Preparation method of large particle crystal form high bulk density 2-hydroxy-4-methylthiobutyrate calcium
A technology of calcium methylthiobutyrate and methylthiobutyric acid is applied to the chemical industry, and can solve the problems of long drying time, destruction of nutrients, poor fluency, etc., so as to improve the total yield, save energy, and avoid emissions. Effect
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Embodiment 1
[0052] Dilute 340.9g of 2-hydroxy-4-methylthiobutyric acid from 88% to 40% with deionized water, then add 0.015g of lactic acid, stir and heat to 60°C, keep warm for 60 minutes, add anhydrous calcium chloride solid 111 g, during the reaction, the pH of the reaction system was adjusted to 6.0 with sodium hydroxide, and the reaction was stirred at a constant temperature for 2 hours. After the reaction was completed, cool to 10°C and press filter to obtain white crystals, which were washed twice with a small amount of cold water, and then vacuum-dried to constant weight at 90°C to obtain 331.1 g of calcium 2-hydroxy-4-methylthiobutyrate with a purity of It was 98%, and the yield was 96%. Analysis results: 2-hydroxy-4-methylthiobutyric acid content 86.2%; calcium: 11.3%; water content: 0.5%; purity 98%; 140 mesh analysis sieve 85%, in the form of smooth powder with crystals Sexual luster, bulk density (g / cm) is 0.69.
[0053] Add water to the obtained 2-hydroxy-4-methylthiobutyr...
Embodiment 2
[0055] Dilute 340.9g of 2-hydroxy-4-methylthiobutyric acid from 88% to 35% with deionized water, then add 0.034g of citric acid, stir and heat to 80°C, keep warm for 30 minutes, add anhydrous calcium chloride The solid was 111 g. During the reaction, the pH of the reaction system was adjusted to 7.0 with sodium hydroxide, and the reaction was stirred at a constant temperature for 2 hours. After the reaction was completed, cool to 10°C and press filter to obtain white crystals, which were washed twice with a small amount of cold water, and then vacuum-dried to constant weight at 90°C to obtain 331.1 g of calcium 2-hydroxy-4-methylthiobutyrate with a purity of It was 98%, and the yield was 96%. Analysis results: 2-hydroxy-4-methylthiobutyric acid content 86.2%; calcium: 11.3%; water content: 0.5%; purity 98%; 140 mesh analysis sieve 84%, in the form of smooth powder with crystals Sexual luster, bulk density (g / cm) is 0.70.
[0056] Add water and the recrystallization mother li...
Embodiment 3
[0058] Dilute 340.9g of 2-hydroxy-4-methylthiobutyric acid from 88% to 60% with deionized water, then add 0.014g of hydroxymethyl cellulose, stir and heat to 70°C, keep it warm for 30 minutes, add anhydrous Calcium carbonate solid 101g, during the reaction, adjust the pH of the reaction system with sodium hydroxide to maintain at 6.0, stir and react at constant temperature for 3 hours. After the reaction was completed, cool to 10°C and press filter to obtain white crystals, which were washed twice with a small amount of cold water, and then vacuum-dried to constant weight at 90°C to obtain 331.1 g of calcium 2-hydroxy-4-methylthiobutyrate with a purity of It was 98%, and the yield was 96%. Analysis results: 2-hydroxy-4-methylthiobutyric acid content 86.2%; calcium: 11.3%; water content: 0.5%; purity 98%; 140 mesh analysis sieve 86%, in the form of smooth powder with crystals Sexual luster, bulk density (g / cm) is 0.65.
[0059] Add water and the recrystallization mother liquo...
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