CN111101191A - Method for preparing gypsum whisker by seed crystal method - Google Patents

Method for preparing gypsum whisker by seed crystal method Download PDF

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CN111101191A
CN111101191A CN202010123170.4A CN202010123170A CN111101191A CN 111101191 A CN111101191 A CN 111101191A CN 202010123170 A CN202010123170 A CN 202010123170A CN 111101191 A CN111101191 A CN 111101191A
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acidolysis
solution
seed crystal
gypsum
whisker
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张华丽
潘益
杨成
潘志权
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Wuhan Institute of Technology
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    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
    • C30B7/14—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions the crystallising materials being formed by chemical reactions in the solution
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10—Inorganic compounds or compositions
    • C30B29/46—Sulfur-, selenium- or tellurium-containing compounds
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
    • C30B29/62—Whiskers or needles

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  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
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  • Inorganic Chemistry (AREA)
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  • General Chemical & Material Sciences (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

The invention provides a method for preparing gypsum crystal whisker by a crystal seed method, which adopts a normal pressure acidification method to mix and react tailing acidolysis solution and concentrated sulfuric acid under the normal pressure condition, firstly prepares gypsum crystal whisker crystal seed, and then reacts the gypsum crystal whisker crystal seed and the acidolysis solution under certain conditions to obtain the gypsum crystal whisker. The gypsum whisker obtained by the method is uniform in distribution, has a length-diameter ratio of about 60, is simple in process and convenient to operate, provides theoretical support for comprehensive utilization and further industrialization of the phosphorus tailings, greatly improves the additional value of phosphorus tailings products, solves environmental pollution caused by the phosphorus tailings, improves ecological environment, and has huge economic, social and environmental benefits.

