Method for preparing DSD acid
A technology of disulfonic acid and dinitrostilbene is used in the preparation of sulfonic acid, chemical instruments and methods, catalysts for physical/chemical processes, etc., and can solve the problems of difficult post-processing procedures, increased labor costs, and incomplete reaction. , to achieve the effect of low cost, good product quality and high selectivity
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example 1
[0035] Example 1: Catalyst Preparation
[0036] 1.33 g of chloroplatinic acid (H 2 PtCl 6 ·6H 2 O) was dissolved in 2 ml of 10% hydrochloric acid, 0.16 g of copper acetate (Cu(CH 3 COO) 2 ·H 2O) and 0.17 g of zinc acetate (Zn(CH 3 COO) 2 2H 2 O) was dissolved in 10 ml of water, and the two solutions were mixed for later use. Add 120 milliliters of water and 9.4 grams of activated carbon treated with nitric acid into a 250 milliliter four-neck flask (with stirrer, thermometer, condenser and dropping funnel), and add the pre-prepared platinum, For the mixed solution of copper and zinc salt, control the time of dropping for about 1 hour, and continue to stir for 30 minutes after dropping to make it completely penetrate into the activated carbon. Use saturated sodium carbonate solution to adjust the pH value between 7-8, add 2.5 ml of 85% hydrazine hydrate, heat up to 90°C, keep warm for 1 hour, then cool down to 25°C, filter, wash with water until neutral, and suction fi...
example 2
[0039] Dissolve 15 grams of 4,4'-dinitrostilbene-2,2'-sodium disulfonate in 100 milliliters of water, adjust the pH value (with 1% hydrochloric acid, the same below) to 5.5, Pt-Cu-Zn / C catalyst (Pt5%, Cu0.5%, Zn0.5%) 0.1 gram, add in the 250 milliliter autoclave with stirring and built-in condensing tube, replace the gas in the still with nitrogen and hydrogen respectively three times, then hydrogen in the still The pressure was adjusted to 1.0MPa, stirring was started, the temperature was raised by heating, and the reaction temperature was controlled at 50°C to carry out the hydrogenation reaction. After reacting for 60 minutes, the pressure did not drop any more; after another 30 minutes of stirring with heat preservation, the reaction ended. Cool down to 25°C, release the pressure and replace with nitrogen twice, discharge the material, filter out the catalyst for recycling, and obtain 4,4'-diaminostilbene-2,2'-sodium disulfonate solution. Add 30% sulfuric acid to acidify...
example 3
[0043] 30 grams of 4,4'-dinitrostilbene-2,2'-sodium disulfonate were dissolved in 200 milliliters of water, and the pH value was adjusted to 5.5, Pt-Cu-Zn / C catalyst (Pt3%, Cu0.3 %, Zn0.3%) 0.3 g, add in the 500 milliliter autoclave with stirring and built-in condensing tube, replace the gas in the still with nitrogen and hydrogen respectively three times, then adjust the hydrogen pressure in the still to 1.0MPa, start stirring, Heating to raise the temperature, controlling the reaction temperature to 50°C, and carrying out the hydrogenation reaction. After reacting for 60 minutes, the pressure did not drop any more; after another 30 minutes of stirring with heat preservation, the reaction ended. After cooling down, the operation was the same as in Example 2, and the catalyst was filtered out to obtain 210 ml of 4,4'-diaminostilbene-2,2'-sodium disulfonate solution, which was divided into two parts and carried out in different processing methods to further synthesize the synth...
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