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Method for preparing active carbon carrying precious metal catalyst

A precious metal catalyst, activated carbon technology, applied in metal/metal oxide/metal hydroxide catalysts, chemical instruments and methods, physical/chemical process catalysts, etc. See the reports on the industrialization of catalyzed synthesis of DSD acid, and the reports on no catalyst preparation methods, etc., to achieve the effects of avoiding human damage, low equipment requirements, and high selectivity

Inactive Publication Date: 2012-09-12
杭州凯大催化金属材料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The patent [CN102205248A, 2011] of Hebei Huage Chemical Group Co., Ltd. reported a method for preparing a highly selective DSD hydrogenation catalyst. However, in the preparation process of this patent, the carrier activated carbon needs to be treated with acid and alkali, and a co-catalyst Fe needs to be added. The preparation process is complicated, and formaldehyde is used as the reducing agent in the reduction process, which will pollute the environment and cause damage to the human body
[0006] In summary, the methods of various patents and literature reports have their own defects, some are poor in selectivity, some are not friendly to the environment, and some do not report in detail on the catalyst preparation method. At the same time, product quality such as benzyl, chroma, Aldehyde by-products and other indicators are far from reaching the quality requirements of the national standard HG / T2279-2000 for DSD acid, so there has been no report on the industrialization of catalytic synthesis of DSD acid

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] The pretreatment process of the activated carbon carrier is as follows: 100-300 mesh coconut shell carbon is used as the activated carbon carrier, and the specific surface area of ​​the activated carbon is 1100m 2 / g, ash content 2.0%. Weigh 100g of coconut shell charcoal, add 1000g of 5.0% EDTA disodium salt solution, stir at 50°C for 3h, then filter with suction, keep the filtrate for use, wash the filter cake with 1000g of deionized water, and dry at 110°C for 8h to obtain the prepared 98.3 g of activated carbon carrier after treatment.

[0031] The preparation process of the catalyst is as follows: take 9.7 g of the above-mentioned pretreated activated carbon carrier, add 50 g of deionized water, stir to form a carbon slurry, and then add 26.8% mass concentration of chloroplatinic acid hexahydrate (H 2 PtCl 6 ·6H 2 O, Pt content: 37.5%) aqueous solution 3.0g, stirred at 60°C for 6h, continued to maintain the temperature at 60°C, added NaOH aqueous solution with a...

Embodiment 2

[0034] Activated carbon carrier pretreatment process is the same as embodiment 1, but activated carbon is changed into wood charcoal, specific surface area is 900m 2 / g, ash content 2.5%, filtrate 910ml is subsequent use, obtains wood activated carbon carrier 97.5g.

[0035] The catalyst preparation process is as follows: take 9.8 g of the above-mentioned pretreated activated carbon carrier, add 50 g of deionized water, stir to form a carbon slurry, and then add 13.4% mass concentration of chloroplatinic acid hexahydrate (H 2 PtCl 6 ·6H 2 O, Pt content: 37.5%) aqueous solution 4.0g, stirred at 30°C for 4h, then heated to 60°C, added Na with a mass concentration of 10% 2 CO 3 Adjust the pH value of the reaction solution to 7.0 with an aqueous solution, keep stirring for 2 hours, then suction filter, and wash the filter cake with deionized water until the washing solution is substantially free of Cl - ions (detected by silver nitrate solution), then added to 30g of deionized...

Embodiment 3

[0038] The catalyst preparation process is as follows: get 9.7g of pretreated activated carbon carrier in Example 1, add 90g of deionized water, stir into carbon slurry, then add mass concentration 26.8% chloroplatinic acid hexahydrate (H 2 PtCl 6 ·6H 2 O, Pt content: 37.5%) aqueous solution 3.0g, stirred at 60°C for 6h, continued to maintain the temperature at 60°C, and added NaHCO with a mass concentration of 10% 3 Adjust the pH value of the reaction solution to 6.0 with the aqueous solution, keep stirring for 1 hour, then cool down to 40°C, add 10 g of hydrazine hydrate aqueous solution with a mass concentration of 10%, and keep stirring for 2 hours. After the reaction, the slurry is suction filtered once to obtain a filter cake. The filter cake is washed with deionized water until the washing liquid is basically free of Cl - ions (detected by silver nitrate solution), and filtered again for 15 minutes to obtain a secondary filter cake, namely 21.0 g of Pt / C catalyst (the...

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Abstract

The invention discloses a method for preparing an active carbon carrying precious metal catalyst. The method comprises the following steps of: immersing an active carbon carrier into an ethylene diamine tetraacetic acid disodium salt (EDTA disodium salt for short) aqueous solution for pretreatment; then mixing the pretreated active carbon carrier and water to prepare carbon slurry; adding a nitrate solution or chlorate aqueous solution which contains precious metal into the carbon slurry, and stirring at the temperature between 25 and 90 DEG C for 2 to 6 hours; adding an alkaline aqueous solution under the condition of the temperature between 25 and 80 DEG C, adjusting the pH value of the reaction solution until the pH value is 6 to 9; stirring at the constant temperature between 25 and 80 DEG C for 0.5 to 4 hours, thus obtaining slurry; and post-treating the slurry, thus obtaining the active carbon carrying precious metal catalyst. According to the method, acid and alkaline are not used during pretreatment of the active carbon carrier, so that environment friendliness is realized; during preparation of the catalyst, any auxiliary catalyst is not added, so that the cost is saved, and the process is simplified; the preparation process is simple in condition; the requirement on equipment is low; and industrialization is facilitated.

Description

(1) Technical field [0001] The invention relates to an activated carbon treatment method and a preparation method of a loaded noble metal catalyst, in particular to an activated carbon loaded noble metal catalyst for catalytic hydrogenation synthesis of 4,4'-diaminostilbene-2,2'-disulfonic acid (DSD acid) method of preparation. (2) Background technology [0002] 4,4'-diaminostilbene-2,2'-disulfonic acid (DSD acid) is a widely used organic compound. There are more than 100 kinds of fluorescent whitening agents based on DSD acid. Five reactive dyes There are more than ten kinds, and more than 70 kinds of direct dyes. The dyes synthesized by DSD acid are used as the substitute of benzidine dyes. Because they are non-toxic and have no accumulation in the human body, they have attracted more and more attention and developed rapidly. [0003] At present, the production of DSD acid worldwide adopts the process of reducing 4,4'-dinitrostilbene-2,2'-disulfonic acid disodium salt (DN...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/52B01J23/46B01J23/44B01J23/42C07C309/46C07C303/22
Inventor 国海光张军华郇昌永李树贵沈强林桂燕姚洪
Owner 杭州凯大催化金属材料股份有限公司
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