Preparation method of rod-shaped [alpha]-calcium sulfate hemihydrate whiskers

A calcium sulfate hemihydrate, rod-shaped technology, which is applied in the field of preparation of rod-shaped α-calcium sulfate hemihydrate whiskers, can solve the problems of incomplete crystal form and low purity of calcium sulfate whiskers, and achieve a green, pollution-free and repeatable preparation process. The effect of good performance and controllable shape rules

Active Publication Date: 2019-08-16
河南博海化工有限公司 +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The object of the present invention is to overcome the problems in the prior art that calcium sulfate precursors are crystal-transformed by a crystal-transforming agent, and the obtained calcium sulfate whiskers have incomplete crystal form and low purity, and then provide a rod-shaped α-hemihydrate The preparation method of calcium sulfate whisker

Method used

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  • Preparation method of rod-shaped [alpha]-calcium sulfate hemihydrate whiskers
  • Preparation method of rod-shaped [alpha]-calcium sulfate hemihydrate whiskers
  • Preparation method of rod-shaped [alpha]-calcium sulfate hemihydrate whiskers

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Embodiment 1

[0052] The present embodiment provides a kind of preparation method of rod shape α-calcium sulfate hemihydrate whisker, comprises the steps:

[0053] 1) Take sodium sulfate solid waste, and use a calciner to calcinate to remove organic residues, the calcining temperature is 700 ° C, and the calcining time is 3 hours; after the calcining is completed, the calcined sodium sulfate is dissolved in water, and the inorganic insolubles are filtered to remove the 2.0 mol / L sodium sulfate aqueous solution;

[0054] 2) Measure 300ml (0.60mol) of 2.0mol / L sodium sulfate aqueous solution into a reaction vessel, then add 22.58g of sodium hydrogen phthalate, heat and stir to raise the temperature to 100°C, and slowly add 133ml of 4.5mol / L calcium chloride aqueous solution (0.60mol), the feed rate is 7.5ml / min, after the addition of the calcium chloride aqueous solution is completed, continue to keep stirring at 100°C for 2h;

[0055] 3) After the reaction was completed, it was allowed to s...

Embodiment 2

[0061] The present embodiment provides a kind of preparation method of rod shape α-calcium sulfate hemihydrate whisker, comprises the steps:

[0062] 1) Take sodium sulfate solid waste, and use a calciner to calcinate to remove organic residues, the calcining temperature is 800 ° C, and the calcining time is 1 hour; after the calcining is completed, the calcined sodium sulfate is dissolved in water, and the inorganic insolubles are filtered to remove the 2.0 mol / L sodium sulfate aqueous solution;

[0063] 2) Measure 335ml (0.67mol) of a 2.0mol / L sodium sulfate aqueous solution into a reaction vessel, then add 20.28g of phthalic anhydride, heat and stir to raise the temperature to 105°C, and slowly add 117ml (0.70mol) of a 6mol / L calcium nitrate aqueous solution ), the feed rate was 7.5ml / min, and after the addition of the calcium nitrate aqueous solution was completed, the stirring reaction was continued at 105°C for 3h;

[0064] 3) After the reaction is completed, leave it t...

Embodiment 3

[0067] The present embodiment provides a kind of preparation method of rod shape α-calcium sulfate hemihydrate whisker, comprises the steps:

[0068] 1) Take sodium sulfate solid waste, and remove organic residues by calcining in a calciner, the calcining temperature is 500° C., and the calcining time is 24 hours; after the calcining is completed, the calcined sodium sulfate is dissolved in water, and the inorganic insolubles are removed by filtration to make 1.0 mol / L sodium sulfate aqueous solution;

[0069] 2) Measure 400ml (0.4mol) of 1.0mol / L sodium sulfate aqueous solution into a reaction vessel, then add 1.15g of sodium benzoate, heat and stir to raise the temperature to 90°C, and slowly add 91.4ml (0.32mol) of 3.5mol / L calcium nitrate aqueous solution , the feeding speed is 7.5ml / min, after the calcium nitrate aqueous solution is added, continue to keep stirring at 90°C for 6h;

[0070] 3) After the reaction is completed, leave it to age for 24 hours to obtain the cru...

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Abstract

The invention relates to the technical field of gypsum material preparation, in particular to a preparation method of rod-shaped [alpha]-calcium sulfate hemihydrate whiskers. The method comprises thefollowing steps: 1) adding an organic crystal form control agent into a sodium sulfate aqueous solution, heating and stirring the solution, adding an inorganic calcium salt, and continuously stirringand reacting the mixture; and 2) after the reaction in the step 1) is finished, standing and aging the reaction product to obtain a rod-shaped [alpha]-calcium sulfate hemihydrate whisker crude product, and washing and drying the crude product to obtain the rod-shaped [alpha]-calcium sulfate hemihydrate whisker. The preparation method has the advantages of advanced method, low synthesis temperature, low raw material price, green and pollution-free preparation process and good repeatability. The [alpha]-calcium sulfate hemihydrate whisker is in a short rod shape, and the morphology is regular and controllable.

Description

technical field [0001] The invention relates to the technical field of gypsum material preparation, in particular to a method for preparing rod-shaped α-calcium sulfate hemihydrate whiskers. Background technique [0002] In the field of medicine and chemical industry, anhydrous sodium sulfate is widely used as desiccant and dehydrating agent, so a large amount of sodium sulfate solid waste containing crystal water is produced. Sodium sulfate solid waste produced by pharmaceutical and chemical industries generally contains residual solvents such as toluene, ethyl acetate, methylene chloride and petroleum ether. For example, in the production process of fine chemical products, strong acid replaces weak acid to produce sodium sulfate solid waste. For example, in the industrial production process of sebacic acid, about 30 tons of waste water needs to be discharged for every ton of sebacic acid produced. The main components contained in the waste water are sodium sulfate, phenol...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B29/46C30B29/62C30B7/14
CPCC30B7/14C30B29/46C30B29/62
Inventor 杨儒李天喜徐杰李松李敏赵国海张建宁史争光许垒
Owner 河南博海化工有限公司
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