CN115974126A - Method for regulating and controlling crystal morphology of phosphogypsum-based calcium sulfate dihydrate - Google Patents

Method for regulating and controlling crystal morphology of phosphogypsum-based calcium sulfate dihydrate Download PDF

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CN115974126A
CN115974126A CN202211621346.4A CN202211621346A CN115974126A CN 115974126 A CN115974126 A CN 115974126A CN 202211621346 A CN202211621346 A CN 202211621346A CN 115974126 A CN115974126 A CN 115974126A
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phosphogypsum
calcium sulfate
sulfate dihydrate
regulating
stirring
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何敏
雷阳
刘玉飞
于杰
张凯
秦舒浩
龙雪彬
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Guizhou University
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Guizhou University
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00Technologies for solid waste management
    • Y02W30/50Reuse, recycling or recovery technologies
    • Y02W30/91Use of waste materials as fillers for mortars or concrete

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Abstract

The invention discloses a method for regulating and controlling the morphology of phosphogypsum-based calcium sulfate dihydrate crystals, which realizes the regulation and control of the morphology of the phosphogypsum-based calcium sulfate dihydrate crystals by regulating the types of anti-solvents and the reaction temperature, improves the added value of products, has obvious economic benefit and widens the use path of phosphogypsum.

Description

Method for regulating and controlling crystal morphology of phosphogypsum-based calcium sulfate dihydrate
Technical Field
The invention relates to a method for regulating and controlling the crystal morphology of phosphogypsum-based calcium sulfate dihydrate, belonging to the technical field of chemical raw material preparation.
Background
The phosphorus chemical industry is one of the national pillar industries, and produces solid waste phosphogypsum while bringing economic benefit, because the yield of the phosphogypsum is huge and the comprehensive utilization rate is low, the phosphogypsum is mainly stockpiled, and the stockpiling of the phosphogypsum not only occupies a large amount of land and wastes a large amount of economy, but also causes a series of environmental problems, so that the acid-base imbalance of the soil around the yard pollutes the farmland around the yard; the filtrate permeates into the underground water, so that the pollution of water resources is caused; because the output is huge, the dam of the storage yard is higher, so that the danger of dam break at any time exists, and the life safety of surrounding residents is threatened; currently, phosphogypsum is applied to the aspects of building materials, roadbeds, soil conditioners, chemical raw materials, polymer filling and the like, and the structure of the phosphogypsum is an important factor influencing the application of the phosphogypsum. Therefore, the phosphogypsum structure is regulated and controlled, and the additional value of the phosphogypsum structure is improved, so that the phosphogypsum resource utilization is of very important practical significance.
In phosphogypsum structure regulation, the structure of calcium sulfate dihydrate is usually regulated by using an atmospheric pressure acidification method, and a crystal form regulator (a crystallization promoter) is used for changing the crystal growth mode. Therefore, an anti-solvent method is provided for regulating and controlling the structure of the phosphogypsum, and the shape of the calcium sulfate dihydrate in the phosphogypsum is regulated and controlled by regulating the type of the anti-solvent and the reaction temperature.
Disclosure of Invention
The invention provides a novel method for adjusting phosphogypsum-based calcium sulfate dihydrate, prepares various phosphogypsum crystals with controllable shapes, solves the problem that the application field of the phosphogypsum is limited due to the shape of the phosphogypsum in the prior art, expands the application field of the phosphogypsum, and has the advantages of simple operation, environment-friendly solvent and obvious effect.
The technical scheme of the invention is as follows: a method for regulating and controlling crystal morphology of phosphogypsum-based calcium sulfate dihydrate comprises the following steps:
