Sulfur carbon ball loaded precious metal catalyst and preparation method and application thereof

A noble metal catalyst and catalyst technology, which are applied in the preparation of amino compounds, chemical instruments and methods, preparation of organic compounds, etc., can solve the problem of the instability of carbon-supported noble metal catalysts, the unsatisfactory effect of doping sulfur, and the need to improve the selectivity, etc. problems, to achieve the effect of improving metal utilization, improving material mass transfer efficiency, and high stability

Inactive Publication Date: 2019-04-26
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there are inevitably differences in the properties of activated carbon produced by different manufacturers, different materials and different batches, resulting in the instability of the preparation process of carbon-supported noble metal catalysts.
[0004] 2) Selectivity needs to be improved
For the surface modification of the support, the method of doping a large number of basic groups such as S is often to combine the support and sulfur-containing compounds such as H 2 S, elemental S, etc. are roasted at high temperature. The experimental steps of this method are complicated, and it is not easy to control the formation of specific surface sulfur-containing groups; for the m

Method used

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  • Sulfur carbon ball loaded precious metal catalyst and preparation method and application thereof
  • Sulfur carbon ball loaded precious metal catalyst and preparation method and application thereof
  • Sulfur carbon ball loaded precious metal catalyst and preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0048] Take 100ml of deionized water in a three-necked flask, install a condensation reflux device in one port, and seal the other two ports with glass stoppers; then add 0.5g cetyltrimethylammonium bromide and 1.5g cysteine ​​solid, set The temperature of the water bath was 30°C, and magnetic stirring was started for 1 h until the solid was completely dissolved. Subsequently, add 5 g of 4,4'-thiodisalicylic acid thiophenol solid, continue to stir for 0.5 h until the solid is completely dissolved, then open one of the glass stoppers, and slowly add 2 ml of concentrated H 2 SO 4 The solution is in the above mixed solution, and the rate of addition is strictly controlled to prevent the temperature rise caused by the heat of dissolution from exceeding 2°C. Continue magnetic stirring, from room temperature to 60°C at a heating rate of 0.1°C / min, keep for 6h, then continue to rise to 90°C at a heating rate of 0.1°C / min, keep for 6h, and finally continue to rise to boiling at a hea...

Embodiment 2

[0052] Take 100ml of deionized water in a three-necked flask, install a condensation reflux device in one port, and seal the other two ports with glass stoppers; then add 1g of cetyltrimethylammonium bromide and 2g of cysteine ​​solid, and set the temperature of the water bath At 30°C, start magnetic stirring for 1 h until the solid is completely dissolved. Subsequently, 8 g of 4,4'-thiodisalicylic acid thiophenol solid was added, and stirring was continued for 0.5 h until the solid was completely dissolved, then one of the glass stoppers was opened, and 2 ml of concentrated H 2 SO 4 The solution is in the above mixed solution, and the rate of addition is strictly controlled to prevent the temperature rise caused by the heat of dissolution from exceeding 2°C. Continue magnetic stirring, from room temperature to 60°C at a heating rate of 0.1°C / min, keep for 8h, then continue to rise to 90°C at a heating rate of 0.1°C / min, keep for 8h, and finally continue to rise at a heating ...

Embodiment 3

[0056]Take 100ml of deionized water in a three-necked flask, install a condensation reflux device in one port, and seal the other two ports with glass stoppers; then add 1g of cetyltrimethylammonium bromide and 2g of cysteine ​​solid, and set the temperature of the water bath At 30°C, start magnetic stirring for 1 h until the solid is completely dissolved. Subsequently, add 10 g of 4,4'-thiodisalicylic acid thiophenol solid, continue to stir for 0.5 h until the solid is completely dissolved, then open one of the glass stoppers, and slowly add 2 ml of concentrated H 2 SO 4 The solution is in the above mixed solution, and the rate of addition is strictly controlled to prevent the temperature rise caused by the heat of dissolution from exceeding 2°C. Continue magnetic stirring, raise the temperature from room temperature to 60°C at a rate of 1°C / min, keep for 12 hours, then continue to increase the rate of temperature at 1°C / min to 90°C, keep for 12 hours, and finally continue t...

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Abstract

The invention discloses a sulfur carbon ball loaded precious metal catalyst and a preparation method and application thereof. The catalyst is prepared from a sulfur carbon ball and an active componentloaded on the surface of the sulfur carbon ball; elemental sulphur of the sulfur carbon ball exists on a skeleton and the surface of the sulfur carbon ball in a C-S bond form, wherein the mass ratioof the elemental sulfur to elemental carbon is 0.05-20%; the active component is platinum family metal particles, and the particle size of the platinum family metal particles is 4-10 nm; and the sulfur carbon ball loaded precious metal catalyst is spherical, and the diameter of the sulfur carbon ball loaded precious metal catalyst is 100-1000 nm. The invention provides application of the catalystto a C=N bond selective catalytic hydrogenation reduction reaction. The sulfur carbon ball is synthetized through 4,4'-thiobis-thiophenol self-polymerization in-situ sulfur doping, thus the elementalsulphur exists on the skeleton and the surface of the sulfur carbon ball in the C-S bond form, and the metal dispersity and the outer-layer electron distribution characteristic of the modulated metalparticles can be effectively improved; and the catalyst is applied to the C=N bond selective catalytic hydrogenation reaction, and represents the advantages of high conversion rate, catalytic activity, stability and reaction rate.

Description

(1) Technical field [0001] The invention relates to a sulfur-carbon sphere-supported noble metal catalyst and its preparation method and application, in particular to the application of the catalyst in C=N bond selective hydrogenation reaction. (2) Technical background [0002] Platinum group metals have shown excellent catalytic performance in many chemical reactions, such as carbonyl addition reaction, acid chloride addition reaction, olefin oxidation reaction, and C-C synthesis reaction in homogeneous catalytic reactions. The heterogeneous catalysts mainly include petroleum reforming Pt -Re / Al 2 o 3 Catalyst, automobile exhaust purification Pt-Rh / Al 2 o 3 Catalyst, Pd / C catalyst for hydrogenation of terephthalic acid purification, Pd / C catalyst for catalytic hydrogenation of chloronitrobenzene. However, there are still several problems to be solved in the selective hydrogenation reduction reaction. [0003] 1) Efficient utilization of metals. Platinum group metals e...

Claims

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Application Information

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IPC IPC(8): B01J27/045B01J35/08C07C209/52C07C211/55
CPCB01J27/045B01J35/08C07C209/52C07C249/02C07C251/24C07C211/55
Inventor 卢春山季豪克王昊张雪洁周烨彬朱倩文李小年
Owner ZHEJIANG UNIV OF TECH
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