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Method for preparing pure calcium sulfate whiskers from carbide slag modified phosphogypsum

A technology of phosphogypsum and calcium carbide slag, applied in the direction of calcium/strontium/barium sulfate, etc., can solve the problems of large solid-liquid ratio, waste, underutilization of resources, etc., and achieve the effect of stable concentration and lower production cost.

Active Publication Date: 2020-11-27
HUBEI UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] Patent CN109695052A uses natural gypsum to prepare calcium sulfate whiskers. Natural gypsum is purified and purified by chemical methods to obtain pure calcium sulfate by hydrothermal synthesis. This industry makes full use of the product, and the production process is clean and environmentally friendly, but it is not fully utilized. Industrial by-product gypsum causes waste of resources
[0007] Patent CN10456180A discloses a method for preparing calcium sulfate whiskers from phosphogypsum. In this method, dilute acid is heated to dissolve phosphogypsum and filtered, and the dihydrate gypsum whiskers are separated out by filtration. Since phosphogypsum still has soluble phosphorus, it is difficult to wash it with water. Removed, the solubility of calcium sulfate in dilute acid is very low, so the solid-liquid ratio is very large and the cost is high

Method used

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  • Method for preparing pure calcium sulfate whiskers from carbide slag modified phosphogypsum

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] The preparation steps are as follows:

[0050] 1. First, take 100 parts of phosphogypsum powder passed through a 0.075mm square hole sieve, then take 5 parts of carbide slag powder, and stir in a mixer for 10 minutes to obtain a powder mixture.

[0051] 2. Take 100 parts of the powder mixture, add 55 parts of n-hexane and water at a ratio of 1:1, add 0.1 part of citric acid, 0.1 part of polycarboxylate superplasticizer, add grinding media, and put it into the grinder , grind for 1 hour, and sieve out the grinding medium to obtain a slurry.

[0052] 3. Take 100 parts of the slurry, add 0.5 parts of magnesium chloride, stir evenly, then transfer to a high-pressure reactor, control the temperature at 80 degrees Celsius, and after 2 hours of reaction time, treat with 1 part of ethanol and centrifuge to obtain a precipitate. Washing was repeated 3 times, and then freeze-dried to obtain anhydrous calcium sulfate whiskers.

Embodiment 2

[0054] The preparation steps are as follows:

[0055] 1. First, take 100 parts of phosphogypsum powder passed through a 0.075mm square hole sieve, then take 10 parts of calcium carbide slag powder, and stir in a mixer for 10 minutes to obtain a powder mixture.

[0056] 2. Take 100 parts of the powder mixture, add 110 parts of cyclohexane and water at a ratio of 1:1, add 0.15 parts of animal protein, 0.2 parts of naphthalene-based water reducer, add grinding media, and put it into the grinder , grind for 1.2 hours, and sieve out the grinding medium to obtain a slurry.

[0057] 3. Take 100 parts of the slurry, add 0.6 parts of sodium citrate, stir evenly, then transfer to a high-pressure reactor, control the temperature at 80 degrees Celsius, and after 2.5 hours of reaction time, treat with 1 part of ethanol and centrifuge to obtain the precipitate . Washing was repeated 3 times, and then freeze-dried to obtain anhydrous calcium sulfate whiskers.

Embodiment 3

[0059] 1. First, take 100 parts of phosphogypsum powder passed through a 0.075mm square hole sieve, then take 15 parts of carbide slag powder, and stir in a mixer for 10 minutes to obtain a powder mixture.

[0060] 2. Take 100 parts of the powder mixture, add 165 parts of chloroform and water at a ratio of 1:1, add 0.2 parts of sodium tripolyphosphate, 0.3 parts of naphthalene-based water reducer, add grinding media, and put it into the grinder , grind for 1.5 hours, and sieve out the grinding medium to obtain a slurry.

[0061] 3. Take 100 parts of the slurry, add 0.7 parts of sodium citrate, stir evenly, then transfer to a high-pressure reactor, control the temperature at 85 degrees Celsius, and after a reaction time of 3 hours, treat with 2 parts of ethanol and centrifuge to obtain a precipitate. Washing was repeated 3 times, and then freeze-dried to obtain anhydrous calcium sulfate whiskers.

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Abstract

The invention discloses a method for preparing calcium sulfate whiskers from carbide slag modified phosphogypsum. The method comprises the following steps: (1) mixing phosphogypsum powder and carbideslag powder to obtain a powder mixture; (2) adding the powder mixture into an organic solvent-water mixed solution, adding a retarder and a water reducing agent, and grinding and sieving to obtain slurry; and (3) taking the slurry, adding a crystal growth promoter, uniformly stirring, transferring the mixture into a high-pressure reaction kettle, controlling the temperature to react completely, carrying out alcohol washing and centrifuging to obtain a precipitate, and carrying out washing, and freeze drying to obtain the anhydrous calcium sulfate whiskers. According to the method, the anhydrous calcium sulfate whiskers are prepared by fully utilizing the phosphorus solid waste and the carbide slag under the condition of room temperature, impurities of the phosphogypsum and the carbide slagare dissolved out by combining a wet grinding process and are removed by utilizing organic matters and water, and the calcium sulfate with relatively high purity is obtained through simple lengthening and crystal growth. The preparation method provided by the invention saves energy, reduces consumption, turns waste into wealth, and realizes green, environment-friendly and sustainable preparationof anhydrous calcium sulfate whiskers.

Description

technical field [0001] The invention belongs to the technical field of solid waste recycling and environment, in particular to a method for preparing calcium sulfate whiskers from calcium carbide slag modified phosphogypsum. Background technique [0002] my country's industrial by-product gypsum mainly includes desulfurization gypsum, phosphogypsum, titanium gypsum, citrate gypsum, etc. In 2018, my country's industrial by-product gypsum discharge was about 200Mt, and the stockpile of gypsum over the years was 850Mt, making it only used in the field of building materials As a gypsum wall and mortar material, the application range of gypsum is relatively limited, especially the industrial side gypsum products, which have a relatively large annual storage capacity, and they are directly stacked and disposed of, which seriously affects the environmental quality; Comprehensive utilization of treatment, due to inappropriate treatment methods, leads to high treatment costs and high e...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F11/46
CPCC01F11/46C01P2004/10C01P2006/80Y02W30/91
Inventor 陈顺刘巧彭圣刚黄佳瑶苏英黄震宇张权钢贺行洋王迎斌秦景燕范朦
Owner HUBEI UNIV OF TECH
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