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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gypsum
sulfuric acid
solid
acid solution
normal temperature
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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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    • 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

一种常温常压制备无水石膏的方法A kind of method for preparing anhydrite at normal temperature and normal pressure

技术领域technical field

本发明属于石膏生产技术领域,具体涉及一种常温常压制备无水石膏的方法。The invention belongs to the technical field of gypsum production, and in particular relates to a method for preparing anhydrite at normal temperature and pressure.

背景技术Background technique

无水石膏在各种工业中用途广泛,例如可用作磨光粉、纸张填充物、气体干燥剂以及医疗上的石膏绷带,也能用于冶金、农业等方面。无水石膏可以替代石膏被压碎用作土壤处理,而且在土壤处理过程中,一吨无水石膏比一吨石膏含有更多的钙,因为石膏中含有大约21%的水。无水石膏还具有更高的溶解度,有助于土壤对钙离子的迅速吸收。此外无水石膏还与石膏一起用作建筑行业石膏,接缝化合物,墙板和其他产品。在硫酸生产中,硬石膏也被用作硫的来源。Anhydrite is widely used in various industries, such as polishing powder, paper filler, gas desiccant, and medical gypsum bandage, as well as metallurgy, agriculture, etc. Anhydrite can be crushed in place of gypsum for soil treatment, and during soil treatment, a ton of anhydrite contains more calcium than a ton of gypsum because gypsum contains about 21% water. Anhydrite also has a higher solubility, which aids the rapid absorption of calcium ions by the soil. In addition, anhydrite is used with gypsum as gypsum in the construction industry, joint compound, wallboard and other products. In sulfuric acid production, anhydrite is also used as a source of sulfur.

传统无水石膏生产途径主要是在高温高压下脱水水合石膏和开采无水石膏原矿,这些途径对设备要求高,操作复杂,能耗极大,且无水石膏原矿丰度远不如石膏。The traditional anhydrite production methods are mainly dehydrating hydrated gypsum under high temperature and high pressure and mining anhydrite raw ore. These methods have high equipment requirements, complex operation, huge energy consumption, and the abundance of anhydrite raw ore is far less than that of gypsum.

发明内容SUMMARY OF THE INVENTION

针对现有技术存在的缺点和不足之处,本发明的目的是提供一种有别于上述高温高压法的石膏脱水方法。本发明所提供的方法是在常温常压下,通过硫酸溶液润湿水合石膏,实现石膏向无水石膏的相变。本发明操作简单,相变后固体产物用水或有机溶液洗涤即可得到无水石膏。In view of the shortcomings and deficiencies existing in the prior art, the purpose of the present invention is to provide a gypsum dehydration method different from the above-mentioned high temperature and high pressure method. The method provided by the invention is to wet the hydrated gypsum with a sulfuric acid solution under normal temperature and normal pressure, so as to realize the phase transition from gypsum to anhydrite. The method is simple to operate, and the solid product after phase transition can be washed with water or organic solution to obtain anhydrite.

本发明解决上述技术问题的技术方案如下:The technical scheme that the present invention solves the above-mentioned technical problems is as follows:

一种常温常压制备无水石膏的方法,在室温条件下,将硫酸溶液加在水合石膏表面,静置生成无水石膏,用乙醇或甲醇洗涤固体产物即可得到无水石膏。具体操作步骤如下:A method for preparing anhydrous gypsum at room temperature and normal pressure, adding sulfuric acid solution on the surface of hydrated gypsum at room temperature, standing to generate anhydrite, and washing the solid product with ethanol or methanol to obtain anhydrite. The specific operation steps are as follows:

1.配制1~9 mol/kg的硫酸溶液,用其润湿水合石膏,得到润湿的固体;1. Prepare the sulfuric acid solution of 1~9 mol/kg, and use it to wet the hydrated gypsum to obtain the wetted solid;

2.静置步骤1)所得固体;2. Let stand the solid obtained in step 1);

3.洗涤步骤2)静置后的固体,得到产物无水石膏固体产物。3. Wash the solid after standing in step 2) to obtain the product anhydrite solid product.