(1) Preparation of phosphogypsum solution: drying the phosphogypsum at 60 ℃, crushing the phosphogypsum, and sieving the crushed phosphogypsum with a 100-mesh sieve according to a solid-to-liquid ratio of 1: 100-500 dissolving the phosphogypsum in deionized water, stirring for a certain time at room temperature, and filtering out insoluble substances to obtain the phosphogypsum solution.
(2) And (3) regulation and control of the structure: putting a certain amount of phosphogypsum solution into a stirring and heating device, heating at the temperature of 1-75 ℃, stirring at the speed of 100-500 r/min, then adding aliphatic alcohol with the same temperature into the phosphogypsum solution, adding the aliphatic alcohol into the phosphogypsum solution by 20-100 percent, stirring and heating for 3-10 min, and filtering while the solution is hot to obtain a filter cake.
(3) And (3) drying: drying the obtained filter cake at 50-80 deg.c for 2-8 hr to obtain the product.
The invention has the beneficial effects that:
the method has the advantages of simple operation, environment-friendly solvent, obvious effect and larger specific surface area, and the obtained phosphogypsum-based calcium sulfate dihydrate crystal has good adsorption performance on metal ions in water.
Drawings
FIG. 1 is a flow chart of regulation;
FIG. 2 shows the morphology of a methanol 55 ℃ product;
FIG. 3 is a plot of ethanol 55 deg.C product;
FIG. 4 shows the morphology of n-propanol product at 55 ℃;
FIG. 5 shows the morphology of a 55 ℃ isopropanol product;
FIG. 6 shows the morphology of the isopropanol 15 ℃.
Figure 7 shows the specific surface area and adsorption performance of phosphogypsum-based calcium sulphate dihydrate crystals prepared by different anti-solvents.
Detailed Description
Example 1
A method for regulating and controlling the crystal morphology of phosphogypsum-based calcium sulfate dihydrate comprises the following steps:
(1) Preparation of phosphogypsum solution: drying the phosphogypsum at 60 ℃, crushing the phosphogypsum, and sieving the crushed phosphogypsum by a 100-mesh sieve according to a solid-liquid ratio of 1:200 dissolving the phosphogypsum in deionized water, stirring for 4hr at room temperature, and filtering out insoluble substances to obtain the phosphogypsum solution.
(2) And (3) regulation and control of the structure: putting a certain amount of phosphogypsum solution into a stirring and heating device, heating at 55 ℃, stirring at the speed of 200r/min, then adding methanol with the same temperature into the phosphogypsum solution, adding 30 percent of the phosphogypsum solution, stirring and heating for 5min, and filtering while hot to obtain a filter cake.
(3) And (3) drying: drying the obtained filter cake at 60 deg.C for 4hr to obtain the final product.
The obtained product is white powder, the microscopic morphology is butterfly-shaped sheet crystal, the length of the crystal is 30-100 mu m, the width is 20-30 mu m, and the thickness is 1-10 mu m; the ingredient is calcium sulfate dihydrate, and the whiteness is 90.60%. See figure 2
(4) The specific surface area and the adsorption performance of the obtained phosphogypsum-based calcium sulfate dihydrate crystal are shown in a figure 7.
Example 2
A method for regulating and controlling the crystal morphology of phosphogypsum-based calcium sulfate dihydrate comprises the following steps:
(1) Preparation of phosphogypsum solution: drying the phosphogypsum at 60 ℃, crushing the phosphogypsum, and sieving the crushed phosphogypsum by a 100-mesh sieve according to a solid-liquid ratio of 1:200 dissolving the phosphogypsum in deionized water, stirring for 4hr at room temperature, and filtering out insoluble substances to obtain the phosphogypsum solution.
(2) And (3) regulation and control of the structure: putting a certain amount of phosphogypsum solution in a stirring and heating device, heating at 55 ℃, stirring at the speed of 200r/min, then adding ethanol with the same temperature into the phosphogypsum solution, adding 30 percent of the phosphogypsum solution, stirring and heating for 5min, and filtering while hot to obtain a filter cake.
(3) And (3) drying: drying the obtained filter cake at 60 deg.C for 4hr to obtain the final product.
