CN112429759A - Micron-sized flower-shaped alpha-CaSO4·0.5H2Method for producing O crystal - Google Patents
Micron-sized flower-shaped alpha-CaSO4·0.5H2Method for producing O crystal Download PDFInfo
- Publication number
- CN112429759A CN112429759A CN202011415169.5A CN202011415169A CN112429759A CN 112429759 A CN112429759 A CN 112429759A CN 202011415169 A CN202011415169 A CN 202011415169A CN 112429759 A CN112429759 A CN 112429759A
- Authority
- CN
- China
- Prior art keywords
- caso
- crystal
- alpha
- sulfate
- micron
- 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.)
- Granted
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/46—Sulfates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/51—Particles with a specific particle size distribution
- C01P2004/52—Particles with a specific particle size distribution highly monodisperse size distribution
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
Micron-sized flower-shaped alpha-CaSO4·0.5H2Preparing a precursor calcium salt and sulfate by using deionized water to obtain a calcium salt solution and a sulfate solution respectively, mixing a composite inducer with the calcium salt solution, and preheating in a closed environment at the temperature of 120-130 ℃ under the stirring condition to obtain a preheated mixed solution; preheating sulfate solution in a closed environment at the temperature of 120-130 ℃ under the condition of stirring; mixing the preheated mixed solution and the preheated sulfate solution in a reaction kettle, stirring and reacting for 3-5 hours, after the reaction is finished, performing suction filtration and separation on a microfiltration membrane with the diameter of 0.2 mu m under the pressure of 0.5MPa to obtain a filter cake, washing the filter cake with deionized water for 2-4 times, then washing the filter cake with absolute ethyl alcohol for 2-4 times, and then drying the filter cake to obtain the micron-sized flower-shaped alpha-CaSO4·0.5H2And (4) O crystals. The synthetic auxiliary agent used in the invention is cheap, nontoxic and environment-friendly, and the synthesized alpha-CaSO4·0.5H2The O crystals are highly uniform with an average size of between 50 and 60 μm.
Description
Technical Field
The invention relates to a micron-sized flower-shaped alpha-CaSO4·0.5H2A preparation method of O crystal.
Background
The calcium sulfate crystal has three phases, namely calcium sulfate dihydrate (CaSO)4·2H2O), calcium sulfate hemihydrate (CaSO)4·0.5H2O) and calcium sulfate Anhydrous (CaSO)4). Wherein the calcium sulfate hemihydrate also has alpha-CaSO4·0.5H2O and beta-CaSO4·0.5H2And O, two crystal forms.
α-CaSO4·0.5H2O belongs to the monoclinic system, alpha-CaSO4·0.5H2-Ca-SO in O unit cell4 2-Ca-SO4 2--Ca-]Bone chain edgecGrowing in the axial direction and growing naturally into hexagonal prism-shaped crystals.
α-CaSO4·0.5H2The O crystal is slightly soluble in water, has hydration property, the compression strength of gypsum formed by the gelatinization of the O crystal exceeds 70MPa, the breaking strength exceeds 18MPa, and the O crystal can be used as a gelatinization material, a hydration adsorption material, a drug carrier and a high-strength building material.
α-CaSO4·0.5H2The preparation of O crystal mainly comprises a hydrothermal method, an atmospheric salt solution method and an atmospheric acidification method, and the alpha-CaSO prepared by the method4·0.5H2O is mostly elongated needle-like whiskers or hexagonsLong columnar crystals, non-one-dimensional ones are rarely reported.
The invention patent with the publication number of CN105603505B discloses a method for preparing calcium sulfate whiskers with high length-diameter ratio by using phosphogypsum as a hydrothermal method, and inorganic amorphous lattice cation pairs of alpha-CaSO4·0.5H2Has significant influence on the growth of O crystal, and inorganic amorphous lattice cations such as MgCl are added in the crystal preparation process2、CuCl2、ZnCl2And FeCl3Can prepare alpha-CaSO with the length-diameter ratio as high as 350:1 and uniform appearance4·0.5H2O crystal whisker.
Publication No. CN105332058A discloses a method for preparing gypsum whisker for papermaking by using phosphogypsum under normal pressure in a circulating dissolving method, and SO in a crystallization system is increased4 2-While introducing NH4 +Can promote alpha-CaSO4·0.5H2The nucleation rate of O crystal is increased, and alpha-CaSO with the length of 2000-5000 mu m and the length-diameter ratio of 300:1-250:1 is formed4·0.5H2O crystal whisker.