Description

Method for preparing gypsum whisker by seed crystal method
Technical Field
The invention relates to the technical field of waste resource utilization, in particular to a method for preparing gypsum whiskers by a seed crystal method.
Background
The high-magnesium phosphate tailings are industrial wastes, mainly come from tailings slag left after ore dressing to extract concentrate, and belong to mining solid wastes among the industrial solid wastes according to subdivision. At present, the treatment and utilization status of high-magnesium phosphate tailings is severe, phosphate tailings which cannot be effectively treated for a long time are accumulated like a mountain, serious pollution is caused to the environment, and the waste of resources is caused, so the treatment of the phosphate tailings is an important subject facing the research of the phosphorus chemical industry at present.
Calcium Sulfate Whisker (CSW), namely gypsum Whisker, is a resource product with broad prospect. The calcium sulfate whisker is a fibrous or acicular monocrystal with high length-diameter ratio, is gray and white fluffy powder, has the advantages of high strength, good thermal stability, chemical corrosion resistance, compatibility and the like, and is cheaper than other types of whiskers. Therefore, the calcium sulfate whisker is widely applied to the fields of rubber, plastics, asphalt, paper making and the like. The method for preparing the calcium sulfate whisker by using the high-magnesium phosphate tailings as the raw material has positive significance in the aspects of cost saving, waste recycling, environmental protection and the like.
The method for preparing the gypsum whisker in the prior art mainly comprises three methods, namely a normal pressure acidification method, a hydraulic pressure thermal method and an organic medium method. The normal pressure acidification method is to convert high concentration dihydrate gypsum suspension into needle calcium sulfate whisker under the conditions of room temperature and acidity, while the hydraulic pressure heating method is to add dihydrate gypsum suspension with content less than 2% into a hydraulic pressure heating container, convert dihydrate gypsum into needle hemihydrate gypsum under saturated steam pressure, and then obtain calcium sulfate hemihydrate whisker through crystal form stabilization treatment. The hydraulic pressure thermal method takes a high-pressure kettle as reaction equipment, and converts the high-pressure kettle into crystals at higher temperature and pressure, so that the energy consumption in the process is higher; the organic mediator method is usually a method comprising Ca2+With an organic solution containing SO4 2-The organic solution is mixed according to a certain volume ratio to react to synthesize the calcium sulfate whisker, but the cost is higher, the operation difficulty is higher, and the industrial mass production is not facilitated. The normal pressure acidification method does not need an autoclave, has simple preparation process and larger concentration of raw materials, theoretically greatly reduces the preparation cost and is easy for industrial production. The method is simple and effective, not only saves the hydrothermal reaction process, but also has low production cost, simple operation and large yield, and is beneficial to industrialized mass production.
In the prior art, a method for preparing calcium sulfate whiskers by decomposing high-magnesium phosphate tailings by hydrochloric acid is available, for example, a Chinese patent with publication number of CN 107419335A discloses a method for preparing calcium sulfate whiskers by circularly decomposing phosphogypsum and phosphate tailings by a hydrochloric acid method, the method can simultaneously treat phosphate tailings and phosphogypsum and prepare calcium sulfate dihydrate whiskers, but the prepared whiskers have wider and uneven length-diameter ratio distribution; chinese patent publication No. CN 110467213 a discloses a method for preparing calcium sulfate whiskers from high-magnesium phosphate tailings, which focuses on promoting the growth of whiskers by adjusting the concentrations of phosphate ions, magnesium ions, hydrogen ions and iron ions in the process of preparing calcium sulfate whiskers, and finally the aspect ratio of whiskers can reach 50-110, but the cost input can be increased in the process of adjusting the concentration, which is not beneficial to mass production; chinese patent publication No. CN 109250736 a discloses a method for preparing active magnesium oxide by reverse flotation of phosphate tailings, which produces active magnesium oxide by reverse flotation of magnesium-removed phosphate tailings by hydrochloric acid method, and the byproduct is calcium sulfate whisker, the process is simple, the energy consumption is low, but the quality of the finally prepared calcium sulfate crystal is general; chinese patent publication No. CN107098372A discloses a method for preparing calcium sulfate whiskers and magnesium hydroxide by decomposing phosphate tailings with hydrochloric acid, which can simultaneously prepare higher-quality calcium sulfate whiskers, magnesium hydroxide and magnesium ammonium phosphate crystals, but has a longer process and more complicated operation; the Chinese patent with publication number CN 107043956A discloses a method for preparing calcium sulfate whiskers and magnesium hydroxide from hydrochloric acid and phosphate tailings, which can simultaneously prepare magnesium hydroxide and calcium sulfate whiskers, and has the advantages of simple whole production process, full-closed circulation, high energy consumption and difficult control in the production process; the Chinese patent with publication number CN 106495191A discloses a method for preparing magnesium hydroxide and calcium sulfate by decomposing phosphate tailings with hydrochloric acid, the production process is simple, clean production can be achieved, and the prepared calcium sulfate whiskers are dispersed.
Disclosure of Invention
In view of the above, the invention aims to provide a method for preparing gypsum whiskers by a seed crystal method, so as to solve the problems of low resource utilization rate of the existing phosphate tailings and low product added value.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
a method for preparing gypsum whiskers by a seed crystal method comprises the following steps:
1) mixing the high-magnesium phosphate tailings with hydrochloric acid, carrying out acidolysis reaction, after the acidolysis reaction is finished, carrying out suction filtration and washing to obtain acidolysis solution A and silicon slag;
2) adding concentrated sulfuric acid into part of the acidolysis solution A at a certain temperature, and reacting for a period of time to obtain a seed crystal solution B;
3) and mixing the residual acidolysis solution A and the seed crystal solution B at a certain temperature, reacting for a period of time, aging, filtering, washing, and drying to obtain the gypsum whisker.
Optionally, the concentration of the hydrochloric acid in the step 1) is 8.80-12.07mol/L, and the mass ratio of the hydrochloric acid to the high-magnesium phosphorus tailings is (2.25-3) to 1.
