The way to obtain calcium gluconate

 

(57) Abstract:

Usage: in medicine. The inventive product is calcium gluconate, exit 70 - 80%. Reagent 1: glucose. Reagent 2: hypobromide sodium resulting from the electrochemical oxidation of bromide of sodium. Process conditions: in the presence of calcium carbonate, followed by desalting of the solution of calcium gluconate from sodium bromide spend electrodialysis method at a density of 15 to 50 a/m2and 15 - 30oWith up to a final concentration of bromide of sodium in the desalted solution is not more than 1.4 g/l and the crystallization of the desired product, washing it from sodium bromide with distilled water, filtering and drying. 3 table.

The invention relates to the field of organic chemistry, in particular for receiving calcium gluconate, which is used in medicine as a pharmaceutical drug.

Calcium gluconate in the industry is produced by oxidation of glucose by hypobromide sodium resulting from the electrochemical oxidation of bromide of sodium (15-20 g/l) on graphite anode at current density of 120-500 a/m2and a temperature of 20-40aboutWith the presence of caso3c concentration of 5.0-7.0%, followed by crystallization of the fir places industrial method of production of calcium gluconate is the stage of removal of the bromide of sodium gluconate calcium by washing with distilled water. Washing of the target product from the inorganic salts are time-consuming and inefficient, as indicated by high consumption of distilled water for this operation (for 1 kg of product is used 7-8 kg of distilled water). In connection with the use of a large amount of water for leaching of calcium gluconate increases its solubility, which leads to a considerable reduction of the drug up to 30-40% in Addition, the allocation of calcium gluconate from the mother liquor and the wash water is an energy-intensive process due to the evaporation of large volumes of solutions and relatively high concentrations of bromide of sodium.

The results of the study by the washing of calcium gluconate distilled water from the sodium bromide are presented in table.1. From table.1 shows that the yield of calcium gluconate significantly depends on the quantity of wash water. When the leaching of calcium gluconate with distilled water according to the current technology, the yield of calcium gluconate is 31.5-35,0 and loss of product in the mother liquor and the wash water of 32.5-35.8% and 31.6% respectively. The yield of calcium gluconate increases with reducing the amount of wash water, but its quality does not meet the requirements of formstate N 121 GF X.

These faults is the process. One of the ways the separation of calcium gluconate from sodium bromide can be electrodialysis method of desalination.

The closest in technical essence to the proposed method is industrial electrochemical technology of production of calcium gluconate. The proposed method can improve the yield of calcium gluconate, to reduce the number of wash water, to simplify the technology excretion of calcium gluconate from the mother liquor and return to production of scarce bromide sodium.

The essence of the proposed method lies in the fact that the demineralization solution of calcium gluconate from sodium bromide spend electrodialysis method at a current density of from 15 to 50 a/m2and the temperature of 15-30aboutWith up to a final concentration of bromide of sodium in the desalted solution is not more than 1.4 g/L.

For the implementation of the proposed method the solution of calcium gluconate is directed to electrodialysis desalination. The process of electrodialysis is carried out at a current density of from 15 to 50 a/m2and the temperature of 15-30aboutWith up to a final concentration of bromide of sodium in the desalted solution is not more than 1.4 g/L. If all these conditions, the yield of calcium gluconate is 50,3-55,0% compared to 31.5% in PR is 15-50/m2. A further increase in current density is impractical because it leads to reduction of the yield of calcium gluconate and increase the intensity of the process (PL.2).

The temperature at which carry out the electrodialysis process in accordance with the invention is limited by thermal stability of the anion-exchange membranes and the crystallization of calcium gluconate.

Desalination solutions of calcium gluconate should be carried out until the residual concentration of bromide of sodium not more than 1.4 g/l At high salt concentration in the solution of calcium gluconate does not meet the requirements of formstate on the content of the bromides.

The results of the demineralization solution of calcium gluconate electrodialysis method are presented in table.3.

In the process of electrodialysis demineralization solution of calcium gluconate sodium bromide, passing through the ion exchange membrane, concentrated in the solution, forming a "concentrate". In "concentrate" transforms calcium gluconate (table.3), which reduces the yield of the target product. However, the whole "concentrate" can be used for the preparation of the electrolyte at the stage of electrochemical oxidation of glucose, eliminating dopolniteolnyh in table.1 and 3, in the mother liquor from the wash water obtained after the electrodialysis demineralization solutions of calcium gluconate, the concentration of bromide of sodium in 9-10 times lower in comparison with the prototype, which simplifies the selection of calcium gluconate. In addition, the number of processed solutions reduced.