A number of patents and literature have shown that alpha-CaSO with high aspect ratio can be efficiently prepared by adding inorganic salts during crystallization4·0.5H2O crystal whisker. But in alpha-CaSO4·0.5H2In the crystallization process of the O crystal, the low length-diameter ratio short column-shaped alpha-CaSO can be prepared in a rotating packed bed reactor with the reaction temperature of 25-60 ℃ by assisting one or more of organic acid or organic acid salt such as citric acid, sodium citrate, sodium succinate, tartaric acid and oxalic acid4·0.5H2O crystals with a length of 15 μm and an aspect ratio of less than 3: 1.
Only one-dimensional alpha-CaSO has been disclosed4·0.5H2Synthesis of O crystals, non-one-dimensional alpha-CaSO4·0.5H2The synthesis of O crystal is rarely reported, which is related to alpha-CaSO4·0.5H2The O crystal growth mode is closely related. The southern hospital of southern medical university reports a process for preparing chitosan-coated strontium-containing calcium sulfate hemihydrate microspheres by heating a 15% sodium chloride solution to 102 deg.C and adding an acid solution to maintain the pH at 4-6Adding the mixture into the solution, adding 1% of chitosan, and reacting for 4-8h to prepare the chitosan-coated strontium-containing calcium sulfate hemihydrate microspheres.
One-dimensional alpha-CaSO with different systems and different length-diameter ratios4·0.5H2O crystal synthesis, and microspherical alpha-CaSO4·0.5H2The synthesis methods of O crystal are reported, but other non-one-dimensional crystal structures are rarely reported.
Disclosure of Invention
The invention aims to provide a micron-sized flower-shaped alpha-CaSO4·0.5H2A preparation method of O crystal.
In order to achieve the above objects and other related objects, the present invention provides the following technical solutions: micron-sized flower-shaped alpha-CaSO4·0.5H2A method for preparing O crystals, comprising the steps of:
step 1: respectively preparing a precursor calcium salt and a precursor sulfate by using deionized water to obtain a calcium salt solution and a sulfate solution, mixing a composite inducer with the calcium salt solution, and preheating in a 120-plus-130 ℃ closed environment under the stirring condition to obtain a preheated mixed solution; preheating a sulfate solution in a closed environment at the temperature of 120-130 ℃ under the stirring condition to obtain the sulfate solution;
step 2: mixing the preheated mixed solution and the preheated sulfate solution in a reaction kettle, stirring and reacting for 3-5 hours, after the reaction is finished, performing suction filtration and separation on a microfiltration membrane with the diameter of 0.2 mu m under the pressure of 0.5MPa to obtain a filter cake, washing the filter cake with deionized water for 2-4 times, then washing the filter cake with absolute ethyl alcohol for 2-4 times, and drying the filter cake to obtain the micron-sized flower-shaped alpha-CaSO4·0.5H2O crystals;
the composite inducer consists of a phase transfer agent, a buffering agent, a modifier and deionized water.
The preferable technical scheme is as follows: the precursor calcium salt is CaCl2Or Ca (NO)3)2Adding calcium salt CaCl2Or Ca (NO)3)2Dissolving in deionized water to obtain calcium salt solution.
The preferable technical scheme is as follows: what is needed isThe precursor sulfate is Na2SO4Dissolving in deionized water to obtain sulfate solution.
The preferable technical scheme is as follows: the phase transfer agent is glycerol, and the mass content of the phase transfer agent is 30-40% of that of the composite inducer; the buffer is sodium polyphosphate, the mass content is 8-15% of the compound inducer, the modifier is sodium propionate, sodium citrate or disodium ethylene diamine tetraacetate, the mass content is 8-15% of the compound inducer; the mass content of the deionized water is 30-40% of that of the composite inducer.
The preferable technical scheme is as follows: the molar ratio of the sulfate to the calcium salt is 1: 2-4; both the sulfate and calcium salts were analytically pure.
Due to the application of the technical scheme, compared with the prior art, the invention has the advantages that:
1. the invention selects a precursor and a compound inducer, wherein the compound inducer controls alpha-CaSO4·0.5H2Anisotropic growth of O crystals, the final growth being flower-like alpha-CaSO4·0.5H2O crystal, and the prepared product is highly uniform and has good dispersibility.
2. The invention has the advantages of simple reaction preparation process, low equipment requirement and environmental friendliness.
3. The invention and the conversion of desulfurized gypsum and phosphogypsum into CaSO4·2H2O is alpha-CaSO4·0.5H2Compared with O crystal, the raw materials are high-concentration calcium salt and sulfate, and the synthesized alpha-CaSO4·0.5H2The O crystal has high purity, less impurity and high production efficiency.