Optionally, the reaction temperature of the acidolysis reaction in the step 1) is 20-60 ℃, and the reaction time is 20-60 min.
Optionally, the suction filtration temperature of the suction filtration in the step 1) is 50-60 ℃.
Optionally, the step 2) of adding concentrated sulfuric acid to a part of the acidolysis solution a at a certain temperature, and reacting for a certain time to obtain a seed crystal solution B includes:
adding concentrated sulfuric acid into part of the acidolysis solution A at 70-95 ℃, and reacting for 1-6h to obtain a seed crystal solution B.
Optionally, the adding amount of the concentrated sulfuric acid in the step 2) is 1-1.5 times of the amount of calcium substances in the acidolysis solution A, wherein the acidolysis solution A comprises part of the acidolysis solution A in the step 2) and the rest of the acidolysis solution A in the step 3).
Optionally, in the step 3), mixing the remaining acidolysis solution a and the seed crystal solution B at a certain temperature, reacting for a certain period of time, and then aging, filtering, washing, and drying to obtain the gypsum whisker, including:
and mixing the residual acidolysis solution A and the seed crystal solution B at the temperature of 70-95 ℃, reacting for 1-6h, aging for 8-16h, and then carrying out suction filtration, washing and drying to obtain the gypsum whisker.
Compared with the prior art, the method for preparing the gypsum whisker by the crystal seed method has the following advantages:
1. the invention adopts the normal pressure acidification method to mix and react the tailing acidolysis solution and concentrated sulfuric acid under the normal pressure condition, firstly prepares the crystal seed of the gypsum whisker, and then promotes the crystal seed to grow under certain conditions to improve the length-diameter ratio of the gypsum whisker, the obtained gypsum whisker is uniformly distributed, the length-diameter ratio is about 60, the process is simple and convenient to operate, theoretical support is provided for the comprehensive utilization and further industrialization of the phosphate tailings, the added value of the phosphate tailings product is greatly improved, the environmental pollution caused by the phosphate tailings is solved, the ecological environment is improved, and the invention has huge economic, social and environmental benefits.
2. The tailings and the industrial hydrochloric acid used in the invention both belong to industrial waste, so that the preparation cost of the gypsum whisker is greatly reduced, the whole preparation process has no pollution to the environment, and a theoretical basis is provided for the reduction of burden and the increase of income of enterprises.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate an embodiment of the invention and, together with the description, serve to explain the invention and not to limit the invention. In the drawings:
FIG. 1 is a process flow diagram of the present invention for preparing gypsum whisker by a seed crystal method;
figure 2 is a microscope image of gypsum whiskers prepared in example 5 of the present invention.
Detailed Description
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict.
The present invention will be described in detail below with reference to the drawings and examples.
Example 1
As shown in fig. 1, the method for preparing gypsum whiskers by using the seed crystal method in this embodiment specifically includes the following steps:
1) 497mL of industrial hydrochloric acid with the mass fraction of 30% (10.30mol/L) is measured and placed in a clean three-neck bottle, 261.8g of high-magnesium phosphorus tailing powder is measured, the high-magnesium phosphorus tailing is gradually added into the three-neck bottle, after the high-magnesium phosphorus tailing is added, condensed water is opened, stirring is started, the mixture is refluxed for 30min at 60 ℃, acidolysis reaction is carried out, after the acidolysis reaction is finished, heat preservation and filtration are carried out at 60 ℃, silicon slag obtained by heat preservation and filtration is washed by 180mL of distilled water for three times, primary water washing liquid and acidolysis filtrate obtained by heat preservation and filtration are mixed to obtain acidolysis liquid A and silicon slag, and the concentration of calcium ions in the acidolysis liquid A is measured;
2) heating 150mL of the acidolysis solution A obtained in the step 2) to 80 ℃ in an oil bath, measuring 120mL of 98% concentrated sulfuric acid, dropwise adding the concentrated sulfuric acid into the acidolysis solution A, wherein the ratio of the addition amount of the concentrated sulfuric acid to the amount of calcium substances in the acidolysis solution A is 1: 1, starting stirring, gradually generating calcium sulfate crystal seeds in the solution, continuing to react for 1.5 hours after the addition of the concentrated sulfuric acid is finished, and obtaining a crystal seed solution B after the reaction is finished;
3) and (3) dropwise adding the residual acidolysis solution A into the seed crystal solution B obtained in the step 2) at 80 ℃, continuing to react for 2h after the addition is finished, aging for 12h after the reaction is finished, performing suction filtration, washing with 300ml of condensed water for three times, and drying to obtain the gypsum whisker, wherein the length-diameter ratio of the gypsum whisker is 58.
Example 2
As shown in fig. 1, the method for preparing gypsum whiskers by using the seed crystal method in this embodiment specifically includes the following steps:
1) weighing 502mL of industrial hydrochloric acid with the mass fraction of 31% (10.35mol/L), placing the industrial hydrochloric acid in a clean three-neck flask, weighing 261.8g of high-magnesium phosphorus tailing powder, gradually adding the high-magnesium phosphorus tailing into the three-neck flask, after the high-magnesium phosphorus tailing is added, opening condensed water, starting stirring, refluxing for 35min at 55 ℃, carrying out acidolysis reaction, after the acidolysis reaction is finished, carrying out heat preservation and suction filtration at 60 ℃, washing silicon slag obtained by heat preservation and filtration for three times by using 190mL of distilled water, mixing primary water washing liquid and acidolysis filtrate obtained by heat preservation and filtration to obtain acidolysis liquid A and silicon slag, and determining the concentration of calcium ions in the acidolysis liquid A;
2) heating 190mL of the acidolysis solution A obtained in the step 2) to 95 ℃ in an oil bath, measuring 160mL of 98% concentrated sulfuric acid, dropwise adding the concentrated sulfuric acid into the acidolysis solution A, wherein the ratio of the addition amount of the concentrated sulfuric acid to the amount of calcium substances in the acidolysis solution A is 1.23: 1, starting stirring, gradually generating calcium sulfate crystal seeds in the solution, continuing to react for 2 hours after the addition of the concentrated sulfuric acid is finished, and obtaining a crystal seed solution B after the reaction is finished;
