Preparation of immobilization molybdate catalyst

A catalyst and molybdate technology, which is applied in the field of preparation of immobilized molybdate catalysts, can solve the problems of high cost, activity loss, and small interaction force, and achieve the effect of good mechanical strength and low loss of molybdenum

Inactive Publication Date: 2008-07-09
广西南宁化学制药有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The interaction force between the carrier and the catalytic active substance is small, and it is easy to cause loss of activity during the catalytic process, making the empty shell of the carrier inactive
Perlite, activated carbon, etc. cannot forcefully adsorb chitosan, so they are not suitable for composite carriers
The use of macroporous absorbent resin can adsorb molybdate, because it is not resistant to high temperature and low pH value, molybdate is easy to deactivate the original activity, the carrier used to adsorb molybdate, the cost is still high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] In 650 milliliters of 1.0% (V / V) acetic acid solution, add 5.0 g of chitosan and stir to dissolve at 60 ° C, add 3.0 g of diatomaceous earth and stir evenly, add 5 mol / l sodium hydroxide solution to adjust the pH value to 10, filter, Wash the precipitate until the pH value reaches 9.0, dry it in vacuum at 90°C for 3 hours, crush the dry matter and add it to 250 ml of 85°C, 75% (V / V) ethanol, and add 0.1% (W / W) molybdic acid at the same time 20 ml of ammonium solution was refluxed for 2 hours and filtered to obtain 6.0 g of milky white catalyst. The obtained catalyst is used to isomerize 45% glucose aqueous solution, and the isomerization rate is 35%. After 10 consecutive isomerizations, the catalyst still maintains 87% isomerization activity.

Embodiment 2

[0026] Add 7.5g chitosan to 550ml 3% (V / V) acetic acid solution and stir to dissolve at 40°C, then add 4.5g diatomaceous earth and stir evenly, then add 4.0mol / l sodium hydroxide solution to adjust the pH value to 12.5 , filter, wash the precipitate to a pH value of 7.5, dry it under vacuum at 90°C for 1 hour, crush the dry matter and add it to 350 ml of 90°C, 80% (V / V) ethanol, while adding 0.35% (W / W) 20 ml of ammonium molybdate solution was refluxed for 3 hours and filtered to obtain 8.8 g of milky white catalyst. The obtained catalyst is used to isomerize 50% glucose aqueous solution, and the isomerization rate is 32%. After 10 consecutive isomerizations, the catalyst still maintains 85% isomerization activity.

Embodiment 3

[0028] Add 10.0 g of chitosan to 950 ml of 2.5% (V / V) acetic acid solution and stir to dissolve at 50 ° C, then add 7.0 g of silica gel and stir evenly, then add 4.5 mol / l sodium hydroxide solution to adjust the pH value to 12, filter , wash the precipitate until the pH value reaches 8.0, dry it in vacuum at 85°C for 3 hours, crush the dry matter and add it to 400 ml of 85°C, 85% (V / V) ethanol, and add 0.25% (W / W) molybdic acid at the same time 20 ml of ammonium solution was refluxed for 2.5 hours, filtered to obtain 14 g of milky white catalyst. The obtained catalyst is used to isomerize 45% glucose aqueous solution, and the isomerization rate is 35%. After 10 consecutive isomerizations, the catalyst still maintains 88% isomerization activity.

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Abstract

The invention relates to a method of preparing a solid molyadate catalyst. Ammonium paramolybdate, i.e. (NH4)6MoO24.4H2O is taken as the active component of the catalyst, and then fixed on a compound carrier which is formed by that silica gel or sillitin forcibly absorbs chitosan. 0.1 percent to 0.5 percent (NH4)6MoO24.4H2O water solution is taken to react with particles of the compound carrier in 70 DEG C to 90 DEG C ethyl alcohol under 70 DEG C to 85 DEG C (V / V) temperature for 1 to 4 hours, which is dried to prepare the solid catalyst with high activity. The prepared solid molyadate catalyst is used for isomeric 50 percent (W / W) glucose solution, which is reusable for at least 10 times, with the activity still above 80percent.

Description

(1) Technical field [0001] The invention relates to the technical field of fine chemicals, in particular to a preparation method of an immobilized molybdate catalyst. (2) Background technology [0002] D~mannitol, molecular weight 182.17, white needle-like crystal or crystalline powder, odorless and sweet. Density 1.489g / cm 3 . Melting point 166~170℃, boiling point 290~295℃ (15.7×10 3 Pa). Optical rotation +23~+24 degrees, non-deliquescence, easily soluble in hot water, hot ethanol, dilute acid, dilute solution, hardly soluble in cold ethanol, insoluble in ether. Appropriate sweetness, low calories, no toxic side effects, metabolism in the human body has nothing to do with insulin, does not increase blood sugar level, does not cause dental caries, can be used as one of the sweeteners for special patients such as diabetes and obesity, and can also be used in food industries such as chewing gum superior. The solubility in water increases with the increase of temperature;...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/28B01J31/06B01J21/08C07C31/26C07C29/56
Inventor 米运宏韦振雷梁智徐斌元邓梁华韦海涛陈星河黄静茹志华
Owner 广西南宁化学制药有限责任公司
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