CN113882021A - Method for preparing calcium sulfate whisker by phosphogypsum high-temperature high-pressure method - Google Patents
Method for preparing calcium sulfate whisker by phosphogypsum high-temperature high-pressure method Download PDFInfo
- Publication number
- CN113882021A CN113882021A CN202111186913.3A CN202111186913A CN113882021A CN 113882021 A CN113882021 A CN 113882021A CN 202111186913 A CN202111186913 A CN 202111186913A CN 113882021 A CN113882021 A CN 113882021A
- Authority
- CN
- China
- Prior art keywords
- phosphogypsum
- calcium sulfate
- pressure
- temperature
- composite system
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 title claims abstract description 96
- PASHVRUKOFIRIK-UHFFFAOYSA-L calcium sulfate dihydrate Chemical compound O.O.[Ca+2].[O-]S([O-])(=O)=O PASHVRUKOFIRIK-UHFFFAOYSA-L 0.000 title claims abstract description 63
- 238000000034 method Methods 0.000 title claims abstract description 52
- 239000002131 composite material Substances 0.000 claims description 38
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 34
- 238000003756 stirring Methods 0.000 claims description 26
- -1 polytetrafluoroethylene Polymers 0.000 claims description 22
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 22
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 21
- 238000001035 drying Methods 0.000 claims description 20
- 239000004033 plastic Substances 0.000 claims description 19
- 229920003023 plastic Polymers 0.000 claims description 19
- 238000006243 chemical reaction Methods 0.000 claims description 17
- 239000002994 raw material Substances 0.000 claims description 15
- 238000005303 weighing Methods 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 238000011049 filling Methods 0.000 claims description 8
- 238000005070 sampling Methods 0.000 claims description 8
- 238000007789 sealing Methods 0.000 claims description 8
- 238000007873 sieving Methods 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000011161 development Methods 0.000 abstract description 6
- 230000008901 benefit Effects 0.000 abstract description 5
- 230000008569 process Effects 0.000 abstract description 4
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 239000002686 phosphate fertilizer Substances 0.000 abstract 1
- 238000009270 solid waste treatment Methods 0.000 abstract 1
- 229940095672 calcium sulfate Drugs 0.000 description 35
- 239000000203 mixture Substances 0.000 description 18
- 239000008367 deionised water Substances 0.000 description 7
- 229910021641 deionized water Inorganic materials 0.000 description 7
- 239000000843 powder Substances 0.000 description 7
- 238000002474 experimental method Methods 0.000 description 6
- 239000004570 mortar (masonry) Substances 0.000 description 6
- 230000018109 developmental process Effects 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 230000000035 biogenic effect Effects 0.000 description 2
- 239000004568 cement Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000010440 gypsum Substances 0.000 description 2
- 229910052602 gypsum Inorganic materials 0.000 description 2
- 239000002440 industrial waste Substances 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000005060 rubber Substances 0.000 description 2
- 239000005909 Kieselgur Substances 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 229940095564 anhydrous calcium sulfate Drugs 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052918 calcium silicate Inorganic materials 0.000 description 1
- 239000000378 calcium silicate Substances 0.000 description 1
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000002783 friction material Substances 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Images
Classifications
-
- 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
-
- 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
- C30B7/10—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by application of pressure, e.g. hydrothermal processes
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention provides a method for preparing calcium sulfate whiskers by a phosphogypsum high-temperature high-pressure method. The calcium sulfate whisker prepared by the method is uniformly dispersed and regular in shape, has the average length of 20-30 mu m and the average length-diameter ratio of 3-10, provides theoretical support for comprehensive utilization and further industrialization of phosphogypsum, effectively solves the problem of environmental pollution caused by the phosphogypsum, improves the ecological environment, and has huge economic, social and environmental benefits; the invention combines the high-temperature and high-pressure technology with solid waste treatment, so as to open up a new road for the reasonable utilization of the phosphogypsum and other tailings and explore a new process, and has important significance for further improving the sustainable development of the phosphate fertilizer industry and the high utilization and environment-friendly development of the phosphogypsum industry.
