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Preparation method of calcium glucarate

A technology of glucaric acid and glucose, which is applied in the direction of carboxylate preparation, carboxylate preparation, organic compound preparation, etc., can solve the problems of low yield, environmental pollution, unfavorable industrial production, etc., and achieve the improvement of total yield, The effect of cost reduction and less industrial waste

Active Publication Date: 2019-04-26
江苏东南纳米材料有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But these methods are serious to environmental pollution, and yield is low, is unfavorable for suitability for industrialized production; Therefore, need to study its preparation method, control reaction condition with high yield, high quality, low cost and the glucose that meets the quality requirement of domestic and foreign pharmaceutical excipients Diacids and their calcium salts

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  • Preparation method of calcium glucarate
  • Preparation method of calcium glucarate
  • Preparation method of calcium glucarate

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preparation example Construction

[0049] Catalyst preparation:

[0050] Dissolve 6.0 g of ammonium metavanadate in deionized water, then add a certain amount of absolute ethanol to the bright yellow clear solution and stir for 10-20 minutes. Then, transfer the obtained solution into a hydrothermal reaction kettle, react at 180-200°C for 24-36 hours, cool down to room temperature after the reaction, filter, wash the solid with deionized water three times, and dry at 100°C 3-5 hours, then calcined at 500°C for 2-3 hours, after cooling and grinding, add 6.0g of Pd / C and continue grinding to obtain the metal catalyst palladium ammonium vanadium.

Embodiment 1

[0051] Embodiment 1 prepares calcium gluconate

[0052] In the high-pressure reaction tank, add 9g glucose, 10mol% nitric acid (the total amount of glucose and the oxygen participating in the reaction is 100%), 0.9g metal catalyst ammonium palladium vanadium and 90mL water, pressurize to 40MPa, and heat up to 100°C. Reaction 15h. After the reaction was completed, the temperature was lowered to room temperature, and solid KOH was added to the reaction solution to adjust the pH to 9. The mixture was lowered to 0°C, adjusted to pH 3-4 with 65% concentrated nitric acid, stirred for 1 h, filtered with suction, and the filter cake was washed three times with water and dried. Pour 10.2g of the dried potassium gluconate into 50ml of pure water, cool down to 0°C, adjust the pH to 1-2 with 65% concentrated nitric acid, then add solid CaO to adjust the pH to 6, stir overnight, and filter with suction , the filter cake was beaten with pure water at 50°C for 2 hours, cooled to room tempe...

Embodiment 2

[0053] Embodiment 2 prepares calcium gluconate

[0054] In the high-pressure reaction tank, add 45g glucose, 10mol% nitric acid (the total substance amount of glucose and oxygen participating in the reaction is 100%), 4.5g metal catalyst ammonium palladium vanadium and 500mL water, pressurize to 40MPa, and heat up to 100°C. Reaction 15h. After the reaction was completed, the temperature was lowered to room temperature, and solid KOH was added to the reaction solution to adjust the pH to 9. The mixture was lowered to 0°C, adjusted to pH 3-4 with 65% concentrated nitric acid, stirred for 1 h, filtered with suction, and the filter cake was washed three times with water and dried. Pour the dried 50g of glucaric acid potassium salt into 50ml of pure water, cool down to 0°C, adjust the pH to 1-2 with 65% concentrated nitric acid, then add solid CaO to adjust the pH to 6, stir overnight, and filter with suction. The filter cake was beaten with pure water at 50°C for 2 hours, lowere...

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Abstract

The invention relates to a preparation method of calcium glucarate, and belongs to the field of pharmacy. The invention provides a preparation method of the calcium glucarate. The preparation method comprises the following steps: (1) putting glucose, oxygen and a metal catalyst palladium vanadium ammonium into a high-pressure reactor for catalytic oxidation reaction to obtain glucaric acid; (2) after the oxidation reaction, adding potassium-containing alkali to convert the glucaric acid into potassium gluconate; (3) enabling the potassium gluconate to react with an acid to release the glucaricacid; (4) enabling the glucaric acid to react with the calcium-containing alkali to obtain the calcium glucarate. The preparation method disclosed by the invention is pollution-free to the environment, and meanwhile, the total yield is increased; the catalyst can be repeatedly used; the cost is reduced; the calcium content is 98 to 102 percent; a small amount of industrial wastewater, waste residues and waste gas are generated; the preparation method is suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of pharmacy, and in particular relates to a preparation method of calcium glucarate. Background technique [0002] Calcium gluconate is a compound containing 4 chiral carbon atoms, which is easily converted into glucaric acid in the human body. The metabolism of glucaric acid in the human body has multiple functions, not only can supplement the calcium of the human body, but also play other roles. some important physiological functions. Calcium gluconate, the structural formula is as follows: [0003] [0004] In mammals, glucaric acid and glucaric acid-1,4-lactone are the final products of the uronic acid pathway, and they can effectively inhibit the activity of β-glucuronidase (β-glucuronidase, βG for short). β-glucuronidase in the intestinal tract can catalyze the combination of glucuronic acid with endogenous toxins, bilirubin and other substances, convert carcinogen precursors into carcinogens, and play an i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/41C07C51/235C07C59/285
CPCC07C51/235C07C51/412C07C59/285
Inventor 刘海东万广朋吉民宗玺王冬冬于文源刘正富
Owner 江苏东南纳米材料有限公司
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