Method of synchronously preparing DL-tartaric acid and DL-potassium hydrogen tartrate
A technology of potassium hydrogen tartrate and tartaric acid, which is applied in chemical instruments and methods, carboxylate preparation, carboxylate preparation, etc., can solve the problems of waste of resources, low conversion rate, increased production cost, etc., and achieve fewer reaction steps, High conversion and yield, easy to control effect
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Embodiment 1
[0029] Embodiment 1, a kind of preparation method of DL-tartaric acid, carries out following steps successively:
[0030] 1) Add 100 g of deionized water, 100 g of maleic anhydride, and 150 g of hydrogen peroxide with a mass concentration of 28% in sequence in the reactor; heat up to 50°C for 3 hours;
[0031] 2) Add 5 g of phosphomolybdenum heteropoly acid as a catalyst to the product obtained in step 1), and then slowly raise the temperature at a rate of 6°C / h; when the temperature rises to 72°C, stop heating;
[0032] 3) Insulate and react at 72°C for 20 hours; then heat up to 110°C, and hydrolyze for 3.5 hours to obtain a solution containing epoxysuccinic acid;
[0033] Cool the solution containing epoxysuccinic acid with cooling water, and use ice brine instead when the temperature drops to about 25°C. When the temperature drops to 6~8°C, it will crystallize naturally, and then filter it with a rotary vacuum pump (vacuum degree 0.08; used Filter paper pore size 15~20 mic...
Embodiment 2
[0037] Embodiment 2,4-aminopyridine chelating resin reclaims the catalyst in the mother liquor
[0038] Put 30mg of 4-aminopyridine resin into 25ml of acetic acid-sodium acetate buffer solution with a pH of 4.1 and soak for 20-24 hours to obtain swollen 4-aminopyridine resin.
[0039] Add 10ml of the secondary mother liquor obtained in the above-mentioned Example 1 (after testing, the molybdenum ion content is 1.7mg / ml) to the above-mentioned swollen 4-aminopyridine resin, and use the pH value of the 4-aminopyridine resin after adsorption equilibrium to be 4.1 After washing with acetic acid-sodium acetate buffer solution (5 times in total, 60ml each time), wash several times with deionized water (5 times in total, 60ml each time), and dry to constant weight After soaking (need to be fully submerged), perform vibration desorption in 25ml of NaOH solution with a concentration of 3mol / L; when the concentration of molybdenum ions in the NaOH solution remains unchanged, the adsorpt...
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