Description
Technical Field
The invention relates to the technical field of waste resource utilization, in particular to a method for preparing calcium sulfate whiskers by a phosphogypsum high-temperature high-pressure method.
Background
Phosphogypsum is an industrial solid waste generated by preparing phosphoric acid by decomposing phosphate ore with sulfuric acid. According to incomplete statistics, the global accumulated phosphogypsum inventory is as high as 56 hundred million t and increases at a rate of 2 hundred million to 3 hundred million t per year. The annual output of phosphogypsum in China is about 7500 million t, and the accumulated stockpiling quantity is over 6 hundred million t. The large amount of stockpiling of the phosphogypsum not only occupies land resources, but also causes pollution to atmosphere, soil and water resources, and has generated serious environmental hazard. At present, the phosphogypsum is mainly applied to the aspects of preparing agricultural fertilizers, building materials, calcium sulfate whiskers and the like. However, only a small amount of phosphogypsum, about 15%, is recovered, as the technical and technological developments involved in the utilization of phosphogypsum are still incomplete. Therefore, the treatment of phosphogypsum is mainly stockpiling at present. Therefore, in order to ensure the healthy development of phosphorus chemical enterprises, an economical and feasible new way for recycling the phosphogypsum is explored, and the technical problem to be solved by the phosphorus chemical enterprises is urgently solved.
China has abundant diatomite resources and the reserves are the second world. Diatomite belongs to biogenic sedimentary rock, and has a well-developed microporous structure due to biogenic reasons, and has the characteristics of light weight, excellent heat insulation performance, strong plasticity and the like, so the diatomite is widely used in light heat insulation wall materials. Researches show that the diatomite is also an active admixture for preparing high-performance cement, and the action mechanism of the diatomite is as follows: active SiO in diatomaceous earth2Can be mixed with cement hydration products Ca (OH)2And a large amount of flocculent calcium silicate hydrate gel (C-S-H) is generated by reaction, so that a cement-diatomite mixed material system is more uniform and compact, and the mechanical property of slurry is improved.
The calcium sulfate whisker is fibrous single crystal of anhydrous calcium sulfate, is also called gypsum whisker, and is needle-shaped white fiber. The calcium sulfate whisker has the advantages of high strength, chemical corrosion resistance, high temperature resistance, good toughness, strong affinity with polymers such as rubber and the like, and can be widely applied to the fields of novel materials such as rubber, plastics, friction materials, coatings, paints, papermaking, catalysis, conductive powder and the like. However, the current domestic and foreign production methods not only have high production cost and complex procedures, but also have serious pollution and worry about development prospects. Therefore, the cheap and simple preparation method for preparing the gypsum whisker by using the industrial waste residue phosphogypsum can protect the environment and can greatly develop the social economy.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a method for preparing calcium sulfate whiskers by a phosphogypsum high-temperature high-pressure method.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a method for preparing calcium sulfate whiskers by a phosphogypsum high-temperature high-pressure method comprises the following steps:
s1: pretreating raw materials of phosphogypsum and diatomite;
s2: weighing a certain amount of raw materials, stirring for a period of time T1 and uniformly mixing to obtain a composite system A;
s3: adding water into the composite system A, and stirring for a period of time T2 to obtain a plastic composite system B;
s4: filling the plastic composite system B into a small polytetrafluoroethylene cap, and then sleeving and sealing the small polytetrafluoroethylene cap by using a large polytetrafluoroethylene cap to obtain a sample C;
s5: and (3) placing the sample C into a reaction kettle for high-temperature high-pressure reaction for a period of T3, relieving pressure, sampling and drying to obtain the calcium sulfate whisker.
Optionally, in step S1, the raw material pretreatment method includes: drying phosphogypsum in an oven at the temperature of (45 +/-3) DEG C to constant weight, and sieving the phosphogypsum by a sieve of 80 meshes; crushing and grinding the blocky diatomite, and sieving the blocky diatomite with a 200-mesh sieve.