Drawings
FIG. 1 is a diagram of α -CaSO prepared in example 14·0.5H2SEM image of O crystal;
FIG. 2 is a diagram of α -CaSO prepared in example 14·0.5H2XRD pattern of O crystal;
FIG. 3 is the α -CaSO prepared in example 24·0.5H2SEM image of O crystal;
FIG. 4 is the α -CaSO prepared in example 24·0.5H2XRD pattern of O crystal;
FIG. 5 shows the preparation of example 3Preparation of alpha-CaSO4·0.5H2SEM image of O crystal;
FIG. 6 is a view of α -CaSO prepared in example 34·0.5H2XRD pattern of O crystal;
FIG. 7 is a view of α -CaSO prepared in example 34·0.5H2The effect graph of Pb adsorption of the O crystal;
FIG. 8 is a flower-like α -CaSO4·0.5H2A process flow diagram of the preparation method of the O crystal.
Detailed Description
The following description of the embodiments of the present invention is provided for illustrative purposes, and other advantages and effects of the present invention will become apparent to those skilled in the art from the present disclosure.
Please refer to fig. 1-8. It should be understood that the structures, ratios, sizes, and the like shown in the drawings and described in the specification are only used for matching with the disclosure of the specification, so as to be understood and read by those skilled in the art, and are not used to limit the conditions under which the present invention can be implemented, so that the present invention has no technical significance, and any structural modification, ratio relationship change, or size adjustment should still fall within the scope of the present invention without affecting the efficacy and the achievable purpose of the present invention. In addition, the terms "upper", "lower", "left", "right", "middle" and "one" used in the present specification are for clarity of description, and are not intended to limit the scope of the present invention, and the relative relationship between the terms and the terms is not to be construed as a scope of the present invention.
Example 1: micron-sized flower-shaped alpha-CaSO4·0.5H2Method for producing O crystal
Taking 1.5g of CaCl2Dissolving the precursor A in 100ml of deionized water, and fully dissolving to prepare a precursor A; taking 3.0g of Na2SO4Dissolving the precursor B in 100ml of deionized water, and fully dissolving to prepare a precursor B; respectively weighing 5g of glycerol, 0.12g of sodium polyphosphate and 0.15g of sodium propionate, dissolving in 15g of deionized water, stirring, heating and fully dissolving to prepare a composite inducer; compounding inducerMixing the mixture in a precursor B, and preheating to 115 ℃; preheating the precursor B to 115 ℃, mixing the precursor A, the composite inducer and the precursor B in a reaction kettle, and reacting at the reaction temperature of 115 ℃ and 200rpm for 4 hours; carrying out solid-liquid separation on the reacted sample, washing the reacted sample for three times by using deionized water and absolute ethyl alcohol, placing the washed sample in a vacuum drying oven, and drying the sample for 12 hours at 70 ℃ and then collecting the sample; the prepared sample is characterized by flower-shaped alpha-CaSO with the diameter of 50-55 mu m4·0.5H2O crystals (see fig. 1 and 2).
Example 2: micron-sized flower-shaped alpha-CaSO4·0.5H2Method for producing O crystal
Taking 1.2g of CaCl2Dissolving the precursor A in 100ml of deionized water, and fully dissolving to prepare a precursor A; 3.6g of Na are taken2SO4Dissolving the precursor B in 100ml of deionized water, and fully dissolving to prepare a precursor B; respectively weighing 4.5g of glycerol, 0.3g of sodium polyphosphate and 0.2g of sodium citrate, dissolving in 15g of deionized water, stirring, heating and fully dissolving to prepare a composite inducer; mixing the composite inducer in the precursor B, and preheating to 120 ℃; preheating the precursor B to 120 ℃, mixing the precursor A, the composite inducer and the precursor B in a reaction kettle, and reacting at the reaction temperature of 120 ℃ and 200rpm for 4 hours; carrying out solid-liquid separation on the reacted sample, washing the reacted sample for three times by using deionized water and absolute ethyl alcohol, placing the washed sample in a vacuum drying oven, and drying the sample for 12 hours at 70 ℃ and then collecting the sample; the prepared sample is characterized by being flower-shaped alpha-CaSO with the diameter of 55-60 mu m4·0.5H2O crystals (see fig. 3 and 4).
