CN115594210A - Method and equipment for preparing calcium sulfate whisker by using ammonia-soda alkaline residue water - Google Patents

Method and equipment for preparing calcium sulfate whisker by using ammonia-soda alkaline residue water Download PDF

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Publication number
CN115594210A
CN115594210A CN202211029371.3A CN202211029371A CN115594210A CN 115594210 A CN115594210 A CN 115594210A CN 202211029371 A CN202211029371 A CN 202211029371A CN 115594210 A CN115594210 A CN 115594210A
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China
Prior art keywords
ammonia
soda
calcium sulfate
alkaline residue
drying
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CN202211029371.3A
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Chinese (zh)
Inventor
关祥瑞
范明磊
关方
刘胜飞
王倩
曹战国
宁长春
郑东新
刘志军
张陆顺
张景云
李雪瞻
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Priority to CN202211029371.3A priority Critical patent/CN115594210A/en
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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

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

Abstract

The invention relates to a method and equipment for preparing calcium sulfate whiskers by using ammonia-soda alkaline residue water, belongs to the technical field of ammonia-soda alkaline residue treatment, and particularly relates to a method for industrially producing calcium sulfate whiskers by using waste acid, alkali and ammonia-soda alkaline residue. The method comprehensively utilizes various components of the caustic sludge, changes waste into valuable, achieves zero emission, and solves the problem of environmental pollution caused by the caustic sludge. The method for preparing the calcium sulfate whisker has simple process and easy realization, and can be applied to batch production.

Description

Method and equipment for preparing calcium sulfate whisker by using ammonia-soda alkaline residue water
Technical Field
The invention relates to a method and equipment for preparing calcium sulfate whiskers by using ammonia-soda alkaline residue water, belongs to the technical field of ammonia-soda alkaline residue treatment, and particularly relates to a method for industrially producing calcium sulfate whiskers by using waste acid, alkali and ammonia-soda alkaline residue.
Background
The production capacity of the enterprises for producing the sodium carbonate by the ammonia-soda process accounts for 46 percent of the whole country (about 1000 ten thousand tons per year), and a large amount of alkali residues and waste liquid are discharged every year, thereby seriously polluting the environment and damaging the growth of crops. Aiming at the practical problem, the enterprises for producing soda ash by the ammonia-soda process adopt a series of solutions, such as: building cofferdam, repairing dam, changing equipment and adjusting process, but the discharge scale of waste liquid and waste caustic sludge can not be changed fundamentally. The reason for this is that the "ammonia-soda process" alkali production process discharges 10 tons of waste liquid and waste caustic sludge for every ton of soda ash produced. The price of soda is only about 2000 yuan per ton, and the high cost for treating 10 cubic meters of waste liquid and waste caustic sludge cannot be borne. In ammonia-soda production enterprises, the comprehensive utilization of caustic sludge is a problem to be solved urgently.
The Shandong building material academy and the Shandong ocean chemical group alkali-making company cooperate together to successfully extract special calcium carbonate from secondary salt mud, and the special calcium carbonate is identified by provincial technology, produced in batches and put on the market; research on extracting light magnesium oxide from primary salty mud is successful in laboratory expansion experiments, and pilot-scale production is currently planned through identification of science committee in Shandong province; the development and research of extracting the remainder of light magnesium oxide from primary salt slurry for manufacturing cement or building cementing materials have also made great progress.
The project of Xinjiang Tianye (group) Tianneng chemical industry limited company for preparing ceramsite by taking alkaline residue as a raw material is in a pilot-scale test stage, and the ceramsite can be widely used in the aspects of building heat preservation, building material production, water treatment filter materials, soilless culture base materials and the like.
However, how to comprehensively utilize various components of the caustic sludge is still an unsolved technical problem in the field. The research provides a method and equipment for industrially producing calcium sulfate whiskers by using waste acid, alkali and ammonia-alkali alkaline residue, aiming at various components of the alkaline residue, the method and the equipment are comprehensively utilized, waste is changed into valuable, zero emission is achieved, and the problem of environmental pollution caused by the alkaline residue is solved.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a method and equipment for preparing calcium sulfate whiskers by using ammonia alkali slag water, which comprehensively utilize various components of alkali slag, change waste into valuable, achieve zero emission and solve the problem of environmental pollution caused by the alkali slag.
In order to realize the aim, the invention provides a method for preparing calcium sulfate whiskers by using ammonia-soda alkaline residue water, which uses the ammonia-soda alkaline residue water and concentrated sulfuric acid as raw materials; the method comprises the following steps:
heating the ammonia-soda residue water to 50-60 ℃, mixing the ammonia-soda residue water with concentrated sulfuric acid until the pH value is 7, standing for 5-6h, filtering to obtain an eleventh filtrate and an eleventh filter cake, washing the obtained eleventh filter cake for 1-2 times by using deionized water, and drying to obtain calcium sulfate whiskers, wherein the drying procedure comprises the steps of drying at 100-110 ℃ for 1-2h at first, and then drying at 170-180 ℃ for 1-2h, and the obtained eleventh filtrate is a sodium chloride aqueous solution, can be directly discharged, and can also be used for ammonia-soda production process, salt dissolving and brine refining sections;
an apparatus for preparing calcium sulfate whisker by using ammonia-soda residue water comprises a material mixer, a filter and an oven;
the material mixer is used for mixing materials;
the filter is used for separating materials to obtain filtrate and filter cakes;
the oven is used for drying the materials.
Advantageous effects
The method for preparing the calcium sulfate whisker has simple process and easy realization, and can be applied to batch production.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the description is intended to be exemplary only, and is not intended to limit the scope of the present invention. Moreover, in the following description, descriptions of well-known structures and techniques are omitted so as to not unnecessarily obscure the concepts of the present invention.
The composition of the alkaline residue obtained by the ammonia-soda process of Sanyou chemical Co., ltd, tangshan is shown in Table 1 after being analyzed by the inspection center of Tianjin chemical research and design institute.
TABLE 1 analysis of alkaline residue composition
Alkaline residue composition Sample 1% by weight Sample 2% by weight Sample 3% by weight Sample 4% by weight
Calcium sulfate 17.3 3 15 3
Calcium carbonate 21.2 64 20 64
Calcium oxide 5.7 8 8
Calcium chloride 22.5 6 3 6
Sodium chloride 3.1 4 10 4
Calcium hydroxide 6.5 10 5 10
Magnesium hydroxide 8.9 27
Silicon dioxide 8.0 3 6 3
Alumina oxide 2.5 2 2 2
Iron oxide 1
Acid insoluble substance 4.3 8 2 8
The method comprehensively utilizes the alkaline residue of the ammonia-soda process, completely recycles the alkaline residue and the wastewater for conveying the alkaline residue, has no pollutant discharge in the whole process, and can realize automatic control and continuous production.
Examples
A method for preparing calcium sulfate whisker by using ammonia-soda alkaline residue water uses the raw materials of ammonia-soda alkaline residue water and concentrated sulfuric acid; the method comprises the following steps:
heating the ammonia-soda ash residue water to 60 ℃, mixing the ammonia-soda ash residue water with concentrated sulfuric acid until the pH value is 7, standing for 5h, filtering to obtain an eleventh filtrate and an eleventh filter cake, washing the obtained eleventh filter cake for 2 times by using deionized water, and drying to obtain calcium sulfate whiskers, wherein the drying procedure comprises the steps of drying at 100 ℃ for 2h at first, and then drying at 175 ℃ for 1.5h, and the obtained eleventh filtrate is a sodium chloride aqueous solution, can be directly discharged, and can also be used in the ammonia-soda production process, salt dissolving and brine refining section;
the obtained calcium sulfate whisker meets the DB43/T1155-2016 calcium sulfate whisker standard (technical supervision agency in Hunan province).
An apparatus for preparing calcium sulfate whisker by utilizing ammonia-soda slag water comprises a material mixer, a filter and an oven;
the material mixer is used for mixing materials;
the filter is used for separating materials to obtain filtrate and filter cakes;
the oven is used for drying the materials.
It is to be understood that the above-described embodiments of the present invention are merely illustrative of or explaining the principles of the invention and are not to be construed as limiting the invention. Therefore, any modification, equivalent replacement, improvement and the like made without departing from the spirit and scope of the present invention should be included in the protection scope of the present invention. Further, it is intended that the appended claims cover all such variations and modifications as fall within the scope and boundaries of the appended claims or the equivalents of such scope and boundaries.