Optionally, in step S2, the addition amount of the phosphogypsum is 85% to 95% of the mass of the composite system a, and the addition amount of the diatomite is 5% to 15% of the mass of the composite system a.
Optionally, in step S2, the stirring time T1 is 30-60 min.
Optionally, in step S3, the solid-to-liquid ratio of the plastic composite system B is 10: 1.
Optionally, in step S3, the stirring time T2 is 5-10 min.
Optionally, in step S4, the size of the small ptfe cap is: the inner diameter is 10mm, the outer diameter is 12mm, and the height is 12 mm; the size of the large polytetrafluoroethylene cap is as follows: 12mm inner diameter, 14mm outer diameter and 12mm height.
Optionally, in step S5, the reaction conditions are: the reaction temperature is 200-300 ℃, the reaction pressure is 200-300 MPa, and the reaction time T3 is 24 h.
Optionally, in step S5, the drying temperature during drying is 60 to 80 ℃.
Compared with the prior art, the invention has the beneficial effects that: (1) the method comprises the steps of pretreating phosphogypsum and kieselguhr, adding a certain amount of deionized water, and finally preparing the calcium sulfate whiskers by a high-temperature high-pressure method, wherein the prepared calcium sulfate whiskers are uniformly distributed, have the average length of 20-30 mu m and the average length-diameter ratio of 3-10, so that a new thought is provided for the comprehensive utilization of the phosphogypsum and the further industrial development of the phosphogypsum whiskers, the problem of environmental pollution caused by the phosphogypsum is effectively solved, the ecological environment is greatly improved, and great economic and environmental benefits are achieved for the society; (2) the phosphogypsum crystal whisker is prepared by taking phosphogypsum and diatomite as experimental raw materials, and no chemical crystallization promoter is added in the whole experimental process, so that the whole experimental process is green, environment-friendly, clean and pollution-free; (3) the diatomite used as the experimental raw material is abundant in China, and the phosphogypsum belongs to industrial waste, so that the preparation cost of the calcium sulfate whisker is greatly reduced, and enterprises can obtain low-cost raw materials to produce the calcium sulfate whisker with high benefit.
Drawings
The above and/or additional aspects and advantages of the present invention will become apparent and readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings of which:
FIG. 1 is a process flow diagram of the high temperature and high pressure method for preparing calcium sulfate whisker by phosphogypsum;
fig. 2 is an SEM picture of calcium sulfate whiskers prepared in example 2 of the present invention.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the accompanying drawings are illustrative only for the purpose of explaining the present invention, and are not to be construed as limiting the present invention.
Example one
As shown in fig. 1, the method for preparing calcium sulfate whiskers by using the phosphogypsum high-temperature high-pressure method in this embodiment specifically includes the following steps:
s1: pretreating raw materials of phosphogypsum and diatomite;
s2: weighing 4.5g of pretreated powdery phosphogypsum and 0.5g of diatomite powder, placing the mixture in an agate mortar, and stirring for 30min to fully and uniformly mix the mixture to prepare a composite system A with the mass of 5 g;
s3: weighing 0.5m L deionized water, pouring into the composite system A in the step S2, stirring for 5min, and obtaining a plastic composite system B after the stirring is finished;
s4: filling the plastic composite system B into a small polytetrafluoroethylene cap (with the inner diameter of 10mm, the outer diameter of 12mm and the height of 12mm), and then sleeving and sealing the small polytetrafluoroethylene cap (with the inner diameter of 12mm, the outer diameter of 14mm and the height of 12mm) to obtain a sample C;
s5: and putting the sample C into a high-temperature high-pressure reaction kettle, keeping the temperature and the pressure constant for 24h under the conditions of 300 ℃ and 300MPa, after the experiment is finished, releasing the pressure and sampling, and drying the pressed sample in a drying oven at 60 ℃ to obtain the calcium sulfate whisker, wherein the average length of the obtained calcium sulfate whisker is 21.51 mu m, and the average length-diameter ratio of the calcium sulfate whisker is 6.83.
