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Method for preparing submillimeter hydryoxyapetite crystal with regular shape

A calcium hydrogen phosphate dihydrate, sub-millimeter technology, which is applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc. Large-size calcium hydrogen phosphate dihydrate crystals, fast crystal nucleation and other problems, to achieve the effect of regular crystal shape, low toxicity, and simple device

Inactive Publication Date: 2015-04-01
SHANDONG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Calcium hydrogen phosphate dihydrate crystals have a wide range of uses as additives such as food, toothpaste and bone cement. Calcium hydrogen phosphate dihydrate crystals, in which the concentration of precursors, mixing methods and reaction temperatures all have an impact on the supersaturation and crystallization behavior of calcium hydrogen phosphate dihydrate in the solution. However, it is difficult to control the growth of calcium hydrogen phosphate dihydrate crystals by traditional methods. Nucleation and growth process, because its small surface energy value will cause the crystal nucleation speed to be very fast, it is often difficult to prepare large-sized calcium hydrogen phosphate dihydrate crystals
The size, phase and shape of calcium hydrogen phosphate dihydrate crystals have a significant impact on its adsorption and degradation properties and phase transformation process, but there are few data on regulating the crystal size of calcium hydrogen phosphate dihydrate, especially to obtain regular shape, There are fewer ways to prepare crystals of uniform size

Method used

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  • Method for preparing submillimeter hydryoxyapetite crystal with regular shape
  • Method for preparing submillimeter hydryoxyapetite crystal with regular shape
  • Method for preparing submillimeter hydryoxyapetite crystal with regular shape

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Step 1. Prepare 25 grams of aqueous solution containing 0.16 moles per liter of L-glutamic acid, 0.043 moles per liter of disodium hydrogen phosphate and 0.070 moles per liter of sodium hydroxide, stir at room temperature to make it completely dissolve, add 20 grams of ice, and then Add L-arginine, urea and calcium nitrate successively so that their concentrations are respectively 0.026 moles per liter, 0.056 moles per liter and 0.026 moles per liter;

[0021] Step 2. Add the uniformly stirred mixed solution into a 50 ml stoppered colorimetric tube, react at 37oC for 24 hours and then cool to room temperature;

[0022] Step 3. The product obtained by the reaction in step 2 is filtered, washed and dried to prepare calcium hydrogen phosphate dihydrate crystals.

[0023] The product was identified as calcium hydrogen phosphate dihydrate through X-ray powder diffraction (see figure 1 ). SEM scanning electron microscope inspection product morphology (see figure 2 ).

Embodiment 2

[0025] Step 1. Prepare 25 grams of aqueous solution containing 0.16 moles per liter of L-glutamic acid, 0.043 moles per liter of disodium hydrogen phosphate and 0.070 moles per liter of sodium hydroxide, stir at room temperature to make it completely dissolve, add 20 grams of ice, and then Add L-arginine, urea and calcium nitrate successively so that their concentrations are respectively 0.026 moles per liter, 0.056 moles per liter and 0.026 moles per liter;

[0026] Step 2. Add the uniformly stirred mixed solution into a 50 ml stoppered colorimetric tube, react at 37oC for 6 hours and then cool to room temperature;

[0027] Step 3. The product obtained by the reaction in step 2 is filtered, washed and dried to prepare calcium hydrogen phosphate dihydrate crystals.

[0028] SEM scanning electron microscope inspection product morphology (see image 3 ).

Embodiment 3

[0030] Step 1. Prepare 25 grams of aqueous solution containing 0.16 moles per liter of L-glutamic acid, 0.043 moles per liter of disodium hydrogen phosphate and 0.070 moles per liter of sodium hydroxide, stir at room temperature to make it completely dissolve, add 20 grams of ice, and then Add L-arginine, urea and calcium nitrate successively to make the concentration respectively 0.038 mole per liter, 0.056 mole per liter and 0.026 mole per liter;

[0031] Step 2. Add the uniformly stirred mixed solution into a 50 ml stoppered colorimetric tube, react at 37oC for 24 hours and then cool to room temperature;

[0032] Step 3. The product obtained by the reaction in step 2 is filtered, washed and dried to prepare calcium hydrogen phosphate dihydrate crystals.

[0033] SEM scanning electron microscope inspection product morphology (see Figure 4 ).

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Abstract

The invention provides a method for preparing a submillimeter hydryoxyapetite crystal with a regular shape, and belongs to the field of ceramic materials. The method for preparing the submillimeter hydryoxyapetite crystal is mainly achieved through the following steps that firstly, water solutions including L-glutamic acid, disodium hydrogen phosphate and sodium hydroxide are prepared, the water solutions are fully stirred at indoor temperature to be dissolved, then ice, L-arginine, carbamide and calcium nitrate are added to the water solutions in sequence, the evenly-stirred mixed solutions are added to a certain amount of acetone, the solutions react for a while at the temperature below 37 DEG C and are cooled to be the indoor temperature, products obtained through the reaction are filtered, washed and dried, and the hydryoxyapetite crystal is prepared. The obtained plate-shaped hydryoxyapetite crystal is regular in shape and even in size, is 20-500 microns long, 5-200 microns wide and 1-10 microns thick, and can be used as drug diluent, bone cement additives, food additives and the like.

Description

technical field [0001] The invention relates to a method for preparing regular-shaped submillimeter calcium hydrogen phosphate dihydrate crystals, belonging to the field of ceramic materials. Background technique [0002] Calcium hydrogen phosphate dihydrate crystals have a wide range of uses as additives such as food, toothpaste and bone cement. Calcium hydrogen phosphate dihydrate crystals, in which the concentration of precursors, mixing methods and reaction temperatures all have an impact on the supersaturation and crystallization behavior of calcium hydrogen phosphate dihydrate in the solution. However, it is difficult to control the growth of calcium hydrogen phosphate dihydrate crystals by traditional methods. Nucleation and growth process, because its small surface energy value will cause the crystal nucleation speed to be very fast, it is often difficult to prepare large-sized calcium hydrogen phosphate dihydrate crystals. Chinese patent CN 101774561 A discloses a ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/32
Inventor 李成峰葛筱璐李国昌白佳海丁锐
Owner SHANDONG UNIV OF TECH
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