3) and (3) dropwise adding the residual acidolysis solution A into the seed crystal solution B obtained in the step 2) at 95 ℃, continuing to react for 4 hours after the addition is finished, aging for 16 hours after the reaction is finished, performing suction filtration, washing with 300ml of condensed water for three times, and drying to obtain the gypsum whisker, wherein the length-diameter ratio of the gypsum whisker reaches 62.
Example 3
As shown in fig. 1, the method for preparing gypsum whiskers by using the seed crystal method in this embodiment specifically includes the following steps:
1) weighing 510mL of industrial hydrochloric acid with the mass fraction of 29% (10.15mol/L), placing the industrial hydrochloric acid in a clean three-neck flask, weighing 261.8g of high-magnesium phosphorus tailing powder, gradually adding the high-magnesium phosphorus tailing into the three-neck flask, after the high-magnesium phosphorus tailing is added, opening condensed water, starting stirring, refluxing for 20min at 55 ℃, carrying out acidolysis reaction, after the acidolysis reaction is finished, carrying out heat preservation and suction filtration at 60 ℃, washing silicon slag obtained by heat preservation and filtration three times with 200mL of distilled water, mixing primary water washing liquid and acidolysis filtrate obtained by heat preservation and filtration to obtain acidolysis liquid A and silicon slag, and determining the concentration of calcium ions in the acidolysis liquid A;
2) heating 210mL of the acidolysis solution A obtained in the step 2) to 75 ℃ in an oil bath, measuring 130mL of 98% concentrated sulfuric acid, dropwise adding the concentrated sulfuric acid into the acidolysis solution A, wherein the ratio of the addition amount of the concentrated sulfuric acid to the amount of calcium substances in the acidolysis solution A is 1.05: 1, starting stirring, gradually generating calcium sulfate crystal seeds in the solution, continuing to react for 3 hours after the addition of the concentrated sulfuric acid is finished, and obtaining a crystal seed solution B after the reaction is finished;
3) and (3) dropwise adding the residual acidolysis solution A into the seed crystal solution B obtained in the step 2) at 75 ℃, continuing to react for 3 hours after the addition is finished, aging for 15.5 hours after the reaction is finished, carrying out suction filtration, washing with 300ml of condensed water for three times, and drying to obtain the gypsum whisker, wherein the length-diameter ratio of the gypsum whisker reaches 65.
Example 4
As shown in fig. 1, the method for preparing gypsum whiskers by using the seed crystal method in this embodiment specifically includes the following steps:
1) weighing 510mL of industrial hydrochloric acid with the mass fraction of 27% (10.01mol/L), placing the industrial hydrochloric acid in a clean three-neck flask, weighing 261.8g of high-magnesium phosphorus tailing powder, gradually adding the high-magnesium phosphorus tailing into the three-neck flask, after the high-magnesium phosphorus tailing is added, opening condensed water, starting stirring, refluxing for 25min at 60 ℃, carrying out acidolysis reaction, after the acidolysis reaction is finished, carrying out heat preservation and suction filtration at 60 ℃, washing silicon slag obtained by heat preservation and filtration for three times by using 220mL of distilled water, mixing primary water washing liquid and acidolysis filtrate obtained by heat preservation and filtration to obtain acidolysis liquid A and silicon slag, and determining the concentration of calcium ions in the acidolysis liquid A;
2) heating 150mL of the acidolysis solution A obtained in the step 2) to 90 ℃ in an oil bath, measuring 120mL of 98% concentrated sulfuric acid, dropwise adding the concentrated sulfuric acid into the acidolysis solution A, wherein the ratio of the addition amount of the concentrated sulfuric acid to the amount of calcium substances in the acidolysis solution A is 1.5: 1, starting stirring, gradually generating calcium sulfate crystal seeds in the solution, continuing to react for 6 hours after the addition of the concentrated sulfuric acid is finished, and obtaining a crystal seed solution B after the reaction is finished;
3) and (3) dropwise adding the residual acidolysis solution A into the seed crystal solution B obtained in the step 2) at 90 ℃, continuing to react for 5 hours after the addition is finished, aging for 14 hours after the reaction is finished, performing suction filtration, washing with 300ml of condensed water for three times, and drying to obtain the gypsum whisker, wherein the length-diameter ratio of the gypsum whisker reaches 60.
Example 5
As shown in fig. 1, the method for preparing gypsum whiskers by using the seed crystal method in this embodiment specifically includes the following steps:
1) weighing 470mL of industrial hydrochloric acid with the mass fraction of 36% (10.95mol/L), placing the industrial hydrochloric acid in a clean three-neck flask, weighing 261.8g of high-magnesium phosphorus tailing powder, gradually adding the high-magnesium phosphorus tailing into the three-neck flask, after the high-magnesium phosphorus tailing is added, opening condensed water, starting stirring, refluxing for 30min at 45 ℃, carrying out acidolysis reaction, after the acidolysis reaction is finished, carrying out heat preservation and suction filtration at 60 ℃, washing silicon slag obtained by heat preservation and filtration for three times by using 250mL of distilled water, mixing primary water washing liquid and acidolysis filtrate obtained by heat preservation and filtration to obtain acidolysis liquid A and silicon slag, and determining the concentration of calcium ions in the acidolysis liquid A;
2) heating 190mL of the acidolysis solution A obtained in the step 2) to 86 ℃ in an oil bath, measuring 118mL of 98% concentrated sulfuric acid, dropwise adding the concentrated sulfuric acid into the acidolysis solution A, wherein the ratio of the addition amount of the concentrated sulfuric acid to the amount of calcium substances in the acidolysis solution A is 1.35: 1, starting stirring, gradually generating calcium sulfate crystal seeds in the solution, continuing to react for 4 hours after the addition of the concentrated sulfuric acid is finished, and obtaining a crystal seed solution B after the reaction is finished;
3) and (3) dropwise adding the residual acidolysis solution A into the seed crystal solution B obtained in the step 2) at 86 ℃, continuing to react for 6 hours after the addition is finished, aging for 16 hours after the reaction is finished, performing suction filtration, washing with 300ml of condensed water for three times, and drying to obtain the gypsum whisker, wherein the length-diameter ratio of the gypsum whisker reaches 63.
The gypsum whiskers of example 5 of the present invention were subjected to SEM test, and the test results are shown in fig. 1.
As can be seen from FIG. 1, the gypsum whiskers of example 5 of the present invention were uniformly distributed, and the aspect ratio thereof reached 63.
The present invention is not limited to the above preferred embodiments, and any modifications, equivalent substitutions, improvements, etc. within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (7)