Example two
As shown in fig. 1, the method for preparing calcium sulfate whiskers by using the phosphogypsum high-temperature high-pressure method in this embodiment specifically includes the following steps:
s1: pretreating raw materials of phosphogypsum and diatomite;
s2: weighing 4.5g of pretreated powdery phosphogypsum and 0.5g of diatomite powder, placing the mixture in an agate mortar, and stirring for 30min to fully and uniformly mix the mixture to prepare a composite system A with the mass of 5 g;
s3: weighing 0.5m L deionized water, pouring into the composite system A in the step S2, stirring for 5min, and obtaining a plastic composite system B after the stirring is finished;
s4: filling the plastic composite system B into a small polytetrafluoroethylene cap (with the inner diameter of 10mm, the outer diameter of 12mm and the height of 12mm), and then sleeving and sealing the small polytetrafluoroethylene cap (with the inner diameter of 12mm, the outer diameter of 14mm and the height of 12mm) to obtain a sample C;
s5: and putting the sample C into a high-temperature high-pressure reaction kettle, keeping the temperature and the pressure constant for 24h under the conditions of 200 ℃ and 200MPa, after the experiment is finished, releasing the pressure and sampling, drying the pressed sample in a drying oven at 60 ℃ to obtain the calcium sulfate whisker, wherein the average length of the obtained calcium sulfate whisker is 20.54 mu m, the average length-diameter ratio is 5.29, and an SEM picture of an experimental finished product is shown in figure 2.
EXAMPLE III
As shown in fig. 1, the method for preparing calcium sulfate whiskers by using the phosphogypsum high-temperature high-pressure method in this embodiment specifically includes the following steps:
s1: pretreating raw materials of phosphogypsum and diatomite;
s2: weighing 4.75g of pretreated powdery phosphogypsum and 0.25g of diatomite powder, placing the mixture in an agate mortar, and stirring for 30min to fully and uniformly mix the mixture to prepare a composite system A with the mass of 5 g;
s3: weighing 0.5m L deionized water, pouring into the composite system A in the step S2, stirring for 5min, and obtaining a plastic composite system B after the stirring is finished;
s4: filling the plastic composite system B into a small polytetrafluoroethylene cap (with the inner diameter of 10mm, the outer diameter of 12mm and the height of 12mm), and then sleeving and sealing the small polytetrafluoroethylene cap (with the inner diameter of 12mm, the outer diameter of 14mm and the height of 12mm) to obtain a sample C;
s5: and putting the sample C into a high-temperature high-pressure reaction kettle, keeping the temperature and the pressure constant for 24h under the conditions of 200 ℃ and 200MPa, after the experiment is finished, releasing the pressure and sampling, and drying the pressed sample in a drying oven at 60 ℃ to obtain the calcium sulfate whisker, wherein the average length of the obtained calcium sulfate whisker is 18.54 mu m, and the average length-diameter ratio of the obtained calcium sulfate whisker is 3.48.
Example four
As shown in fig. 1, the method for preparing calcium sulfate whiskers by using the phosphogypsum high-temperature high-pressure method in this embodiment specifically includes the following steps:
s1: pretreating raw materials of phosphogypsum and diatomite;
s2: weighing 4.25g of pretreated powdery phosphogypsum and 0.75g of diatomite powder, placing the mixture in an agate mortar, and stirring for 30min to fully and uniformly mix the mixture to prepare a composite system A with the mass of 5 g;
s3: weighing 0.5m L deionized water, pouring into the composite system A in the step S2, stirring for 5min, and obtaining a plastic composite system B after the stirring is finished;
s4: filling the plastic composite system B into a small polytetrafluoroethylene cap (with the inner diameter of 10mm, the outer diameter of 12mm and the height of 12mm), and then sleeving and sealing the small polytetrafluoroethylene cap (with the inner diameter of 12mm, the outer diameter of 14mm and the height of 12mm) to obtain a sample C;
s5: and putting the sample C into a high-temperature high-pressure reaction kettle, keeping the temperature and the pressure constant for 24h under the conditions of 200 ℃ and 200MPa, after the experiment is finished, releasing the pressure and sampling, and drying the pressed sample in a drying oven at 60 ℃ to obtain the calcium sulfate whisker, wherein the average length of the obtained calcium sulfate whisker is 20.84 mu m, and the average length-diameter ratio is 4.35.
