Preparation method of large-particle spherical sodium sulfate crystals

A sodium sulfate and large particle technology, applied in the preparation form of alkali metal sulfite/sulfate, chemical instruments and methods, selection of crystallization auxiliary conditions, etc., can solve the problem of difficult to stably control the nucleation and growth of sodium sulfate, increase equipment Cost and production costs, uneven product particle size distribution, etc., to achieve the effect of increasing added value, good filtration performance and anti-caking performance, and improving anti-caking performance

Pending Publication Date: 2020-09-15
云南省盐业有限公司 +2
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

Patent CN110217805A uses the method of adding seed crystals to prepare large-particle sodium sulfate, but this method is difficult to stably control the nucleation and growth of sodium sulfate, resulting in uneven particle size distribution of the product. Only through primary cyclone separation can large-particle sodium sulfate be obtained product, which increases equipment costs and production costs
Patent CN101007640A prepares large particle sodium sulfate by adding solid surfactant, and the product above 40 mesh (425um) can reach 80%, but introduces solid impurity in the production process, causes the reduction of product quality
[0004] The preparation method of above report all devotes oneself to improving the particle size of sodium sulfate, but is difficult in the situation that does not introduce solid impurity, obtains the large granular sodium sulfate product of uniform particle size
Moreover, simply increasing the particle size of sodium sulfate cannot solve the problem of its easy caking

Method used

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  • Preparation method of large-particle spherical sodium sulfate crystals
  • Preparation method of large-particle spherical sodium sulfate crystals
  • Preparation method of large-particle spherical sodium sulfate crystals

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] (1) At 35°C, add 10.5g of sodium sulfate to 35.0g of water (the volume of the solute sodium sulfate is 3.92cm 3 ), configure sodium sulfate aqueous solution.

[0037] (2) At 35° C., 35.0 g of methanol and 3.92 mL of dichloromethane were mixed to prepare a methanol-dichloromethane mixed solvent.

[0038] (3) Add the sodium sulfate aqueous solution dropwise into the methanol-dichloromethane mixed solvent at a rate of 1% / min, and keep stirring at a stirring rate of 300 rpm; after the dropwise addition, keep stirring for 5 hours.

[0039] (4) Filtrate, wash with ethanol with a mass fraction of 95%, and dry at normal pressure at 40° C. for 12 hours to obtain large spherical sodium sulfate crystals.

[0040] Photos of large spherical sodium sulfate crystals as figure 1 As shown, the optical microscope photographs are as figure 2 As shown in the scanning electron micrograph image 3 As shown, its average particle size is 850 microns, the angle of repose is 29°, the residual...

Embodiment 2

[0042] (1) At 40°C, add 14.0g of sodium sulfate to 35.0g of water (the volume of the solute sodium sulfate is 5.22cm 3 ), configure sodium sulfate aqueous solution.

[0043] (2) At 40° C., 70.0 g of ethanol was mixed with 2.61 mL of dichloromethane to prepare a mixed solvent of ethanol-dichloromethane.

[0044] (3) Add the sodium sulfate aqueous solution dropwise into the ethanol-dichloromethane mixed solvent at a rate of 2% / min, and keep stirring at a stirring rate of 500 rpm; after the dropwise addition, keep stirring for 1 h.

[0045] (4) Filtrate, wash with ethanol with a mass fraction of 70%, and dry at normal pressure at 50° C. for 6 hours to obtain large spherical sodium sulfate crystals.

[0046] The average particle size of the spherical particles is 650 microns, the angle of repose is 31°, the residual solvent after filtration is 2.3%, and the caking rate is 3.5%.

Embodiment 3

[0048] (1) At 45°C, add 7.0g of sodium sulfate to 35.0g of water (the volume of the solute sodium sulfate is 2.61cm 3 ), configure sodium sulfate aqueous solution.

[0049] (2) At 45° C., 70.0 g of n-propanol and 2.09 mL of n-hexane were mixed to prepare a n-propanol-n-hexane mixed solvent.

[0050] (3) Add the sodium sulfate aqueous solution dropwise into the n-propanol-n-hexane mixed solvent at a rate of 0.5% / min, and keep stirring at a stirring rate of 400 rpm; after the dropwise addition, keep stirring for 4 hours.

[0051] (4) Filtrate, wash with ethanol with a mass fraction of 95%, and dry at normal pressure at 50° C. for 24 hours to obtain large spherical sodium sulfate crystals.

[0052] The average particle size of the spherical particles is 730 microns, the angle of repose is 30°, the residual solvent after filtration is 1.7%, and the caking rate is 4.8%.

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Abstract

The invention discloses a preparation method of large-particle spherical sodium sulfate crystals. The preparation method comprises the following steps: at 35-50 DEG C, preparing a sodium sulfate aqueous solution with a certain concentration, wherein the mass ratio of solute sodium sulfate to water is 0.2: 1 to 0.45: 1; preparing a mixed solvent of an organic solvent and a bridging agent at the same temperature, wherein the mass ratio of the organic solvent to water is 1: 1 to 3: 1, and the volume ratio of the bridging agent to solute sodium sulfate is 0.5: 1 to 1: 1; then, dropwise adding a sodium sulfate aqueous solution into the organic solvent-bridging agent mixed solvent at a speed of 0.5-4%/min to separate out crystals, and continuously stirring; and after dropwise adding, keeping stirring for 0.5-5 hours; and filtering, washing and drying to obtain the spherical sodium sulfate crystals. The sodium sulfate crystals prepared by the method are good in sphericity degree and large inparticle size, and the average particle size is greater than 600 [mu]m; and the filtering performance is good, the flowability is high, caking is not likely to happen, the product production efficiency can be improved, and the caking phenomenon in transportation and storage is reduced.

Description

technical field [0001] The invention belongs to the technical field of chemical engineering industrial crystallization, and in particular relates to a preparation method of large-particle spherical sodium sulfate crystals. Background technique [0002] Sodium sulfate (CAS: 7757-82-6), molecular formula Na 2 SO 4 , also known as Yuanmingfen, is a basic inorganic chemical product. Sodium sulfate is an important raw material in the process of synthetic detergent, paper making and glass making. It is also widely used in the production of dyes, feed and pharmaceutical products, and it is also a commonly used desiccant in laboratories. In recent years, with the continuous upgrading and development of downstream industries, the market demand for special sodium sulfate is increasing day by day. Large particle sodium sulfate is favored by the market due to its unique advantages such as beautiful appearance, easy electrolysis, easy separation from mother liquor, and convenient washi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01D5/00B01D9/02
CPCB01D9/005C01D5/002C01D5/004C01P2004/32C01P2004/60C01P2006/80
Inventor 龚俊波王烁王显军黄孟阳汤伟伟刘烨陈明洋张明宇王静康荀春尹秋响张国莹侯宝红
Owner 云南省盐业有限公司
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