1. A method for preparing gypsum whiskers by a seed crystal method is characterized by comprising the following steps:
1) mixing the high-magnesium phosphate tailings with hydrochloric acid, carrying out acidolysis reaction, after the acidolysis reaction is finished, carrying out suction filtration and washing to obtain acidolysis solution A and silicon slag;
2) adding concentrated sulfuric acid into part of the acidolysis solution A at a certain temperature, and reacting for a period of time to obtain a seed crystal solution B;
3) and mixing the residual acidolysis solution A and the seed crystal solution B at a certain temperature, reacting for a period of time, aging, filtering, washing, and drying to obtain the gypsum whisker.
2. The seed crystal method for preparing gypsum whiskers according to claim 1, wherein the concentration of the hydrochloric acid in the step 1) is 8.80-12.07mol/L, and the mass ratio of the hydrochloric acid to the high-magnesium-phosphorus tailings is (2.25-3) to 1.
3. The method for preparing gypsum whiskers by using the seed crystal method as claimed in claim 1, wherein the reaction temperature of the acidolysis reaction in the step 1) is 20-60 ℃ and the reaction time is 20-60 min.
4. The method for preparing gypsum whiskers according to claim 1, wherein the suction filtration temperature of the suction filtration in the step 1) is 50-60 ℃.
5. The method for preparing gypsum whiskers by using the seed crystal method as claimed in claim 1, wherein the step 2) of adding concentrated sulfuric acid to a part of the acidolysis solution A at a certain temperature and reacting for a certain time to obtain a seed crystal solution B comprises the following steps:
adding concentrated sulfuric acid into part of the acidolysis solution A at 70-95 ℃, and reacting for 1-6h to obtain a seed crystal solution B.
6. The method for preparing gypsum whiskers by using the seed crystal method as claimed in claim 1 or 4, wherein the addition amount of the concentrated sulfuric acid in the step 2) is 1-1.5 times of the amount of calcium substances in the acidolysis solution A, wherein the acidolysis solution A comprises part of the acidolysis solution A in the step 2) and the rest of the acidolysis solution A in the step 3).
7. The method for preparing gypsum whiskers by using the seed crystal method as claimed in claim 1, wherein the step 3) comprises mixing the remaining acidolysis solution A and the seed crystal solution B at a certain temperature, reacting for a certain period of time, aging, filtering, washing, and drying to obtain gypsum whiskers, and comprises the following steps:
and mixing the residual acidolysis solution A and the seed crystal solution B at the temperature of 70-95 ℃, reacting for 1-6h, aging for 8-16h, and then carrying out suction filtration, washing and drying to obtain the gypsum whisker.
CN202010123170.4A 2020-02-27 2020-02-27 Method for preparing gypsum whisker by seed crystal method Withdrawn CN111101191A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114000187A (en) * 2021-09-16 2022-02-01 昆明理工大学 Method for preparing high-length semi-hydrated phosphogypsum whisker through two-stage reaction
CN115074815A (en) * 2022-06-28 2022-09-20 中盐金坛盐化有限责任公司 Method for preparing calcium sulfate dihydrate whisker at normal temperature by taking brine salt preparation by-product as raw material