EXAMPLE five
As shown in fig. 1, the method for preparing calcium sulfate whiskers by using the phosphogypsum high-temperature high-pressure method in this embodiment specifically includes the following steps:
s1: pretreating raw materials of phosphogypsum and diatomite;
s2: weighing 4.5g of pretreated powdery phosphogypsum and 0.5g of diatomite powder, placing the mixture in an agate mortar, and stirring for 45min to fully and uniformly mix the mixture to prepare a composite system A with the mass of 5 g;
s3: weighing 0.5m L deionized water, pouring into the composite system A in the step S2, stirring for 7.5min, and obtaining a plastic composite system B after stirring;
s4: filling the plastic composite system B into a small polytetrafluoroethylene cap (with the inner diameter of 10mm, the outer diameter of 12mm and the height of 12mm), and then sleeving and sealing the small polytetrafluoroethylene cap (with the inner diameter of 12mm, the outer diameter of 14mm and the height of 12mm) to obtain a sample C;
s5: and putting the sample C into a high-temperature high-pressure reaction kettle, keeping the temperature and the pressure constant for 24h under the conditions of 250 ℃ and 250MPa, after the experiment is finished, releasing the pressure and sampling, and drying the pressed sample in a drying oven at 70 ℃ to obtain the calcium sulfate whisker, wherein the average length of the obtained calcium sulfate whisker is 20.09 mu m, and the average length-diameter ratio of the obtained calcium sulfate whisker is 4.96.
EXAMPLE six
As shown in fig. 1, the method for preparing calcium sulfate whiskers by using the phosphogypsum high-temperature high-pressure method in this embodiment specifically includes the following steps:
s1: pretreating raw materials of phosphogypsum and diatomite;
s2: weighing 4.75g of pretreated powdery phosphogypsum and 0.25g of diatomite powder, placing the mixture in an agate mortar, and stirring for 60min to fully and uniformly mix the mixture to prepare a composite system A with the mass of 5 g;
s3: weighing 0.5m L deionized water, pouring into the composite system A in the step S2, stirring for 10min, and obtaining a plastic composite system B after the stirring is finished;
s4: filling the plastic composite system B into a small polytetrafluoroethylene cap (with the inner diameter of 10mm, the outer diameter of 12mm and the height of 12mm), and then sleeving and sealing the small polytetrafluoroethylene cap (with the inner diameter of 12mm, the outer diameter of 14mm and the height of 12mm) to obtain a sample C;
s5: and putting the sample C into a high-temperature high-pressure reaction kettle, keeping the temperature and the pressure constant for 24h under the conditions of 300 ℃ and 300MPa, after the experiment is finished, releasing the pressure and sampling, and drying the pressed sample in a drying oven at 80 ℃ to obtain the calcium sulfate whisker, wherein the average length of the obtained calcium sulfate whisker is 24.56 mu m, and the average length-diameter ratio is 9.17.
While embodiments of the invention have been shown and described, it will be understood by those of ordinary skill in the art that: various changes, modifications, substitutions and alterations can be made to the embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the claims and their equivalents.
Claims (9)
1. A method for preparing calcium sulfate whiskers by a phosphogypsum high-temperature high-pressure method is characterized by comprising the following steps:
s1: pretreating raw materials of phosphogypsum and diatomite;
s2: weighing a certain amount of raw materials, stirring for a period of time T1 and uniformly mixing to obtain a composite system A;
s3: adding water into the composite system A, and stirring for a period of time T2 to obtain a plastic composite system B;
s4: filling the plastic composite system B into a small polytetrafluoroethylene cap, and then sleeving and sealing the small polytetrafluoroethylene cap by using a large polytetrafluoroethylene cap to obtain a sample C;
s5: and (3) placing the sample C into a reaction kettle for high-temperature high-pressure reaction for a period of T3, relieving pressure, sampling and drying to obtain the calcium sulfate whisker.
