Modified palladium-carbon catalyst, preparation method and applications thereof

A palladium-carbon catalyst and modifier technology, which is applied in the field of modified palladium-carbon catalysts, can solve problems such as difficult industrialization, low efficiency, and inability to apply industrial production, and achieve the effects of improving stability and reducing use costs

Active Publication Date: 2019-12-31
方晓亮
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For example, JP0413644A discloses the preparation of 1,3-cyclohexanedione by catalytic hydrogenation with metal catalysts (Pt, Pd, Rh, Ru) through the neutralization of butanediamine with resorcinol as raw material, and the conversion rate is as high as 99%. Above, but the selectivity is only 79.6% and organic bases are used, which are expensive and cannot be used in industrial production
[0007] CN106083545A reported the preparation of 1,3-cyclohexanedione with platinum carbon as a catalyst. After the inorganic alkali treatment, it reacted for more than 5h at 95-105°C. The reaction time was long, the reaction rate was slow, the efficiency was low, and the yield was only 93%; CN108623443A discloses a method for preparing 1,3-cyclohexanedione by gas-phase hydrogenation of resorcinol, dissolving resorcinol in benzene and directly vaporizing it and mixing it with hydrogen, the reaction temperature is 180-280°C, Reaction pressure is 1.0~2.0MPa, although yield and selectivity are all very high, organic benzene solvent is unfriendly to environment, and needs very high vaporization temperature; CN105111058A is catalyst with lanthanum chloride, palladium dichloride, under pressure The value is 4-7.5MPa, the heating temperature is 115-145°C, the cond

Method used

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  • Modified palladium-carbon catalyst, preparation method and applications thereof
  • Modified palladium-carbon catalyst, preparation method and applications thereof
  • Modified palladium-carbon catalyst, preparation method and applications thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0059] According to the synthesis method provided by the present invention, 3% Pd / C and PAA are dispersed in methanol, wherein the mass ratio of Pd to PAA is 20:1, and after 8 hours of ultrasonic stirring at room temperature, the modified palladium carbon catalyst is obtained by suction filtration , and washed 3 to 5 times with ultrapure water; put 11.0 g of the substrate 11.0 g of resorcinol alkalized by sodium hydroxide and 120 mL of ultrapure water in a 500-mL reactor, and add 1.0 g of modified palladium Carbon catalyst (wet product, water content 60%, the molar ratio of substrate to Pd is about 830:1), the air in the reaction is replaced with hydrogen for 3 times, and the test is carried out at 60-80°C and 1.2-1.8MPa . The experimental data are shown in Table 1.

[0060] Table 1 prepares the result of 1,3-cyclohexanedione by the method described in Example 1 of the present invention under different reaction conditions

[0061]

[0062] The results of Example 1 show th...

Embodiment 2

[0064] According to the synthesis method provided by the present invention, 3% Pd / C and PVA are dispersed in ethanol, wherein the mass ratio of Pd to PVA is 10:1, and after ultrasonic stirring at room temperature for 6 hours, suction filtration obtains the modified palladium carbon catalyst , and washed 3 to 5 times with ultrapure water; put 11.0 g of the substrate 11.0 g of resorcinol alkalized by sodium hydroxide and 120 mL of ultrapure water in a 500-mL reactor, and add 1.0 g of modified palladium Carbon catalyst (wet product, water content 60%, substrate to Pd molar ratio is about 830:1), replace the air in the reaction with hydrogen for 3 times, test at 80°C and 1.8MPa, and react when applied mechanically Same conditions. The experimental data are shown in Table 2.

[0065] Table 2 prepares the result of 1,3-cyclohexanedione by the method described in the embodiment of the present invention 2

[0066]

[0067] The result of embodiment 2 shows that the 3%Pd / C of PVA m...

Embodiment 3

[0069] According to the synthesis method provided by the present invention, 3% Pd / C and different quality SDBS are dispersed in DMF, and after ultrasonic stirring at room temperature for 10 hours, the modified palladium carbon catalyst is obtained by suction filtration, and washed with ultrapure water for 3- 5 times; 11.0 g of the substrate 11.0 g of resorcinol alkalized by sodium hydroxide and 120 mL of ultrapure water were placed in a 500-mL reaction kettle, and 1.0 g of modified palladium carbon catalyst (wet product, water content 60 %, the substrate to Pd molar ratio is about 830:1), the air in the reaction is replaced with hydrogen 3 times, and the test is carried out at 80°C and 1.8MPa, and the reaction conditions are the same when applied mechanically. The experimental data are shown in Table 3.

[0070] Table 3 prepares the result of 13-cyclohexanedione by the method described in the embodiment of the present invention 3

[0071]

[0072] The results of Example 3 ...

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Abstract

The invention provides a modified palladium-carbon catalyst, which comprises: a supported palladium-carbon material; and a modifier located on the surface of the supported palladium-carbon material, wherein the modifier at least comprises one selected from polyvinyl alcohol (PVA), an acrylic resin (PAA), sodium triphenylphosphine monosulfonate, polyvinylpyrrolidone (PVP) and sodium dodecyl benzenesulfonate (SDBS). The modified palladium-carbon catalyst provided by the invention is good in stability, can be applied to a method for synthesizing 1,3-cyclohexanedione multiple times, and has highselectivity.

Description

technical field [0001] The present invention relates to a modified palladium carbon catalyst, in particular to a method for preparing the modified palladium carbon catalyst and a method for using it to synthesize 1,3-cyclohexanedione. Background technique [0002] 1,3-cyclohexanedione has a lively β-dicarbonyl structure and is an important chemical intermediate, which is an important intermediate for many pesticides, medicines and cosmetics. [0003] At present, there are two methods for synthesizing 1,3-cyclohexanedione. One is to synthesize 1,3-cyclohexanedione by condensation using γ-acetylbutyrate as raw material and sodium methoxide as a condensing agent as described in the patent US3922307 , but its raw material γ-acetobutyrate is difficult to prepare, and sodium alkoxide is expensive, and post-processing is difficult, so it is not suitable for large-scale production. [0004] Another method is the catalytic hydrogenation method, which is currently the most commonly u...

Claims

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Application Information

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IPC IPC(8): B01J31/06B01J31/02C07C45/00C07C49/403
CPCB01J31/0225B01J31/06B01J2231/646C07C45/006C07C2601/14C07C49/403
Inventor 郑南峰李志恺刘圣杰陈洁
Owner 方晓亮
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