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Method for preparing gypsum whisker by calcium citrate

A technology of gypsum whiskers and calcium citrate, which is applied in the direction of chemical instruments and methods, single crystal growth, crystal growth, etc., can solve the problems of unreasonable development and utilization of citrate gypsum, and achieve relaxed reaction conditions and high whisker quality The effect of increasing and reducing production costs

Inactive Publication Date: 2010-06-09
ANHUI UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Aiming at the problem that citric acid gypsum has not been rationally developed and utilized so far in the existing citric acid production, the present invention reforms the calcium citrate acidolysis process in the citric acid plant, and provides a method for preparing gypsum whiskers with calcium citrate method for the direct generation of gypsum whiskers

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] Embodiment 1: water content 10% calcium citrate 200g, add concentration and be 290 milliliters of 30% sulfuric acid (density 1.22 grams / ml), add water 1000 milliliters, the mass ratio of calcium sulfate dihydrate and water is 1: 8, after stirring Put it into the autoclave, raise the temperature to 130°C, and keep the pressure at 270kPa for 10 minutes. Cool after the reaction, filter, wash the filter material once with water, and dry at 80° C. to obtain gypsum whiskers with a length of 100-400 microns, a diameter of 1-3 microns, and an aspect ratio of 100-160. The filtrate was collected for physical and chemical analysis, and the citric acid did not decompose in the hydrothermal reaction, and the recovery rate was greater than 95%. Gypsum whiskers were analyzed by XRD, and their composition was mainly dihydrate gypsum (CaSO 4 2H 2 O), with a small amount of hemihydrate gypsum (CaSO 4 1 / 2H 2 O).

Embodiment 2

[0012] Embodiment 2: water content 50% calcium citrate 200g, add 95% sulfuric acid (density 1.83 grams / ml) 34 milliliters, add water 100 milliliters, the mass ratio of calcium sulfate dihydrate and water is 1: 2, after stirring, add high pressure In the kettle, the temperature was raised to 120°C, the pressure was 200kPa, and maintained for 50 minutes. Cool after the reaction, filter, wash the filter material with water three times, and dry at 100°C to obtain gypsum whiskers with a length of 50-200 microns, a diameter of 2-4 microns, and an aspect ratio of 40-80.

Embodiment 3

[0013] Embodiment 3: water content 50% calcium citrate 200g, add 50% sulfuric acid (density 1.4 gram / ml) 84 milliliters, add water 350 milliliters, the mass ratio of calcium sulfate dihydrate and water is 1: 5, add high pressure after stirring In the kettle, the temperature was raised to 125°C, the pressure was 230kPa, and maintained for 30 minutes. Cool after the reaction, filter, wash the filter material twice with water, and dry at 90° C. to obtain gypsum whiskers with a length of 100-300 microns, a diameter of 1-4 microns, and an aspect ratio of 70-110.

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Abstract

The invention provides a method of manufacturing plaster crystal whiskers by utilizing calcium citrate and belongs to the field of fine chemical manufacturing technology. Combined with the citric acidmanufacturing technique, the invention manufactures plaster crystal whiskers while the calcium citrate is acidolysised to generate citric acid. The invention includes the following steps: firstly, after the sulphuric acid is added in, the calcium citrate serum is well stirred, placed in an autoclave for reaction at a temperature of 120 to 130 EDG C for 10 to 50 minutes and then cooled to be filtered; and secondly, the filtrate is used for crystallizing and separating out the citric acid product. The filtering medium is washed in water for 1 to 3 times, drained and then dried at a temperatureof 80 to 100 DEG C and finally plaster crystal whiskers with a length of 50 to 400 micrometers, a diameter of 1 to 4 micrometers and a diameter ratio of 40 to 160 are obtained. The invention generatesplaster crystal whiskers from the medium rich in citric acid by using the hydrothermal method, the reacting conditions are loose, the quality of the crystal whisker is obviously enhanced and the manufacturing cost for the crystal whisker is greatly reduced.

Description

technical field [0001] The invention belongs to the technical field of fine chemical production, and in particular relates to a method for preparing gypsum whiskers with calcium citrate. Background technique [0002] Whiskers refer to whisker-like single crystals that grow in the form of single crystals, whose shape is similar to short fibers, but whose radial dimension is much smaller than short fibers. Whiskers can be widely used as reinforcing and modifying components of composite materials. [0003] Gypsum whiskers have attracted the attention of the industry due to their excellent physical and chemical properties and relatively low cost. Compared with other short fibers, gypsum whiskers have the advantages of high temperature resistance, chemical corrosion resistance, good toughness, high strength, easy surface treatment, strong affinity with polymers such as rubber and plastics, and low toxicity. [0004] At present, most of the citric acid production in my country a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C30B29/10C30B29/62C30B7/10
Inventor 朱伟长郑翠红闫勇俞海云檀杰杨文燕韩甲兴刘柱
Owner ANHUI UNIVERSITY OF TECHNOLOGY
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