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A kind of preparation method of rod-shaped α-calcium sulfate hemihydrate whisker

A calcium sulfate hemihydrate and rod-shaped technology is applied in the field of preparation of rod-shaped α-calcium sulfate hemihydrate whiskers, which 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 low synthesis temperature

Active Publication Date: 2020-09-04
河南博海化工有限公司 +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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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  • A kind of preparation method of rod-shaped α-calcium sulfate hemihydrate whisker
  • A kind of preparation method of rod-shaped α-calcium sulfate hemihydrate whisker
  • A kind of preparation method of rod-shaped α-calcium sulfate hemihydrate whisker

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Embodiment 1

[0052] This embodiment provides a method for preparing rod-shaped α-calcium sulfate hemihydrate whiskers, which includes the following steps:

[0053] 1) Take the solid waste of sodium sulfate, calcinate in a calciner to remove organic residues, calcining temperature 700℃, calcining time 3 hours; after calcining, dissolve the calcined sodium sulfate with water, filter to remove inorganic insolubles, and make 2.0 mol / L sodium sulfate aqueous solution;

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

[0055] 3) After the reaction is completed, let it stand and age for 30h to obtain the crude rod-shaped α-calcium sulfate hemihydrate whisker. Wash the rod-shap...

Embodiment 2

[0061] This embodiment provides a method for preparing rod-shaped α-calcium sulfate hemihydrate whiskers, which includes the following steps:

[0062] 1) Take sodium sulfate solid waste, calcined in a calciner to remove organic residues, calcining temperature is 800℃, calcining time is 1 hour; after calcining, dissolve the calcined sodium sulfate with water, filter to remove inorganic insolubles to make 2.0 mol / L sodium sulfate aqueous solution;

[0063] 2) Measure 335ml (0.67mol) of 2.0mol / L sodium sulfate aqueous solution in the reaction vessel, then add 20.28g of phthalic anhydride, heat and stir to raise the temperature to 105°C, slowly add 117ml (0.70mol) of 6mol / L calcium nitrate aqueous solution ), the feeding speed is 7.5ml / min, after the calcium nitrate aqueous solution has been fed, continue to stir and react at 105°C for 3h;

[0064] 3) After the reaction is completed, let stand and age for 15 hours to obtain the crude α-calcium sulfate hemihydrate whiskers. Wash the crud...

Embodiment 3

[0067] This embodiment provides a method for preparing rod-shaped α-calcium sulfate hemihydrate whiskers, which includes the following steps:

[0068] 1) Take sodium sulfate solid waste, calcined in a calciner to remove organic residues, calcining temperature is 500℃, calcining time is 24 hours; after calcining, dissolve the calcined sodium sulfate with water, filter to remove inorganic insolubles to make 1.0 mol / L sodium sulfate aqueous solution;

[0069] 2) Measure 400ml (0.4mol) of 1.0mol / L sodium sulfate aqueous solution in the reaction vessel, then add 1.15g of sodium benzoate, heat and stir to raise the temperature to 90℃, slowly add 3.5mol / L calcium nitrate aqueous solution 91.4ml (0.32mol) , The feeding rate 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, let stand for 24 hours to obtain the crude rod-shaped α-calcium sulfate hemihydrate whisker. Wash the rod-shaped crud...

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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 pharmaceutical and chemical industry, anhydrous sodium sulfate is widely used as a desiccant and dehydrating agent, so a large amount of sodium sulfate solid waste containing crystal water is generated. The sodium sulfate solid waste produced by the pharmaceutical and chemical industry generally contains residual solvents such as toluene, ethyl acetate, dichloromethane 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, for every ton of sebacic acid produced at present, about 30 tons of wastewater needs to be discharged. The main components in the wastewater are sodium sulfate, phenol, ...

Claims

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Application Information

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Patent Type & Authority Patents(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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