CN114506872A - Method for preparing anhydrous gypsum at normal temperature and pressure - Google Patents

Method for preparing anhydrous gypsum at normal temperature and pressure Download PDF

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Publication number
CN114506872A
CN114506872A CN202210006295.8A CN202210006295A CN114506872A CN 114506872 A CN114506872 A CN 114506872A CN 202210006295 A CN202210006295 A CN 202210006295A CN 114506872 A CN114506872 A CN 114506872A
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China
Prior art keywords
gypsum
sulfuric acid
solid
acid solution
anhydrous gypsum
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Pending
Application number
CN202210006295.8A
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Chinese (zh)
Inventor
张静
王春雳
李文静
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University of Chinese Academy of Sciences
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University of Chinese Academy of Sciences
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Priority to CN202210006295.8A priority Critical patent/CN114506872A/en
Publication of CN114506872A publication Critical patent/CN114506872A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F11/00Compounds of calcium, strontium, or barium
    • C01F11/46Sulfates
    • C01F11/466Conversion of one form of calcium sulfate to another
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B11/00Calcium sulfate cements
    • C04B11/02Methods and apparatus for dehydrating gypsum
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/70Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/03Particle morphology depicted by an image obtained by SEM

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)

Abstract

The invention discloses a method for preparing anhydrous gypsum at normal temperature and normal pressure, and belongs to the technical field of gypsum production. The method comprises the following steps: selecting any hydrated gypsum as a raw material, and preparing a sulfuric acid solution with a certain concentration; fully wetting the hydrated gypsum by using a prepared sulfuric acid solution; reacting the fully wetted gypsum at normal temperature and normal pressure; and washing after the reaction is finished to obtain the anhydrous gypsum product. The method effectively reduces the energy consumption and the time consumption for dehydrating the hydrated gypsum and has higher social benefit and economic benefit.

Description

Method for preparing anhydrous gypsum at normal temperature and pressure
Technical Field
The invention belongs to the technical field of gypsum production, and particularly relates to a method for preparing anhydrous gypsum at normal temperature and normal pressure.
Background
Anhydrous gypsum is used in a wide variety of industries, for example, as a polishing powder, a paper filler, a gas desiccant, and a medical plaster bandage, and also in metallurgy, agriculture, and the like. Anhydrous gypsum can be crushed for soil treatment instead of gypsum, and one ton of anhydrous gypsum contains more calcium than one ton of gypsum during soil treatment because gypsum contains about 21% water. The anhydrous gypsum also has higher solubility, and is beneficial to the rapid absorption of calcium ions by soil. In addition, anhydrite is also used with gypsum as construction gypsum, joint compounds, wallboard, and other products. Anhydrite is also used as a source of sulfur in sulfuric acid production.
The traditional anhydrous gypsum production approaches are mainly to dehydrate hydrated gypsum and mine anhydrous gypsum raw ore under high temperature and high pressure, and have high requirements on equipment, complex operation and extremely high energy consumption, and the abundance of the anhydrous gypsum raw ore is far less than that of gypsum.
Disclosure of Invention
Aiming at the defects and shortcomings of the prior art, the invention aims to provide a gypsum dehydration method which is different from the high-temperature high-pressure method. The method provided by the invention is to wet the hydrated gypsum by a sulfuric acid solution at normal temperature and normal pressure to realize the phase change from gypsum to anhydrous gypsum. The method is simple to operate, and the solid product after phase change is washed by water or organic solution to obtain the anhydrous gypsum.
The technical scheme for solving the technical problems is as follows:
a process for preparing anhydrous gypsum at ordinary temp and pressure includes such steps as adding sulfuric acid solution to the surface of hydrated gypsum, laying aside to generate anhydrous gypsum, and washing the solid product with alcohol or methanol. The specific operation steps are as follows:
1. preparing 1-9 mol/kg of sulfuric acid solution, and wetting hydrated gypsum with the sulfuric acid solution to obtain a wetted solid;
2. standing the solid obtained in the step 1);
3. washing the solid after standing in the step 2) to obtain the anhydrous gypsum solid product.
Drawings
FIG. 1 is a SEM photograph of a sample before being processed in example 1 of the present invention.
FIG. 2 is an SEM photograph of the treated film of example 1.
FIG. 3 is a comparison graph of XRD and standard cards before treatment in examples 1-3 of the present invention, and PDF # 00-033-.
FIG. 4 is a comparison of XRD and standard card after treatment in examples 1-3 of the present invention, and PDF # 00-037-.
Detailed Description
The present invention will be further described with reference to the following examples, but the embodiments of the present invention are not limited thereto.
Example 1
A method for preparing anhydrous gypsum at normal temperature and normal pressure comprises the following specific operation steps:
0.1 g of dihydrate gypsum is wetted with 20 mu L of 1.8 mol/kg sulfuric acid solution, the solid-to-liquid ratio is 4.6, and the mixture is kept stand for 24 h at 25 ℃. The solid product obtained after standing was washed and subjected to the relevant SEM and XRD tests (figures 1-4). Test results show that the dihydrate gypsum is converted into an anhydrous gypsum phase under the action of interfacial sulfuric acid.
Example 2
A method for preparing anhydrous gypsum at normal temperature and normal pressure comprises the following specific operation steps:
0.1 g of dihydrate gypsum is wetted with 20 mu L of 3.2 mol/kg sulfuric acid solution with the solid-liquid ratio of 4.3, and is kept stand for 12 h at 25 ℃. The results of the tests show that dihydrate gypsum is converted into the anhydrous gypsum phase by the action of interfacial sulfuric acid (fig. 4).
Example 3
A method for preparing anhydrous gypsum at normal temperature and normal pressure comprises the following specific operation steps:
0.1 g of dihydrate gypsum is wetted with 20 mu L of 5.6 mol/kg sulfuric acid solution with the solid-liquid ratio of 3.8, and is kept stand for 4 h at 25 ℃. The results of the tests show that the dihydrate gypsum is converted into the anhydrous gypsum phase by the action of the interfacial sulfuric acid (figure 4).