2. The method for preparing calcium sulfate whiskers by using the phosphogypsum high-temperature high-pressure method according to claim 1, wherein in the step S1, the method for pretreating raw materials comprises the following steps: drying phosphogypsum in an oven at the temperature of (45 +/-3) DEG C to constant weight, and sieving the phosphogypsum by a sieve of 80 meshes; crushing and grinding the blocky diatomite, and sieving the blocky diatomite with a 200-mesh sieve.
3. The method for preparing calcium sulfate whiskers by using the phosphogypsum high-temperature high-pressure method according to claim 1, wherein in the step S2, the adding amount of the phosphogypsum is 85-95% of the mass of the composite system A, and the adding amount of the diatomite is 5-15% of the mass of the composite system A.
4. The method for preparing calcium sulfate whiskers through a phosphogypsum high-temperature high-pressure method according to claim 1, wherein in the step S2, the stirring time T1 is 30-60 min.
5. The method for preparing calcium sulfate whiskers by using the phosphogypsum high-temperature high-pressure method according to claim 1, wherein in the step S3, the solid-to-liquid ratio of the plastic composite system B is 10: 1.
6. The method for preparing calcium sulfate whiskers through a phosphogypsum high-temperature high-pressure method according to claim 1, wherein in the step S3, the stirring time T2 is 5-10 min.
7. The method for preparing calcium sulfate whiskers by using the phosphogypsum high-temperature high-pressure method according to claim 1, wherein in the step S4, the size of the small polytetrafluoroethylene cap is as follows: the inner diameter is 10mm, the outer diameter is 12mm, and the height is 12 mm; the size of the large polytetrafluoroethylene cap is as follows: 12mm inner diameter, 14mm outer diameter and 12mm height.
8. The method for preparing calcium sulfate whiskers by using the phosphogypsum high-temperature high-pressure method according to claim 1, wherein in the step S5, the reaction conditions are as follows: the reaction temperature is 200-300 ℃, the reaction pressure is 200-300 MPa, and the reaction time T3 is 24 h.
9. The method for preparing calcium sulfate whiskers by using the phosphogypsum high-temperature high-pressure method according to claim 1, wherein in the step S5, the drying temperature is 60-80 ℃ during drying.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111186913.3A CN113882021A (en) | 2021-10-12 | 2021-10-12 | Method for preparing calcium sulfate whisker by phosphogypsum high-temperature high-pressure method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111186913.3A CN113882021A (en) | 2021-10-12 | 2021-10-12 | Method for preparing calcium sulfate whisker by phosphogypsum high-temperature high-pressure method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113882021A true CN113882021A (en) | 2022-01-04 |
Family
ID=79006115
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111186913.3A Pending CN113882021A (en) | 2021-10-12 | 2021-10-12 | Method for preparing calcium sulfate whisker by phosphogypsum high-temperature high-pressure method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113882021A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115572455A (en) * | 2022-11-04 | 2023-01-06 | 贵州省材料产业技术研究院 | Phosphogypsum whisker/fiber reinforced composite material and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101092734A (en) * | 2007-04-16 | 2007-12-26 | 云南常青树化工有限公司 | Method for preparing crystal whisker of calcium sulphate, and phosphonic acid |
| CN102534801A (en) * | 2012-02-23 | 2012-07-04 | 云南民族大学 | Method for improving quality of calcium sulfate whiskers |
| CN103523814A (en) * | 2013-09-18 | 2014-01-22 | 西南科技大学 | Gypsum abnormity powder preparation and modification integrated method in normal-pressure open system |
| CN103526277A (en) * | 2012-10-26 | 2014-01-22 | 青岛科技大学 | Method for manufacturing gypsum whisker with hexagonal cross section and low phosphorus content |
| CN105568387A (en) * | 2016-02-26 | 2016-05-11 | 烟台大学 | Preparation method of calcium sulfate whiskers |
-
2021
