Process for preparing 2-hydroxy-4-methylthiobutanoic acid
A technology for the production of methylthiobutyric acid, which is applied in organic chemistry methods, chemical instruments and methods, and preparation of sulfides, and can solve problems such as poor separability and poor extraction efficiency
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Embodiment 1 and comparative example 1 and 2
[0035] Into 40.1g (0.35mol) of 85.6wt% sulfuric acid aqueous solution, 82.7g (0.50mol) of 79.2wt% 2-hydroxy-4-methylthiobutyronitrile aqueous solution was added dropwise within 30min under stirring at 50°C to obtain the mixture Maintain at 50°C for 2h. To this mixture was added 57.2 g of water, and then, the mixture was stirred at 110°C for 4 h. The analysis result of the formed reaction mixture showed that the yield of 2-hydroxy-4-methylthiobutyric acid was 95%-96%.
Embodiment 1
[0036] Example 1: After adding 8.0 g (0.20 mol) of granular sodium hydroxide to the reaction mixture obtained in the same manner as above, the resulting reaction mixture was stirred and separated into an oil layer and a water layer.
Embodiment 2-1~ Embodiment 2~15
[0042] The reaction was carried out in the same manner as in Example 1. To each of the obtained reaction mixtures (180 g), a specific amount (as shown in Table 2) of 48 wt% sodium hydroxide aqueous solution was added, and the resulting mixture was fully stirred. The pH value of the obtained mixture at 25°C is shown in Table 2. Each mixture separated into an oil layer and a water layer at 60°C. Each oil layer is concentrated by evaporating in an evaporator until the liquid water content of the oil layer (determined by Karl Fischer method) reaches the value shown in Table 2. Each concentrated liquid (slurry) thus obtained was filtered at 70°C. Water was added to each filtrate thus obtained so that the content of 2-hydroxy-4-methylthiobutyric acid reached 89.0 wt% (measured by potentiometric titration), thereby obtaining each product.
[0043] The sulfate ion concentration and kinematic viscosity at 25°C measured by ion chromatography for each product are shown in Table 2.
[0044] ...
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