Claims (6)

1. The method for preparing the anhydrous gypsum at normal temperature and normal pressure is characterized by comprising the following steps:
preparing a sulfuric acid solution, and wetting the hydrated gypsum solid;
standing the wetted solid of step 1);
washing the solid after standing in the step 2) to obtain the anhydrous gypsum solid product.
2. The method of claim 1, wherein: the hydrated gypsum comprises natural dihydrate or hemihydrate gypsum minerals; comprises flue gas desulfurization gypsum; including gypsum and calcined gypsum produced by natural sources, or the phosphate industry and some other industries.
3. The method as claimed in claim 1, wherein the concentration of sulfuric acid in the sulfuric acid solution in the step 1) is 1-9 mol/kg.
4. The method according to claim 1, wherein the solid-to-liquid ratio of the aqueous gypsum to the sulfuric acid solution in step 1) is 1:1 to 100: 1.
5. The method according to claim 1, wherein the standing temperature in the step 2) is 15-60 ℃ and the time is 0-36 hours.
6. The method of claim 1, wherein the washing solution of step 3) is ethanol or methanol.
CN202210006295.8A 2022-01-05 2022-01-05 Method for preparing anhydrous gypsum at normal temperature and pressure Pending CN114506872A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202210006295.8A CN114506872A (en) 2022-01-05 2022-01-05 Method for preparing anhydrous gypsum at normal temperature and pressure

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202210006295.8A CN114506872A (en) 2022-01-05 2022-01-05 Method for preparing anhydrous gypsum at normal temperature and pressure

Publications (1)

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CN114506872A true CN114506872A (en) 2022-05-17

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104529206A (en) * 2014-12-28 2015-04-22 北京工业大学 Method for preparing self-assembled flaky anhydrous gypsum on basis of desulfurized gypsum
JP2016138006A (en) * 2015-01-26 2016-08-04 住友大阪セメント株式会社 Method for producing anhydrous gypsum
CN109112635A (en) * 2018-08-10 2019-01-01 瓮福化工科技有限公司 A method of quickly preparing semi-hydrated gypsum whisker and anhydrous gypsum whisker using ardealite
CN110372236A (en) * 2019-08-14 2019-10-25 江苏一夫科技股份有限公司 A kind of Desulphurization prepares method of alpha semi-hydrated gypsum and products thereof
CN110395919A (en) * 2019-08-09 2019-11-01 中国科学院沈阳应用生态研究所 A kind of method that the gypsum resourceization containing arsenic is handled and the application for handling the low arsenic gypsum of gained
CN110629279A (en) * 2018-06-22 2019-12-31 北新集团建材股份有限公司 Self-assembled lamellar anhydrous gypsum single crystal material and preparation method thereof
KR102273096B1 (en) * 2020-12-24 2021-07-05 남해화학주식회사 Manufacturing method of anhydrous gypsum using byproduct gypsum

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104529206A (en) * 2014-12-28 2015-04-22 北京工业大学 Method for preparing self-assembled flaky anhydrous gypsum on basis of desulfurized gypsum
JP2016138006A (en) * 2015-01-26 2016-08-04 住友大阪セメント株式会社 Method for producing anhydrous gypsum
CN110629279A (en) * 2018-06-22 2019-12-31 北新集团建材股份有限公司 Self-assembled lamellar anhydrous gypsum single crystal material and preparation method thereof
CN109112635A (en) * 2018-08-10 2019-01-01 瓮福化工科技有限公司 A method of quickly preparing semi-hydrated gypsum whisker and anhydrous gypsum whisker using ardealite
CN110395919A (en) * 2019-08-09 2019-11-01 中国科学院沈阳应用生态研究所 A kind of method that the gypsum resourceization containing arsenic is handled and the application for handling the low arsenic gypsum of gained
CN110372236A (en) * 2019-08-14 2019-10-25 江苏一夫科技股份有限公司 A kind of Desulphurization prepares method of alpha semi-hydrated gypsum and products thereof
KR102273096B1 (en) * 2020-12-24 2021-07-05 남해화학주식회사 Manufacturing method of anhydrous gypsum using byproduct gypsum

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
吕智慧等: "一步常压酸化法制备无水硫酸钙晶须", 《无机盐工业》, pages 22 - 25 *

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