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Method for recovering heteropoly acid from deactivated supported type heteropoly acid catalyst

A heteropolyacid and catalyst technology, which is applied in chemical recovery, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of undisclosed heteropolyacid recovery and purity, and achieve high purity, single structure, and high yield. high rate effect

Active Publication Date: 2010-12-22
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The patent also does not disclose the recovery and purity data of heteropolyacids

Method used

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  • Method for recovering heteropoly acid from deactivated supported type heteropoly acid catalyst
  • Method for recovering heteropoly acid from deactivated supported type heteropoly acid catalyst
  • Method for recovering heteropoly acid from deactivated supported type heteropoly acid catalyst

Examples

Experimental program
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Effect test

Embodiment 1

[0042] Take by weighing 20 grams of deactivated supported phosphotungstic acid catalyst in the alkylation reaction of isobutane and butene, the active component of this catalyst is H 3 PW 12 o 40 , the carrier is silicon oxide SiO 2 , 25% by weight of phosphorus-containing tungstic acid, adding this catalyst and the concentration of equal volume in the crucible is 35% by weight of HClO 4 25.1 grams of aqueous solution makes the catalyst just wet completely, makes HClO 4 The amount of the catalyst is 44% of the dry weight of the catalyst. After standing for 0.5h, the above system is put into a muffle furnace and burned for 1h (air atmosphere) at 230°C. After cooling, the catalyst treated in this way is put into an Erlenmeyer flask , add 40g of water, fully stir on a magnetic stirrer, control the temperature of the system at 25°C, and process for 1 hour. Suction filtration to remove the carrier; at 55°C, depressurize to 15.75×10 3 Under the condition of Pa, the solution is ...

Embodiment 2

[0052] The deactivated loaded phosphotungstic acid catalyst is the same as that in Example 1, with an amount of 50 grams. In crucible, add this catalyst and 16.3g concentration respectively and be the HClO of 15% by weight 4 solution, and 15.0 g of HNO at a concentration of 15% by weight 3 solution, stirred evenly and left for 0.5h, put the above system into a muffle furnace and burn at 120°C for 3h (oxygen atmosphere), take it out and add 16.3g of HClO with a concentration of 15% by weight in the catalyst after cooling 4 solution and 15.0 g of HNO at a concentration of 15% by weight 3 solution, placed in a muffle furnace for 30 minutes and then burned at 120°C for 3h (oxygen atmosphere), the catalyst treated in this way was put into a conical flask, 50g of methanol was added, fully stirred, and the temperature of the control system was 50 °C, reflux for 5 hours. Then suction filtration to remove the carrier, distill methanol at 85°C to obtain a distillate containing hetero...

Embodiment 3

[0054] Weigh 2 grams of supported heteropolyacid catalyst deactivated in the alkylation reaction of isobutane and butene, the active component of the catalyst is phosphotungstic acid H 3 PW 12 o 40 , the content is 25% by weight, and the carrier is a silica-alumina mixture, namely SiO 2 -Al 2 o 3 . Add this catalyst and 2g concentration in crucible and be the HNO of 40% by weight3 Aqueous solution, stirred evenly and left for 0.5h, put the above system into a muffle furnace and burn at 175°C for 2.5h (oxygen atmosphere), repeat 3 times. After taking out and cooling, put the catalyst into an Erlenmeyer flask, add 20 g of methanol, fully stir on a magnetic stirrer, control the temperature of the system at 10° C., and process for 24 hours. Then the carrier is removed by suction filtration, methanol is steamed out at 85°C to obtain a residue containing heteropolyacid; add 6g of water to dissolve the residue of heteropolyacid, then add 2 grams of 65% by weight nitric acid and ...

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Abstract

The invention provides a method for recovering an active component heteropoly acid from an inactive supported heteropoly acid catalyst, which comprises the steps as follows: (1) a catalyst to be processed contacts with an oxidizer-containing water solution; (2) the above-mentioned system is processed in an oxygen-containing atmosphere; (3) the processed heteropoly acid catalyst is dissolved in water or an organic polar solvent, and a heteropoly acid solution A and a heteropoly acid solution B are obtained respectilvey after a carrier is separated out; (4) the organic polar solvent is separated from the heteropoly acid solution B; remainders are dissolved in water to obtain a heteropoly acid solution C; and (5) the heteropoly acid solution A or the heteropoly acid solution C contacts with an inorganic acid to lead the heteropoly acid to be purified and precipitated, and a heteropoly acid crystal is obtained through filtration and drying. Compared with the prior art, the method has simple flow and is suitable for the application in a large-scale industry, and the coefficient of recovery can reach about 95 percent; the recovered heteropoly acid has high purity quotient, and can satisfy the requirement for preparing a novel supported catalyst.

Description

technical field [0001] The present invention relates to a kind of method of reclaiming heteropolyacid, more specifically, the present invention relates to a kind of method of reclaiming heteropolyacid from deactivated load-type heteropolyacid catalyst. Background technique [0002] Heteropolyacid is a kind of acid with cage structure and pores obtained by acidification, condensation and dehydration of two or more inorganic oxoacid ions. This type of heteropolyacid has both strong acidity and oxidation Reducing, so it can be used as an acid catalyst, but also as a redox catalyst. The heteropolyacid is evenly supported on a carrier, such as silicon oxide, aluminum oxide, silicon oxide-alumina mixture or activated carbon, to obtain a supported heteropolyacid catalyst. This supported heteropolyacid catalyst can be used in hydrocarbon conversion reactions requiring strong acidic catalysts, such as alkylation reactions, olefin hydration, aldehyde oxidation reactions, etherificati...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G39/00C01G41/00B01J23/28B01J23/30
CPCY02P20/584
Inventor 杜勇何奕工
Owner CHINA PETROLEUM & CHEM CORP