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Pd/C catalyst for preparing alcohol ether carboxylate and production method and use thereof

A technology of alcohol ether carboxylate and catalyst is applied in the field of modified palladium/carbon catalyst and preparation, and achieves the effects of high selectivity, improved yield and good catalytic activity

Active Publication Date: 2009-02-04
SHANGHAI FINE CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] Adding alkaline earth metals and transition metals to Pd / C catalysts as auxiliary components to improve catalyst performance has not been reported

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Take by weighing 0.25g palladium chloride, dissolve and make solution with 10ml 5wt% HCl, take by weighing 4.85g gac (particle diameter is 200nm, specific surface area 1300m 2 / g), add 40ml deionized water, after stirring evenly, slowly drop in the metal chloride solution, stir for 4h, then adjust the pH value to pH=12 with 5wt% NaOH solution, then slowly add 10ml of 5wt% formaldehyde solution dropwise, Raise the temperature to 60°C and reduce for 60 minutes, cool down to room temperature and filter, wash the precipitate with deionized water until neutral, filter, and seal it for storage. (The catalyst is composed of Pd 3wt%, activated carbon 97wt%)

[0034] Add AEO to the reactor 9 50g, 200g of deionized water, 3.9g of KOH and 10g of the catalyst prepared above, stirred, heated to 50°C, fed with oxygen, kept the pressure of the reactor at 0.03MPa for 6h, filtered out the catalyst to obtain the product. Analyzed AEC 9 The yield was 68%.

Embodiment 2

[0036] Take by weighing 0.25g palladium chloride, 0.45g strontium chloride dissolves with 6ml 10wt% HCl and is made into solution, takes by weighing 4.70g gac (particle diameter is 400nm, specific surface area 1400m 2 / g), add 60ml of deionized water, stir the metal chloride solution slowly dropwise, stir for 6h, then use 10wt% NaHCO 3 Adjust the pH value of the solution to pH=14, then slowly add 5ml of 10wt% formaldehyde solution dropwise, heat up to 90°C for 20 minutes, cool down to room temperature and filter, wash the precipitate with deionized water until neutral, filter, and seal it for storage. (The catalyst is composed of Pd 3wt%, Sr3wt%, activated carbon 94wt%)

[0037] Add AEO to the reactor 9 50g, 300g of deionized water, 3.8g of KOH and 20g of the catalyst prepared above, stirred, heated to 90°C, fed with oxygen, kept the pressure of the reactor at 0.20MPa for 3h, filtered out the catalyst to obtain the product. Analyzed AEC 9 The yield was 81.%.

Embodiment 3

[0039] Take by weighing 0.25g palladium chloride, 0.61g nickel chloride, dissolve and make solution with 8ml 8wt% HCl, take by weighing 4.70g gac (particle diameter is 300nm, specific surface area 1300m 2 / g), add 50ml deionized water, after stirring evenly, slowly drop in metal chloride solution, stir for 4h, then use 8wt% Na 2 CO 3 Adjust the pH value of the solution to pH=12, then slowly add 7ml of 8wt% formaldehyde solution dropwise, heat up to 70°C for 40 minutes, cool down to room temperature and filter, wash the precipitate with deionized water until neutral, filter, and seal it for storage. (The catalyst is composed of Pd 3wt%, Ni3wt%, activated carbon 94wt%)

[0040] Add AEO to the reactor 6 50g, 250g deionized water, NaHCO 3 4.1 g and 15 g of the above-prepared catalyst were stirred, and the temperature was raised to 70° C., and oxygen was introduced to keep the pressure of the reactor at 0.07 MPa for 5 h, and the catalyst was filtered out to obtain the product. ...

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Abstract

A Pd / C catalyst for preparing alcohol ether carboxylate consists of the following components by weight percentages: 1-10% of palladium, 1-10% of alkaline earth metals, 1-10% of transition metals and 70-97% of active carbon. The Pd / C catalyst has the advantages that alkaline earth metal atoms and transition metal atoms are added to a palladium carbon catalyst, the used amount of the precious metal palladium is reduced, the catalyst property is improved, the catalytic activity is good and selectivity is high, and the catalyst can increase the yield of the alcohol ether carboxylate by 10-20%.

Description

technical field [0001] The invention relates to a Pd / C catalyst, its preparation method and application, in particular to a modified palladium / carbon catalyst, preparation method and application for catalyzing the oxidation of fatty alcohol polyoxyethylene ether to prepare alcohol ether carboxylate. Background technique [0002] Fatty alcohol ether carboxylate (Alcohol Ether Carboxylate, AEC) is an important class of anionic surfactants, and its chemical structure can be expressed as: [0003] R(CH 2 CH 2 O) n OCH 2 COOH acid form [0004] R(CH 2 CH 2 O) n OCH 2 COOM salt type [0005] In the formula, R is an open chain alkyl or cycloalkyl, n is an integer greater than 1, M=Na + 、K + , Li + . Fatty alcohol ether carboxylate is very similar to soap in chemical structure, except that polyoxyethylene group is embedded between hydrophobic group and hydrophilic group. Due to the change in chemical structure, it not only has the incomparable water solubility and Hard...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/44B01J23/89B01J23/63B01J21/18C07C51/23
Inventor 李小秋张望李运玲
Owner SHANGHAI FINE CHEM CO LTD
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