Example 3: micron-sized flower-shaped alpha-CaSO4·0.5H2Method for producing O crystal
Take 2.2gCa (NO)3)2Dissolving the precursor A in 100ml of deionized water, and fully dissolving to prepare a precursor A; taking 4.5g of Na2SO4Dissolving the precursor B in 100ml of deionized water, and fully dissolving to prepare a precursor B; respectively weighing 4g of glycerol, 0.25g of sodium polyphosphate and 0.1g of disodium ethylene diamine tetraacetate, dissolving in 15g of deionized water, stirring, heating and fully dissolving to prepare a composite inducer; mixing the composite inducer in the precursor B, and preheating to 128 ℃; preheating the precursor B to 128 ℃, and then adding the precursor A, a composite inducer andmixing the precursor B in a reaction kettle, and reacting for 4 hours at the reaction temperature of 128 ℃ and the rpm of 200; carrying out solid-liquid separation on the reacted sample, washing the reacted sample for three times by using deionized water and absolute ethyl alcohol, placing the washed sample in a vacuum drying oven, and drying the sample for 12 hours at 70 ℃ and then collecting the sample; the prepared sample is characterized by flower-shaped alpha-CaSO with the diameter of 50-55 mu m4·0.5H2O crystals (see fig. 5 and 6); soaking the prepared flower-shaped crystal in Pb-containing water solution, standing for 12h, separating out solid, drying, detecting a large amount of Pb adsorbed on the crystal surface by SEM energy spectrum (see figure 7), and measuring the content of flower-shaped alpha-CaSO per gram by atomic absorption spectrometry4·0.5H2The O crystals adsorbed 0.207 g of Pb.
Example 4: micron-sized flower-shaped alpha-CaSO4·0.5H2Method for producing O crystal
Micron-sized flower-shaped alpha-CaSO4·0.5H2A method for preparing O crystals, comprising the steps of:
step 1: respectively preparing a precursor calcium salt and a precursor sulfate by using deionized water to obtain a calcium salt solution and a sulfate solution, mixing a composite inducer with the calcium salt solution, and preheating in a 120 ℃ closed environment under the stirring condition to obtain a preheated mixed solution; preheating a sulfate solution in a closed environment at 120 ℃ under the condition of stirring to obtain the sulfate solution;
step 2: mixing the preheated mixed solution and the preheated sulfate solution in a reaction kettle, stirring and reacting for 3 hours, after the reaction is finished, performing suction filtration and separation on a microfiltration membrane with the diameter of 0.2 mu m under the pressure of 0.5MPa to obtain a filter cake, washing the filter cake for 2 times by using deionized water, washing the filter cake for 2 times by using absolute ethyl alcohol, and drying the filter cake to obtain the micron-sized flower-shaped alpha-CaSO4·0.5H2O crystals;
the composite inducer consists of a phase transfer agent, a buffering agent, a modifier and deionized water.
The preferred embodiment is: the precursor calcium salt is CaCl2Adding calcium salt CaCl2Dissolving in deionized water to obtain calcium salt solution.
The preferred embodiment is: the precursor sulfate is Na2SO4Dissolving in deionized water to obtain sulfate solution.
The preferred embodiment is: the phase transfer agent is glycerol, and the mass content of the phase transfer agent is 30% of that of the composite inducer; the buffer is sodium polyphosphate, the mass content of the buffer is 15% of that of the compound inducer, the modifier is sodium propionate, and the mass content of the modifier is 15% of that of the compound inducer; the mass content of the deionized water is 40% of that of the composite inducer.
The preferred embodiment is: the molar ratio of the sulfate to the calcium salt is 1: 2; both the sulfate and calcium salts were analytically pure.
Example 5: micron-sized flower-shaped alpha-CaSO4·0.5H2Method for producing O crystal
Micron-sized flower-shaped alpha-CaSO4·0.5H2A preparation method of O crystal. The synthetic auxiliary agent used in the embodiment is cheap, nontoxic and environment-friendly, and the synthesized alpha-CaSO4·0.5H2The O crystals are highly uniform with an average size of between 50 and 60 μm. The flower-shaped alpha-CaSO of the invention4·0.5H2The O crystal has good adsorption capacity for Pb in wastewater, and has the advantages of simple reaction preparation process, low equipment requirement, environmental friendliness and the like.
This example synthesizes flower-like alpha-CaSO4·0.5H2The precursor used by the O crystal is Na2SO4、CaCl2Or Ca (NO)3)2The raw materials are AR grade, and the molar concentration of the two precursors is controlled to be 1: 3.
This example synthesizes flower-like alpha-CaSO4·0.5H2The addition amount of the compound inducer used by the O crystal is less than 10 percent of the total mass of the crystallization system, and the compound inducer consists of a phase transfer agent, a buffering agent, a modifying agent and an auxiliary agent.
