Polyacid supramolecular crystal material and preparation method thereof

A technique for supramolecular crystals and heteropolyacid salts, applied in the field of polyacid supramolecular crystal materials and their preparation, can solve the problems of difficult to control production, difficult to control reaction rate, difficult to obtain crystals, etc.

Inactive Publication Date: 2019-11-22
XINJIANG AGRI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the extremely fast reaction rate of the two salts in the same solution, it is difficult to obtain crystals. Therefore, the prior art generally has the problem that the reaction rate is difficult to control and it is difficult to control the production of larger single crystals.

Method used

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  • Polyacid supramolecular crystal material and preparation method thereof
  • Polyacid supramolecular crystal material and preparation method thereof
  • Polyacid supramolecular crystal material and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0023] Embodiment 1 heteropolyacid salt (NH 4 ) 3 [CrMo 6 o 24 h 6 ]·7H 2 O synthesis process

[0024] (1) Weigh 3.100g of chromium sulfate, 5.012g of ammonium molybdate and heat the 80mL aqueous solution of ammonium molybdate to boiling (oil bath heating 140°C);

[0025] (2) 20mL aqueous solution of chromium sulfate is added thereto, and the solution becomes blue-black;

[0026] (3) Cool the solution to room temperature, then evaporate in a water bath until a large amount of purple substance is precipitated, and a small amount of liquid remains in the solution (about two hours);

[0027] (4) After filtering the remaining hot solution while hot, get the filtrate and seal it with a film to prevent pollution;

[0028] (5) The filtrate was allowed to stand for 1 to 2 days, and a small amount of liquid remained, which was filtered and dried to obtain product 1, and the weight of the yield was 3.286 g. And this product 1 carries out infrared spectrogram analysis, consistent...

Embodiment 2

[0029] Embodiment 2 (DABCO 2HBF 4 ) synthesis of salt

[0030] Weigh 0.500g of DABCO and dissolve it with 10mL of methanol, then weigh 1.9568g of 40% tetrafluoroboric acid and dissolve it with 10mL of methanol, drop the latter into the former solution and immediately generate a white substance, seal it with a paper towel and a rubber band, After the solvent was evaporated to dryness, the product 2 was obtained. Product 2 is carried out infrared spectrogram analysis, the result is as follows figure 1 As shown, through its infrared spectrogram analysis, it can be known that the materials required for the synthesis of raw materials all exist, and it is determined that the product 2 is the target raw material (DABCO 2HBF 4 )Salt.

Embodiment 3

[0031] The synthesis of embodiment 3 polyacid supramolecular crystal material

[0032] Weigh separately (NH 4 ) 3 [CrMo 6 o 24 h 6 ]·7H 2 O and (DABCO·2HBF 4 ) salt 0.020g and 0.005g, and dissolve them with 50mL of deionized water respectively. All controlled in the beaker of the solution to be replenished (such as figure 2 As shown), after the solution in the dripping bottle has been dripped for one day, use the same method to replenish the solution again, but when replenishing the solution for the second time, first absorb part of the solution in the beaker with a dropper, and the remaining solution in the beaker is about 50mL. After 5 days it was processed to afford 1 as purple rod-shaped crystals.

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Abstract

The invention discloses a polyacid supramolecular crystal material and a preparation method thereof. The preparation method comprises the following steps of (1) dropwise adding 50mL of a solution A and 50mL of a solution B into a beaker at a speed of 29-31 seconds/drop at the same time, wherein 50 mL of the solution A contains 0.020 g of a heteropolyacid salt (NH4) 3 [CrMo6O24H6].7H2O, and 50 mL of the solution B contains 0.005 g of a (DABCO.2HBF4) salt; and (2) sucking 50mL of solution in the beaker after finishing dropping, repeating the step (1), and standing for 5 days to obtain the purplerodlike polyacid supramolecular crystal material. According to the invention, a better crystal material is grown by a double-component dropping method, and meanwhile, different quantities of crystalscan be obtained by controlling the dropping speed, and even a nanoscale crystal material can be prepared; the polyacid supramolecular crystal material prepared by the method can be widely applied tothe aspects of information storage materials, dielectric materials, polyacid catalytic materials, novel electrode materials, energy storage materials and the like.

Description

technical field [0001] The invention belongs to the technical field of inorganic synthesis, and in particular relates to a polyacid supramolecular crystal material and a preparation method thereof. Background technique [0002] In recent years, Anderson-type polyoxometalates have shown good application prospects in the fields of electrochemistry, photocatalysis, and magnetism, and have attracted extensive discussion by researchers. Anderson-type polyoxometalates are nanometer-sized metal oxygen clusters that can be combined with organic molecules to construct novel hybrid materials. At present, the most researched and developed heteropolyacids can be divided into two categories: molybdenum-based and tungsten-based. Because the reaction rate of the two salts in the same solution is extremely fast, it is difficult to obtain crystals. Therefore, the prior art generally has the problem that the reaction rate is difficult to control and it is difficult to control the production ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G83/00
CPCC08G83/008
Inventor 刘尊奇刘洋朱春立
Owner XINJIANG AGRI UNIV
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