Clean and efficient preparation method of 1, 6-Cleve's acid and 1, 7-Cleve's acid
An efficient and clean technology, applied in the preparation of sulfonic acid, sulfonic acid salt, chemical instruments and methods, etc., can solve the problems of serious environmental pollution of waste, strong carcinogenicity and corrosiveness, and high pressure on environmental protection, so as to improve economic benefits. , the effect of improving the reduction efficiency and reducing the production cost
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[0033] Example 1:
[0034] (1) Reduction reaction: 5 g of Raney nickel catalyst was added to the hydrogenation reactor, 250 g of a solution containing 33 g of mixed nitrosulfonic acid magnesium salt was added, and the reaction was carried out at a reaction temperature of 60 °C and a hydrogen pressure of 0.5 MPa for 5 h.
[0035] (2) Concentration and separation: the reducing solution is filtered to remove the catalyst, then the temperature is increased and concentrated to 40g / L, then cooled to 30°C, and the magnesium salt of 1,6-cliffeate is separated out, filtered, and the filter cake is magnesium 1,6-cliffeate. salt, the filtrate is a solution of magnesium 1,7-cliffeate.
[0036] (3) Acid precipitation: add 48% sulfuric acid solution to the 1,6-cliffeate and 1,7-cliffeate solutions concentrated and separated in step (2), until the pH of the system is equal to 1, filter, After washing and drying, corresponding 11.7 g of 1,6-Cliff acid and 12.1 g of 1,7-Cliff acid were obtain...
Example Embodiment
[0037] Example 2:
[0038] (1) Reduction reaction: 2 g of Pd / C catalyst was added to the hydrogenation reaction kettle, 250 g of a solution containing 33 g of mixed nitrosulfonic acid magnesium salt was added, and the reaction was carried out at a reaction temperature of 150 °C and a hydrogen pressure of 8 MPa for 0.1 h.
[0039] (2) Concentration and separation: the reducing solution was filtered to remove the catalyst, then the temperature was increased and concentrated to 120 g / L, and then cooled to 30 ° C, and the magnesium salt of 1,6-cliffeate was separated out, filtered, and the filter cake was magnesium 1,6-cliffeate. salt, the filtrate is a solution of magnesium 1,7-cliffeate.
[0040] (3) Acid precipitation: add 48% sulfuric acid solution to the 1,6-cliffeate and 1,7-cliffeate solutions concentrated and separated in step (2) respectively, to pH=2 of the system, filter, After washing and drying, corresponding 12.5 g of 1,6-Cliff acid and 12.6 g of 1,7-Cliff acid were...
Example Embodiment
[0041] Example 3:
[0042] 2g of Pd / C catalyst was added to the hydrogenation reaction kettle, 250g of a solution containing 33g of mixed nitrosulfonic acid magnesium salt was added, and the reaction was carried out at a reaction temperature of 150°C and a hydrogen pressure of 2MPa for 0.5h. The remaining steps were the same as those in Example 2, and 12.3 g of 1,6-Cliff acid and 13.5 g of 1,7-Cliff acid were obtained, respectively, with a total yield of 92.4%.
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