The obtained product is white powder, the microscopic morphology is coexistence of butterfly-shaped sheet crystals and columnar crystals, the length of the white butterfly-shaped sheet crystals is 30-150 mu m, the width is 20-30 mu m, and the thickness is 1-10 mu m; the length of the columnar crystal is 30-150 mu m, and the diameter is 3-mu m; the product component is calcium sulfate dihydrate, and the whiteness is 91.86%.
(4) The specific surface area and the adsorption performance of the obtained phosphogypsum-based calcium sulfate dihydrate crystal are shown in a figure 7.
Example 3
A method for regulating and controlling the crystal morphology of phosphogypsum-based calcium sulfate dihydrate comprises the following steps:
(1) Preparation of phosphogypsum solution: drying the phosphogypsum at 60 ℃, crushing the phosphogypsum, and sieving the crushed phosphogypsum by a 100-mesh sieve according to a solid-liquid ratio of 1:200 dissolving the phosphogypsum in deionized water, stirring for 4hr at room temperature, and filtering out insoluble substances to obtain the phosphogypsum solution.
(2) And (3) regulation and control of the structure: putting a certain amount of phosphogypsum solution into a stirring and heating device, heating at 55 ℃, stirring at the speed of 200r/min, then adding n-propanol with the same temperature into the phosphogypsum solution, adding 30% of the phosphogypsum solution, stirring and heating for 5min, and filtering while hot to obtain a filter cake.
(3) And (3) drying: drying the obtained filter cake at 60 deg.C for 4hr to obtain the final product.
The obtained product is white powder, the micro appearance is hexagonal prism-shaped crystal, the length is 5-50 mu m, and the diameter is 1-2 mu m; the product component is calcium sulfate dihydrate, and the whiteness is 96.26%.
Example 4
A method for regulating and controlling the crystal morphology of phosphogypsum-based calcium sulfate dihydrate comprises the following steps:
(1) Preparation of phosphogypsum solution: drying the phosphogypsum at 60 ℃, crushing the phosphogypsum, and sieving the crushed phosphogypsum by a 100-mesh sieve according to a solid-liquid ratio of 1:200 dissolving the phosphogypsum in deionized water, stirring for 4hr at room temperature, and filtering out insoluble substances to obtain the phosphogypsum solution.
(2) And (3) regulation and control of the structure: putting a certain amount of phosphogypsum solution into a stirring and heating device, heating at 55 ℃, stirring at the speed of 200r/min, then adding isopropanol at the same temperature into the phosphogypsum solution, adding 30 percent of the phosphogypsum solution, stirring and heating for 5min, and filtering while hot to obtain a filter cake.
(3) And (3) drying: drying the obtained filter cake at 60 deg.C for 4hr to obtain the final product.
The obtained product is white powder, the micro appearance is hexagonal prism-shaped crystal, the length is 10-70 μm, and the diameter is 1-2 μm; the product component is calcium sulfate dihydrate, and the whiteness is 95.93%.
(4) The specific surface area and the adsorption performance of the obtained phosphogypsum-based calcium sulfate dihydrate crystal are shown in a figure 7.
Example 5
A method for regulating and controlling the crystal morphology of phosphogypsum-based calcium sulfate dihydrate comprises the following steps:
(1) Preparation of phosphogypsum solution: drying the phosphogypsum at 60 ℃, crushing the phosphogypsum, and sieving the crushed phosphogypsum with a 100-mesh sieve according to a solid-to-liquid ratio of 1:200 dissolving the phosphogypsum in deionized water, stirring for 4hr at room temperature, and filtering out insoluble substances to obtain the phosphogypsum solution.
(2) And (3) regulation and control of the structure: putting a certain amount of phosphogypsum solution into a stirring and heating device, heating at 15 ℃, stirring at the speed of 200r/min, adding n-propanol with the same temperature into the phosphogypsum solution, adding 30% of the phosphogypsum solution, stirring and heating for 5min, and filtering to obtain a filter cake.
(3) And (3) drying: drying the obtained filter cake at 60 deg.C for 4hr to obtain the final product.
The obtained product is white powder, the microscopic appearance is hexagonal prism-shaped crystal, the length is 1-5 mu m, and the diameter is 0.1-0.3 mu m; the product component is calcium sulfate dihydrate, and the whiteness is 95.74%.

