrogen protection, mix 15ml of dimethyldiallylammonium chloride and 0.5g of EDTA evenly, add dropwise 5% hydrochloric acid (V / V) to adjust the pH to 5, heat to 40°C, add dropwise ammonium persulfate and Sodium bisulfite, react for 1h; add 5% initiator V-44 (V / V) 5ml dropwise, react for 1h; heat to 50°C, add 5% V-44 (V / V) 5ml dropwise, react for 2h; heat To 70 ° C, the reaction 5h.

[0049] Step S102: The reactant obtained in step S101 was poured into acetone to precipitate an off-white crude product, which was vacuum-dried at 80° C. to constant weight. Product quality 8.1g, molecular weight 30000.

[0050] FT-IR (KBr), ν / cm -1 : 2941 (C-H stretching vibration), 1631, 1130 (C-N bond stretching vibration), 1476 (saturated C-H in-plane bending vibration), 943 (C-H bond bending stretching vibration).

Embodiment 2

[0051] Embodiment 2: the synthesis of cationic polyquaternary ammonium salt

[0052] Step S101: Under nitrogen protection, mix 15ml dimethyldiallylammonium chloride and 0.5g EDTA evenly, add 5% hydrochloric acid (V / V) dropwise to adjust the pH to 5, heat to 40°C, add ammonium persulfate dropwise React with sodium bisulfite for 1 hour; add 7ml of 5% V-44 (V / V) dropwise, react for 1 hour; heat to 50°C, add 7ml of 5% V-44 (V / V), react for 2 hours; heat to 70°C, react for 5h.

[0053] Step S102: The step polymerization is the same as in Example 1, the product quality is 5.5 g, and the molecular weight is 15,000.

[0054] FT-IR (KBr), ν / cm -1 : 2937 (C-H stretching vibration), 1642, 1132 (C-N bond stretching vibration), 1476 (saturated C-H in-plane bending vibration), 946 (C-H bond bending stretching vibration).

Embodiment 3

[0055] Embodiment 3: the synthesis of cationic polyquaternary ammonium salt

[0056] Step S101: Under nitrogen protection, mix 15mD dimethyldiallylammonium chloride and 0.5g EDTA evenly, add 5% hydrochloric acid (V / V) dropwise to adjust the pH to 5, heat to 40°C, add ammonium persulfate dropwise React with sodium bisulfite for 1 hour; add 5% V-50 (V / V) 5ml dropwise, react for 1 hour; heat to 50°C, add 5% V-50 (V / V) 5ml dropwise, react for 2 hours; heat to 70°C, react for 5h.

[0057] Step S102: The steps are the same as in Example 1, with a product quality of 9.5 g and a molecular weight of 25,000.

[0058] FT-IR (KBr), ν / cm -1 : 2937 (C-H stretching vibration), 1642, 1132 (C-N bond stretching vibration), 1476 (saturated C-H in-plane bending vibration), 946 (C-H bond bending stretching vibration).

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Abstract

The invention belongs to the technical field of chemical products and preparation therefore, and specifically relates to preparation and applications of a cationic poly(quaternary ammonium salt) vanadium doped heteropolyacid supramolecular system. In the supramolecular system, poly(quaternary ammonium salt) cation is a homopolymer with a linear structure, and the homopolymer is prepared through free radical polymerization of dimethyl diallyl ammonium chloride monomers. The matched heteropolyacid anion is Dawson type vanadium doped P2Mo17VO62<-7>, P2Mo16VO62<-8>, and P2Mo15VO62<-9>. The supramolecular system is a heterogeneous catalyst, industrial hydrogen peroxide with a mass percentage of 3 to 5% is used as an oxidant, and cyclic ketone is oxidized to synthesize omega-dicarboxylic acid through one-step ring opening in the absence of solvent. The omega-dicarboxylic acid preparation method has the advantages of high catalytic activity, good selectivity, wide substrate range, friendly synthesis technology environment, mild operation conditions, large elasticity, and high product purity, and the catalytic system is reusable.

Description

technical field [0001] The invention belongs to the technical field of chemical products and their preparation, and specifically relates to the preparation and application of a cationic polyquaternary ammonium vanadium-doped heteropolyacid supramolecular system. Background technique [0002] ω-dicarboxylic acid is a dicarboxylic acid with two carboxyl functional groups at both ends of the carbon chain. As an important class of high value-added refined products, it is widely used and has a huge market demand. For example, 1,6-adipic acid, also known as fatty acid, is a dicarboxylic acid with a global annual consumption of tens of millions of tons. It is widely used in the chemical industry to produce nylon-66, engineering plastics, polyurethane foam, Plasticizers, food additives, spices, pharmaceutical intermediates, adhesives and dyes, etc. The safety of 1,6-adipic acid is similar to that of citric acid and tartaric acid, and it is not easy to absorb moisture, so it can kee...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/18C07C51/285C07C55/10C07C55/12C07C55/14C07C55/16C07C55/18C07C55/20C07C55/02C08F126/02
CPCB01J27/199B01J31/0239B01J2231/70C07C51/285C08F126/02C07C55/10C07C55/12C07C55/14C07C55/16C07C55/18C07C55/20C07C55/02
Inventor 李心忠
Owner MINJIANG UNIV
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