Preparation method of calcium sulfate whiskers

A technology of calcium sulfate whiskers and calcium sulfate, applied in the field of fillers, can solve the problems of environmental pollution, low efficiency, high energy consumption, etc., and achieve the effects of high reaction efficiency, low energy consumption, and uniform particle size

Active Publication Date: 2015-02-25
SHANGHAI BAOTIAN NOVEL BUILDING MATERIALS +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The above-mentioned method for manufacturing calcium sulfate whiskers has a series of problems such as low efficiency, high energy consumption, and serious environmental pollution, which have become important constraints for the sustainable and healthy development of the phosphorus chemical industry

Method used

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  • Preparation method of calcium sulfate whiskers
  • Preparation method of calcium sulfate whiskers
  • Preparation method of calcium sulfate whiskers

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] (1), preparation of calcium sulfate particles

[0031] D 50 Particles of 2 to 25 μm.

[0032] (2) Preparation of stabilizer

[0033] Add 180g water, 150gPEG (molecular weight is 2000) in the glass reactor, pass N under stirring 2 Substitution, the temperature was raised to 60° C., and 0.2 g of benzoyl peroxide was added. 15 g of methacrylic acid, 24.5 g of methyl methacrylate and 3 g of sodium methallyl sulfonate were added dropwise within 4 hours. Simultaneously, 40 g of an aqueous solution containing 0.3 g of ascorbic acid and 0.2 g of sodium edetate was added dropwise, and kept at 60° C. for 4 hours to complete the reaction. Adjust the pH of the reaction solution to 7 with a 30% sodium hydroxide aqueous solution, cool, filter with suction, and dry in vacuum to obtain a stabilizer. The structural formula of the stabilizer is shown in Formula II.

[0034] (3) Preparation of calcium sulfate whiskers

[0035] The calcium sulfate particle of 172g, the stabilizing ag...

Embodiment 2

[0037] (1), the preparation of calcium sulfate particle is with embodiment 1.

[0038] (2) Preparation of stabilizer

[0039] In glass reactor, add 170g water, 151gPEG (molecular weight is 2000), pass N under stirring 2 Replacement, warming up to 65°C, adding 17.05g of H 2 o 2 (mass concentration is 2%). 13.5 g of methacrylic acid, 24 g of methyl methacrylate and 5 g of sodium methallylsulfonate were added dropwise within 5 hours. Simultaneously, 40 g of an aqueous solution containing 0.2 g of vitamin E and 0.2 g of potassium persulfate was added dropwise and kept at 60° C. for 3 hours to complete the reaction. Use 30% sodium hydroxide aqueous solution to adjust the pH of the reaction solution to 7, cool, filter with suction, and dry to obtain a stabilizer. The structural formula of the stabilizer is shown in formula II.

[0040] (3) Preparation of calcium sulfate whiskers

[0041] The calcium sulfate particle of 172g, the stabilizing agent of 0.35g and the water of 800g...

Embodiment 3

[0043] (1), the preparation of calcium sulfate particle is with embodiment 1.

[0044] (2) Preparation of stabilizer

[0045] In the glass reactor, add 175g water, 158gPEG (molecular weight is 2000), pass N under stirring 2 replacement, warming up to 65°C, adding 14g of H 2 o 2 (mass concentration is 2%). 11 g of methacrylic acid, 19 g of methyl methacrylate, 4.5 g of sodium methallylsulfonate and 35 g of allyl polyethylene glycol (50) ether were added dropwise within 4 hours. Simultaneously, 38 g of an aqueous solution containing 0.3 g of ascorbic acid and 0.35 g of sodium edetate was added dropwise, and kept at 60° C. for 4 hours to complete the reaction. Adjust the pH of the reaction solution to 7 with a 30% sodium hydroxide aqueous solution, cool, filter with suction, and dry to obtain a stabilizer. The structural formula of the stabilizer is shown in Formula I.

[0046] (3) Preparation of calcium sulfate whiskers

[0047] The calcium sulfate particle of 172g, the st...

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Abstract

The invention belongs to the technical field of fillers, and particularly relates to a preparation method of calcium sulfate whiskers. The preparation method comprises the steps of pulverizing phosphogypsum or desulfurization gypsum to obtain calcium sulfate granules; adding polyethylene glycol and water in the presence of nitrogen, stirring, heating to 50-70 DEG C, adding an oxidant, then adding methacrylic acid, methyl methacrylate, sodium methallylsulphonate and allyl polyethylene glycol (50) ether, preserving the heat, performing reflux reaction, adding a reducing agent and a chelating agent, continuously preserving the heat, adjusting the pH value of the reaction solution to be neutral, cooling, carrying out suction filtration, and drying to obtain a stabilizer; and stirring the calcium sulfate granules, the stabilizer and water for 2-3 hours, adjusting the pH value of the reaction system to be 3-5, reacting for 1-6 hours at 120-130 DEG C, discharging, filtering and drying. The carboxylate block copolymer type stabilizer is added in the preparation method, so that the whiskers are grown regularly and have uniform particle diameter and controllable length and length-diameter ratio; and the preparation method has the advantages of low production cost, little pollution, low energy consumption and high yield.

Description

technical field [0001] The invention belongs to the technical field of fillers, in particular to a preparation method of calcium sulfate whiskers. Background technique [0002] Phosphogypsum is a utilizable by-product of wet-process phosphoric acid production for the mining of natural phosphate sands. In the traditional wet-process phosphoric acid production process, the ratio of wet-process phosphoric acid to by-product phosphogypsum is about 1:4-5 (weight ratio). At present, the annual output of phosphogypsum in the world exceeds 200 million tons, and the figure in my country has reached nearly 30 million tons. The phosphogypsum produced in the production process of wet-process phosphoric acid and phosphate fertilizer (the content of calcium sulfate dihydrate is 85%) also contains some other impurities. For a long time, it has been discharged in large quantities, which has caused great pressure on the surrounding land and water environment. At present, the utilization ra...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B29/62C30B29/46C30B7/14
CPCC30B7/14C30B29/46C30B29/62
Inventor 徐莉赵敏童敏程雲蒋青周维华文怡康明
Owner SHANGHAI BAOTIAN NOVEL BUILDING MATERIALS
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