Claims (3)

1. A method for preparing calcium sulfate whiskers by using ammonia-soda caustic sludge water is characterized by comprising the following steps:
the raw materials used in the method are ammonia-soda alkaline residue water and concentrated sulfuric acid; the method comprises the following steps:
heating the ammonia-soda residue water to 50-60 ℃, mixing the ammonia-soda residue water with concentrated sulfuric acid until the pH value is 7, standing for 5-6h, filtering to obtain an eleventh filtrate and an eleventh filter cake, washing the obtained eleventh filter cake for 1-2 times by using deionized water, and drying to obtain calcium sulfate whiskers, wherein the drying procedure comprises the steps of drying at 100-110 ℃ for 1-2h at first, and then drying at 170-180 ℃ for 1-2h.
2. The method for preparing calcium sulfate whiskers by using ammonia-soda caustic sludge water as claimed in claim 1, wherein the method comprises the following steps:
the eleventh filtrate is sodium chloride aqueous solution which can be directly discharged or used in ammonia-soda production process, salt dissolving and brine refining sections.
3. An apparatus for preparing calcium sulfate whisker by using ammonia alkali slag water when the method of any one of claims 1 to 2 is realized, which is characterized in that:
the equipment comprises a material mixer, a filter and an oven;
the material mixer is used for mixing materials;
the filter is used for separating materials to obtain filtrate and filter cakes;
the oven is used for drying the materials.
CN202211029371.3A 2022-08-26 2022-08-26 Method and equipment for preparing calcium sulfate whisker by using ammonia-soda alkaline residue water Pending CN115594210A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202211029371.3A CN115594210A (en) 2022-08-26 2022-08-26 Method and equipment for preparing calcium sulfate whisker by using ammonia-soda alkaline residue water

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202211029371.3A CN115594210A (en) 2022-08-26 2022-08-26 Method and equipment for preparing calcium sulfate whisker by using ammonia-soda alkaline residue water

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CN115594210A true CN115594210A (en) 2023-01-13

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Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102453951A (en) * 2010-10-21 2012-05-16 华东理工大学 Method for preparing high quality calcium sulfate crystal whisker by using waste liquid from alkali preparation and waste sulfuric acid

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102453951A (en) * 2010-10-21 2012-05-16 华东理工大学 Method for preparing high quality calcium sulfate crystal whisker by using waste liquid from alkali preparation and waste sulfuric acid

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