附图说明Description of drawings

图1为本发明实施例1处理前的SEM图。Fig. 1 is the SEM image of Example 1 of the present invention before treatment.

图2为本发明实施例1处理后的SEM图。FIG. 2 is the SEM image after the treatment of Example 1 of the present invention.

图3为本发明实施例1-3处理前的XRD与标准卡片的对比图,PDF#00-033-0311为二水石膏的标准卡片,从图中可以产出处理前的主要物相为二水石膏。Figure 3 is a comparison diagram of the XRD and standard cards before treatment in Example 1-3 of the present invention. PDF#00-033-0311 is a standard card of dihydrate gypsum. From the figure, it can be seen that the main phases before treatment are two Gypsum.

图4为本发明实施例1-3处理后的XRD与标准卡片的对比图,PDF#00-037-1496为无水石膏的标准卡片,从图中可以产出处理后的主要物相为无水石膏。Figure 4 is a comparison diagram of the XRD and standard cards after treatment in Examples 1-3 of the present invention, PDF#00-037-1496 is a standard card of anhydrite, and it can be seen from the figure that the main phase after treatment is no Gypsum.

具体实施方式Detailed ways

以下结合实施例对本发明作进一步地说明,但本发明的实施方式不限于此。The present invention will be further described below with reference to the examples, but the embodiments of the present invention are not limited thereto.

实施例1Example 1

一种常温常压制备无水石膏的方法,具体操作步骤如下:A method for preparing anhydrite at normal temperature and pressure, the specific operation steps are as follows:

取0.1 g的二水石膏,用20 μL 1.8 mol/kg的硫酸溶液将其润湿,固液比4.6,25℃静置24 h。对静置后得到的固体产物洗涤后进行相关SEM和XRD测试(附图说明图1-图4)。试验结果表明,二水石膏在界面硫酸作用下转变为无水石膏相。Take 0.1 g of gypsum dihydrate and wet it with 20 μL of 1.8 mol/kg sulfuric acid solution, with a solid-liquid ratio of 4.6, and let it stand at 25 °C for 24 h. The solid product obtained after standing was washed and then subjected to relevant SEM and XRD tests (description of drawings Fig. 1-Fig. 4). The experimental results show that the dihydrate gypsum is transformed into anhydrous gypsum phase under the action of interfacial sulfuric acid.

实施例2Example 2

一种常温常压制备无水石膏的方法,具体操作步骤如下:A method for preparing anhydrite at normal temperature and pressure, the specific operation steps are as follows:

取0.1 g的二水石膏,用20 μL 3.2 mol/kg的硫酸溶液将其润湿,固液比为4.3,25℃静置12 h。试验结果表明,二水石膏在界面硫酸作用下转变为无水石膏相 (图4)。Take 0.1 g of gypsum dihydrate, wet it with 20 μL of 3.2 mol/kg sulfuric acid solution, the solid-liquid ratio is 4.3, and stand at 25 °C for 12 h. The experimental results showed that the dihydrate gypsum was transformed into the anhydrite phase under the action of interfacial sulfuric acid (Fig. 4).

实施例3Example 3

一种常温常压制备无水石膏的方法,具体操作步骤如下:A method for preparing anhydrite at normal temperature and pressure, the specific operation steps are as follows:

取0.1 g的二水石膏,用20 μL 5.6 mol/kg的硫酸溶液将其润湿,固液比为3.8,25℃静置4 h。试验结果表明,二水石膏在界面硫酸作用下转变为无水石膏相(图4)。Take 0.1 g of gypsum dihydrate, wet it with 20 μL of 5.6 mol/kg sulfuric acid solution, the solid-liquid ratio is 3.8, and let it stand at 25 °C for 4 h. The experimental results showed that the dihydrate gypsum was transformed into anhydrous gypsum phase under the action of interfacial sulfuric acid (Fig. 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)

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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 method for recycling arsenic-containing gypsum and the application of the obtained low-arsenic 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
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 method for recycling arsenic-containing gypsum and the application of the obtained low-arsenic gypsum
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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Application publication date: 20220517