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS54151592A (en) * 1978-05-22 1979-11-28 Idemitsu Kosan Co Ltd Gypsum wisker and its manufacture
CN103922372A (en) * 2014-04-11 2014-07-16 武汉工程大学 Method for recovering phosphorus in phosphate tailings with high magnesium content and preparing magnesium sulfate by adopting indirect sulfuric acid method
CN107419335A (en) * 2017-07-13 2017-12-01 湖北三宁化工股份有限公司 The method that hydrochloric acid method Cycle-decomposition ardealite and phosphorus mine tailing prepare calcium sulfate crystal whiskers
CN110451473A (en) * 2019-09-11 2019-11-15 武汉工程大学 A kind of method of comprehensive utilization recycling acidleach High-Mg phosphate tailings
CN110467213A (en) * 2019-09-11 2019-11-19 武汉工程大学 A method of calcium sulfate crystal whiskers are prepared using High-Mg phosphate tailings

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS54151592A (en) * 1978-05-22 1979-11-28 Idemitsu Kosan Co Ltd Gypsum wisker and its manufacture
CN103922372A (en) * 2014-04-11 2014-07-16 武汉工程大学 Method for recovering phosphorus in phosphate tailings with high magnesium content and preparing magnesium sulfate by adopting indirect sulfuric acid method
CN107419335A (en) * 2017-07-13 2017-12-01 湖北三宁化工股份有限公司 The method that hydrochloric acid method Cycle-decomposition ardealite and phosphorus mine tailing prepare calcium sulfate crystal whiskers
CN110451473A (en) * 2019-09-11 2019-11-15 武汉工程大学 A kind of method of comprehensive utilization recycling acidleach High-Mg phosphate tailings
CN110467213A (en) * 2019-09-11 2019-11-19 武汉工程大学 A method of calcium sulfate crystal whiskers are prepared using High-Mg phosphate tailings

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
杨成: "磷尾矿的综合利用试验研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114000187A (en) * 2021-09-16 2022-02-01 昆明理工大学 Method for preparing high-length semi-hydrated phosphogypsum whisker through two-stage reaction
CN115074815A (en) * 2022-06-28 2022-09-20 中盐金坛盐化有限责任公司 Method for preparing calcium sulfate dihydrate whisker at normal temperature by taking brine salt preparation by-product as raw material
CN115074815B (en) * 2022-06-28 2023-05-05 中盐金坛盐化有限责任公司 Method for preparing calcium sulfate dihydrate whisker at normal temperature by taking brine salt-making byproducts as raw materials

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Application publication date: 20200505