P R I m e R 1 (comparative). In the cell capacitive type with graphite electrodes (cathode and anode), equipped with a stirrer and a jacket for temperature control, load 190 g of glucose, 1 l of a solution containing 65 g/l of calcium gluconate and 15.5 g/l sodium bromide and stirred until complete dissolution of glucose when heated to 35-40aboutC. To the resulting electrolyte is added 74 g caso3. At a temperature of 40aboutC and stirring of the electrolyte through the cell pass DC current, the strength of which corresponds to a current density 300,0 a/m2. Electrooxidation of glucose is considered complete when reaching concentrations of calcium gluconate solution 215-220 g/l In the electrolysis process after filtration from CaCO3get 1,07 l reaction mixture containing 218 g/l of calcium gluconate, 15.2 g/l sodium bromide and 20 g/l glucose. Calcium gluconate are separated from the solution by crystallization when ohla the th water from the sodium bromide in the amount of 1.6 L. The washed calcium gluconate is dried at a temperature of 80aboutC. Obtain 82 g of calcium gluconate, appropriate formstate N 121 GPH. The yield of calcium gluconate is 35% without recycling of the mother liquor and wash water.

P R I m m e R 2. The reaction mass in the amount of 0.35 l, containing 218,0 g/l of calcium gluconate and 15.2 g/l sodium bromide, obtained after electrochemical oxidation of glucose analogously to example 1, is subjected to electrodialysis desalination in a multi-chamber apparatus of electrodialyzer filterpresses type, consisting of alternating membranes type MK-40 and MA-40 with the intermediate part of paramita and separators-energizers. The cathode is a plate of stainless steel 18CR10NITI with the working surface 1 DM2, anode platinized titanium with the same surface. Electrodialyzer consisted of 6 cameras desalting and 7 cameras "concentration", and two electrode chambers. The working surface of each membrane 1 DM2and the distance between them is 1.5 mm Solution of calcium gluconate bromide with the sodium pump pumped through the camera "desalting" electrodialyzer with a linear speed of 4.0 cm/s, at the same time through the camera "concentration" Prokofiev 15aboutThrough electrodialyzer miss DC power which corresponds to a current density of 25 a/m2. The temperature in the process of electrodialysis is performed by the supply of cooled water in the coils of the intermediate containers. In the process of electrodialysis purification receive 0,325 l desalted solution with a concentration of sodium bromide 1.4 g/l, and calcium gluconate 166,4 g/l and 0,19 l "concentrate" with the concentration of sodium bromide to 26.2 g/l, and calcium gluconate 61,9 g/L.

Calcium gluconate from the desalted solution is crystallized by cooling the solution to a temperature of 4aboutC. the resulting suspension of calcium gluconate is filtered off and the mother liquor from the precipitate displace 70 ml of distilled water. Get to 39.3 g of calcium gluconate, appropriate formstate 121 GPH. The yield of calcium gluconate is 51,5% excluding the use of "concentrate" and recycling the mother liquor.

P R I m e R 3. The solution of calcium gluconate is subjected to electrodialysis desalination similar to example 2, but at current density of 15 a/m2and a temperature of 20aboutC. In the process of electrodialysis purification receive 0,32 l desalted solution with a concentration of sodium bromide to 1.37 g/l and gluco the Oia, appropriate formstate N 121 GPH. The yield of the target product is 55%

P R I m e R 4. The solution of calcium gluconate is subjected to electrodialysis desalination similar to example 2, but at current density of 50 a/m2. In the process of electrodialysis purification receive 0,33 l desalted solution with a concentration of sodium bromide 1.4 g/l, and calcium gluconate 169,2 g/L. the Selection of the target product from the solution as in example 2. Get to 38.4 g of calcium gluconate, appropriate formstate N 121 GPH. The yield of the target product is 50.3% of

P R I m e R 5. The solution of calcium gluconate is subjected to electrodialysis desalination similar to example 4, but to the concentration of bromide of sodium in the desalted solution of 2.0 g/L. In the process of electrodialysis purification receive 0.3 l with the concentration of calcium gluconate 185,6 g/L. the Selection of the target product from the solution as in example 2. Receive and 39.9 g of calcium gluconate, which corresponds to a yield of 52.3% of the quality of calcium gluconate does not meet the requirements of formstate N 121 GPH.

Thus, the proposed method of obtaining calcium gluconate can improve the yield of the target product to 51-55% and with the use of "concentration is STV wash with distilled water 6-7 times and return to the process scarce sodium bromide.

The WAY to OBTAIN CALCIUM GLUCONATE by oxidation of glucose by hypobromide sodium resulting from the electrochemical oxidation of bromide of sodium, in the presence of caso3with the crystallization of the desired product, washing it from sodium bromide with distilled water, filtering and drying, characterized in that before crystallization was carried out desalting solution of calcium gluconate from the sodium bromide by electrodialysis at current density of 15 a 50 a/m2and a temperature of 15 to 30oWith up to a final concentration of bromide of sodium in the desalted solution is not more than 1.4 g/L.

 

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