Claims (9)

1. A method for regulating and controlling a crystal structure of phosphogypsum-based calcium sulfate dihydrate is characterized by comprising the following steps: mixing, stirring and heating phosphogypsum serving as a calcium sulfate dihydrate source, water serving as a phosphogypsum solvent and aliphatic alcohol serving as an anti-solvent to obtain the phosphogypsum-calcium-phosphate composite material.
2. The method for regulating and controlling the crystal morphology of phosphogypsum-based calcium sulfate dihydrate according to claim 1, which is characterized in that: the method comprises the following steps:
(1) Preparation of phosphogypsum solution: drying the phosphogypsum according to the solid-liquid ratio of 1: dissolving 100-500 parts of the raw materials in deionized water, stirring at room temperature, and filtering insoluble substances to obtain a phosphogypsum solution;
(2) And (3) regulation and control of the structure: placing the phosphogypsum solution in a stirring and heating device, heating at the temperature of 1-75 ℃, stirring at the speed of 100-500 r/min, adding aliphatic alcohol with the same temperature into the phosphogypsum solution, adding the aliphatic alcohol into the phosphogypsum solution by 20-100 percent, stirring and heating for 3-10 min, and filtering while hot to obtain a filter cake;
(3) And (3) drying: and drying the obtained filter cake at 50-80 ℃ for 2-8 h to obtain the product.
3. The method for regulating and controlling the crystal morphology of phosphogypsum-based calcium sulfate dihydrate according to claim 2, which is characterized in that: in the step (1), the solid-liquid ratio is 1:200.
4. the method for regulating and controlling the crystal morphology of phosphogypsum-based calcium sulfate dihydrate according to claim 2, which is characterized in that: in the step (1), the stirring time at room temperature is 4h.
5. The method for regulating and controlling the crystal morphology of phosphogypsum-based calcium sulfate dihydrate according to claim 2, characterized in that: in the step (2), the heating temperature is 55 ℃.
6. The method for regulating and controlling the crystal morphology of phosphogypsum-based calcium sulfate dihydrate according to claim 2, which is characterized in that: in the step (2), the stirring speed is 200r/min.
7. The method for regulating and controlling the crystal morphology of phosphogypsum-based calcium sulfate dihydrate according to claim 2, characterized in that: in the step (2), the addition amount of the fatty alcohol is 30% of the phosphogypsum solution.
8. The method for regulating and controlling the crystal morphology of phosphogypsum-based calcium sulfate dihydrate according to claim 2, characterized in that: in the step (2), the stirring and heating time is 5min.
9. The method for regulating and controlling the crystal morphology of phosphogypsum-based calcium sulfate dihydrate according to claim 2, which is characterized in that: in the step (3), the drying time is 4h.
CN202211621346.4A 2022-12-16 2022-12-16 Method for regulating and controlling crystal morphology of phosphogypsum-based calcium sulfate dihydrate Pending CN115974126A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104005086A (en) * 2014-04-04 2014-08-27 贵阳中化开磷化肥有限公司 Method for preparing calcium sulfate dihydrate crystal whisker from phosphorus gypsum
US20180273384A1 (en) * 2015-09-18 2018-09-27 Kingenta Norsterra Chemical Co., Ltd. Method for producing wet-process phosphoric acid and by-producing alpha-hemihydrate gypsum and high-purity and high-whiteness alpha-hemihydrate gypsum
CN111850698A (en) * 2020-07-21 2020-10-30 上海畅清生态环境科技有限公司 Phosphogypsum whisker and preparation method thereof
CN114940508A (en) * 2022-06-20 2022-08-26 湖北三峡实验室 Process for settling and purifying phosphogypsum

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104005086A (en) * 2014-04-04 2014-08-27 贵阳中化开磷化肥有限公司 Method for preparing calcium sulfate dihydrate crystal whisker from phosphorus gypsum
US20180273384A1 (en) * 2015-09-18 2018-09-27 Kingenta Norsterra Chemical Co., Ltd. Method for producing wet-process phosphoric acid and by-producing alpha-hemihydrate gypsum and high-purity and high-whiteness alpha-hemihydrate gypsum
CN111850698A (en) * 2020-07-21 2020-10-30 上海畅清生态环境科技有限公司 Phosphogypsum whisker and preparation method thereof
CN114940508A (en) * 2022-06-20 2022-08-26 湖北三峡实验室 Process for settling and purifying phosphogypsum

Non-Patent Citations (1)

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Title
周华锋;张肖肖;李响;: "磷石膏制备硫酸钙晶须的工艺研究", 硅酸盐通报, no. 06, 15 June 2017 (2017-06-15), pages 285 - 289 *

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