- 2021-10-12 CN CN202111186913.3A patent/CN113882021A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101092734A (en) * | 2007-04-16 | 2007-12-26 | 云南常青树化工有限公司 | Method for preparing crystal whisker of calcium sulphate, and phosphonic acid |
| CN102534801A (en) * | 2012-02-23 | 2012-07-04 | 云南民族大学 | Method for improving quality of calcium sulfate whiskers |
| CN103526277A (en) * | 2012-10-26 | 2014-01-22 | 青岛科技大学 | Method for manufacturing gypsum whisker with hexagonal cross section and low phosphorus content |
| CN103523814A (en) * | 2013-09-18 | 2014-01-22 | 西南科技大学 | Gypsum abnormity powder preparation and modification integrated method in normal-pressure open system |
| CN105568387A (en) * | 2016-02-26 | 2016-05-11 | 烟台大学 | Preparation method of calcium sulfate whiskers |
Non-Patent Citations (2)
| Title |
|---|
| 周登峰等: "磷石膏-硅藻土高温高压试验及孔隙结构研究" * |
| 周登峰等: "磷石膏高温高压实验及其改性" * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115572455A (en) * | 2022-11-04 | 2023-01-06 | 贵州省材料产业技术研究院 | Phosphogypsum whisker/fiber reinforced composite material and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106278377B (en) | A kind of regeneration lightweight aggregate concrete self-insulating light wallboard and preparation method entirely | |
| CN106866052B (en) | A kind of red mud-slag geo-polymer and preparation method thereof | |
| CN106478002A (en) | A kind of vibration insulation and noise reduction rubber concrete and preparation method thereof | |
| CN102992717A (en) | Preparation method for high-molecular compound-containing metakaolin-based geopolymer cement | |
| CN103435319A (en) | Ardealite-based high-strength light building blocks prepared from ardealite and production process thereof | |
| CN111233360A (en) | Method for preparing geopolymer-based recycled aggregate from micro-fine particle copper tailings | |
| CN113651548B (en) | Ca/Al layered double hydroxide carbonate-based cementing material and preparation method and application thereof | |
| CN105152610A (en) | Method for modifying raw soil material by utilizing starch residue | |
| CN105060828A (en) | Dechlorinated alkali residue solidified soil for road engineering | |
| CN106187299B (en) | A method of hollow brick is manufactured using building waste | |
| CN113882021A (en) | Method for preparing calcium sulfate whisker by phosphogypsum high-temperature high-pressure method | |
| CN110258278A (en) | The press mortar and processing method to be come to nothing using microbial strains punishment cement pavement | |
| CN105777022A (en) | Ardealite concrete extrusion partition board and preparation method thereof | |
| CN102515581B (en) | Method for preparing ordinary portland cement by taking gold mine tailings as raw materials | |
| CN104386978A (en) | Plant fiber lightweight aggregate-raw soil thermal insulation block and preparation method thereof | |
| CN106277986A (en) | A kind of non-burning brick preparation method | |
| CN108178533A (en) | The preparation method of high-strength regenerative gel material product | |
| CN103864360A (en) | Heat insulation mortar with sound absorbing effect and manufacturing method thereof | |
| CN108706988A (en) | A kind of novel environment-friendly composite material and preparation method thereof applied to assembled architecture | |
| CN113200712A (en) | Iron-rich sludge/slag composite geopolymer and preparation method thereof | |
| CN113135724A (en) | Negative carbon emission modified raw soil base building block and manufacturing method thereof | |
| CN108409249A (en) | A kind of preparation method of resistance to compression water-permeable brick | |
| CN111548115A (en) | Preparation method for preparing environment-friendly insulating brick from tailing waste residues | |
| CN108675709B (en) | Method for preparing slope protection brick by utilizing soil after thermal desorption remediation and product thereof | |
| CN102503267B (en) | Flame-retardant type light-weight heat-preservation wall body material mixed with iron tailings and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20220104 |
|
| RJ01 | Rejection of invention patent application after publication |