Method for preparing gypsum whiskers from calcium hydrogen citrate

A technology of calcium hydrogen citrate and gypsum whiskers, which is applied in chemical instruments and methods, single crystal growth, crystal growth, etc., can solve problems such as low output, poor quality of whiskers, and inability to obtain technical effects, so as to reduce production costs , Whisker quality improvement, the effect of relaxed reaction conditions

Inactive Publication Date: 2016-05-11
RIZHAO JINHE BOYUAN BIOCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the poor quality of this part of citrate gypsum, it has not been rationally developed and utilized so far, and has always been one of industrial solid wastes.
[0005] Disclosed in CN101230483B is a method for producing gypsum whiskers with calcium citrate. It adopts the method of adding lime slurry in the production of citric acid to obtain calcium citrate slurry, adding sulfuric acid with a concentration of 30%-98% of the amount of calcium and other substances Obtain calcium sulfate, obtain whisker in autoclave afterwards, inventor has carried out repeated test according to the technical scheme of its record, the result finds that after it adopts calcium citrate slurry, the reaction condition in the autoclave that adopts is comparatively simple, and its prepared The quality of the whiskers is extremely poor, and the yield is low, most of the calcium sulfate still exists in the form of granular crystals of uneven size, so the expected technical effect cannot be obtained

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] (1) After the citric acid is purified, the citric acid content in the citric acid solution obtained is 30wt%, and the mol ratio of citric acid and the vitriol oil in the citric acid solution is controlled by adding 92wt% concentrated sulfuric acid to be 1:1, and the pressure of the reactor is adjusted to be 1 kg pressure, the reaction temperature is 60°C;

[0020] (2) Slowly add citric acid in the reactor to obtain calcium hydrogen citrate slurry, stir, and the feeding time is 80 minutes; the final reaction end point is that the content of calcium ion and sulfate ion in the reaction system is 1:1, after the reaction finishes Maintain the reaction conditions for not less than 30 minutes;

[0021] (3) depressurize and cool after the above reaction finishes, adopt belt filter to filter, filtrate goes to the citric acid refining section, and the calcium sulfate whisker obtained by filtering is washed with 15wt% lime water to a pH value of 5, and dried after filtering , to ...

Embodiment 2

[0023] (1) after the citric acid is purified, the citric acid content in the citric acid solution obtained is 60wt%, and the mol ratio of citric acid and the vitriol oil in the citric acid solution is controlled by adding 90wt% concentrated sulfuric acid to be 1:1, and the pressure of the reactor is adjusted to be 2 kg pressure, the reaction temperature is 100°C;

[0024] (2) Slowly add citric acid in the reactor to obtain calcium hydrogen citrate slurry, stir, and the feeding time is 600 minutes; the final reaction end point is that the content of calcium ion and sulfate ion in the reaction system is 1:1, after the reaction finishes Maintain the reaction conditions for not less than 30 minutes;

[0025] (3) depressurize and cool after the above reaction finishes, adopt belt filter to filter, filtrate goes to citric acid refining workshop, and the calcium sulfate crystal whisker that filter obtains is washed to pH value 9 with 15wt% lime water, dries after filtering , to obta...

Embodiment 3

[0027] (1) after the citric acid is purified, the citric acid content in the citric acid solution obtained is 50wt%, and the mol ratio of citric acid and the vitriol oil in the citric acid solution controlled by adding 95wt% vitriol oil is 1:1, and the adjustment reactor pressure is 2 kg pressure, the reaction temperature is 80°C;

[0028] (2) Slowly add citric acid in the reactor to obtain calcium hydrogen citrate slurry, stir, and the feeding time is 400 minutes; the final reaction end point is that the content of calcium ion and sulfate ion in the reaction system is 1:1, after the reaction finishes Maintain the reaction conditions for not less than 30 minutes;

[0029] (3) depressurize and cool after the above reaction finishes, adopt belt filter to filter, filtrate goes to citric acid refining section, and the calcium sulfate whisker that filters obtains is washed to pH value 7 with the lime water of 15wt%, is dried after filtering , to obtain gypsum whiskers with a lengt...

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Abstract

The invention relates to the field of citric acid production, and particularly provides a method for preparing gypsum whiskers from calcium hydrogen citrate; the method comprises that calcium hydrogen citrate in a citric acid production process is used as a raw material and undergoes a reaction with concentrated sulfuric acid, and the gypsum whiskers are prepared while citric acid is obtained; the method mainly comprises the steps: carrying out a reaction of a calcium hydrogen citrate slurry with sulfuric acid in a citric acid solution with the pressure of 1-2 kg for 80-600 minutes, to obtain the gypsum whiskers; and filtering with a belt type filter, refining and purifying the filtrate to obtain the citric acid product, and after the filter cake is dried, drying at the temperature of 80-100 DEG C, to obtain the gypsum whiskers with the whisker length of 50-400 microns, the diameter of 1-4 microns and the diameter ratio of 20-100. The gypsum whiskers are generated through the hydrothermal method in a medium having a large amount of citric acid, the reaction conditions are loose, the whisker quality is obviously improved, and moreover, the production cost of the gypsum whiskers is greatly reduced.

Description

technical field [0001] The invention relates to the field of citric acid production, and specifically provides a method for preparing gypsum whiskers with calcium hydrogen 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 adopts ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B29/62C30B29/46C30B7/10
CPCC30B29/62C30B7/10C30B29/46
Inventor 寇光智李昌涛周昊秦绪斌于海滨周一江
Owner RIZHAO JINHE BOYUAN BIOCHEM
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