Preparation method and application of active trivalent organic chromium compound
A technology of organic chromium and compounds, which is applied in the field of preparation of active trivalent organic acid chromium, can solve problems such as yield limitation, and achieve the effects of good stability, high yield and high catalytic activity
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[0029] The invention provides a preparation method of an active trivalent organic chromium compound, and the preparation method comprises the following steps:
[0030] Step 1, metathesis reaction of organic acid salt and chromium reagent;
[0031] In step 2, the reaction mixture is washed with water, heated to 150-300° C., and purified to obtain an active trivalent organic chromium compound;
[0032] Wherein, the chromium reagent is a water-soluble chromium compound, and the chromium in the chromium reagent is trivalent.
[0033] The method of the invention is to carry out metathesis reaction of organic acid salt and chromium reagent to obtain organic acid chromium hydrate, then wash out water-soluble ionic compounds, and then carry out high-temperature de-impurification and dissociation of coordination water through refining, so as to prepare active trihydrate Chromium organic acid. By adopting the method of the invention to prepare active trivalent organic acid chromium, t...
Embodiment 1
[0057] In a 1L flask, add 6.0g of sodium hydroxide and dissolve it in 50ml of deionized water, then add 20.4g of n-valeric acid, and start stirring. Weigh 16.85 g of chromium acetate hexahydrate, quickly drop it into the flask, add 40 ml of hexane, and heat up to 80 °C for 2 h. After the reaction, the heating was stopped, cooled to room temperature, poured into a separatory funnel, and the bottom liquid phase was released after the layers were separated. Add 50ml of decane and 80ml of deionized water to the separatory funnel, stand still after shaking, and release the bottom liquid after layering; in this way, repeatedly wash with deionized water 4 times, pour the upper layer liquid into the flask, and gradually heat up to 150 ℃, The temperature was kept at about 150°C for 3 hours, and nitrogen was introduced into the distillation system during the heating process to make the distillation system slightly positive pressure. The heating was stopped and cooled to room temperatur...
Embodiment 2
[0060] In a 1L flask, add 6.0g of sodium hydroxide to dissolve in 50ml of deionized water, and then add 26.0g of isooctanoic acid to start stirring. 12.8g of chromium chloride hexahydrate was added to the flask, 40ml of heptane was added, the temperature was raised to 100°C and the reaction was carried out for 1h. After the reaction, the heating was stopped, cooled to room temperature, poured into a separatory funnel, and the bottom liquid phase was released after the layers were separated. Add 90ml of deionized water to the separatory funnel, stand still after shaking, and release the bottom liquid after stratification; repeat washing with deionized water 4 times in this way, pour the upper layer liquid into the flask, add 60ml of dodecane, stir, and gradually heat up to 210°C and kept at about 210°C for 2h. The heating was stopped and cooled to room temperature to obtain 29.2 g of a green viscous liquid. The obtained product, chromium isooctanoate, was measured to obtain C...
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