Wherein the content of the phase transfer agent in the composite inducer is 40 percent of the mass percentage of the composite inducer.
The content of the buffer is less than 10% of the mass percentage of the composite inducer.
The content of the modifier is less than 10% of the mass percent of the composite inducer.
The content of the auxiliary agent is less than 40 percent of the mass percent of the composite inducer.
The phase transfer agent is glycerol.
The buffer is sodium polyphosphate.
The modifier is sodium propionate, sodium citrate or disodium ethylene diamine tetraacetate; this example is specifically sodium citrate
The auxiliary agent is deionized water.
The synthesis temperature was 125 ℃ and the stirring rate was 200 rpm.
The application of the composite inducer in the embodiment is to prepare micron-sized flower-shaped alpha-CaSO in the presence of the composite inducer4·0.5H2O crystal, the preparation steps are as follows:
preparing precursor calcium salt and sulfate solution with deionized water respectively; preparing a compound inducer solution; dissolving and mixing a composite inducer and calcium salt, fully stirring and preheating at 125 ℃ in a closed environment; stirring and preheating the sulfate at 125 ℃ in a closed environment; mixing the two preheated solutions in a reaction kettle after the two preheated solutions reach the set temperature, and stirring for reaction for 4 hours; after the reaction is finished, a microfiltration membrane with the diameter of 0.2 mu m is used for filtering and separating solids under the pressure of 0.5 MPa; washing the filter cake 3 times with 100g of normal temperature deionized water and absolute ethyl alcohol; the resulting filter cake was collected, dispersed and dried in a vacuum oven at 70 ℃ for 12 hours.
The characterization test shows that the synthesized product is flower-shaped alpha-CaSO with the diameter of 50-60 mu m4·0.5H2O crystal with purity of 99.5-99.9%.
Flower-shaped alpha-CaSO per gram4·0.5H2The O crystals adsorbed 0.207 g of Pb.
The foregoing is illustrative of the preferred embodiment of the present invention and is not to be construed as limiting thereof in any way, and any modifications or variations thereof that fall within the spirit of the invention are intended to be included within the scope thereof.
Claims (5)
1. Micron-sized flower-shaped alpha-CaSO4·0.5H2The preparation method of the O crystal is characterized by comprising the following steps: comprises the following steps:
step 1: respectively preparing a precursor calcium salt and a precursor sulfate by using deionized water to obtain a calcium salt solution and a sulfate solution, mixing a composite inducer with the calcium salt solution, and preheating in a 120-plus-130 ℃ closed environment under the stirring condition to obtain a preheated mixed solution; preheating a sulfate solution in a closed environment at the temperature of 120-130 ℃ under the stirring condition to obtain the sulfate solution;
step 2: mixing the preheated mixed solution and the preheated sulfate solution in a reaction kettle, stirring and reacting for 3-5 hours, after the reaction is finished, performing suction filtration and separation on a microfiltration membrane with the diameter of 0.2 mu m under the pressure of 0.5MPa to obtain a filter cake, washing the filter cake with deionized water for 2-4 times, then washing the filter cake with absolute ethyl alcohol for 2-4 times, and drying the filter cake to obtain the micron-sized flower-shaped alpha-CaSO4·0.5H2O crystals;
the composite inducer consists of a phase transfer agent, a buffering agent, a modifier and deionized water.
2. The micron-sized flower-like alpha-CaSO of claim 14·0.5H2The preparation method of the O crystal is characterized by comprising the following steps: the precursor calcium salt is CaCl2Or Ca (NO)3)2Adding calcium salt CaCl2Or Ca (NO)3)2Dissolving in deionized water to obtain calcium salt solution.
3. The micron-sized flower-like alpha-CaSO of claim 14·0.5H2The preparation method of the O crystal is characterized by comprising the following steps: the precursor sulfate is Na2SO4Dissolving in deionized water to obtain sulfate solution.
4. The micron-sized flower-like alpha-CaSO of claim 14·0.5H2The preparation method of the O crystal is characterized by comprising the following steps: the phase transfer agent is glycerol, and the mass content of the phase transfer agent is 30-40% of that of the composite inducer; the buffer is sodium polyphosphate with the mass content of8-15% of the composite inducer, wherein the modifier is sodium propionate, sodium citrate or disodium ethylene diamine tetraacetate, and the mass content of the modifier is 8-15% of the composite inducer; the mass content of the deionized water is 30-40% of that of the composite inducer.
5. The micron-sized flower-like alpha-CaSO of claim 14·0.5H2The preparation method of the O crystal is characterized by comprising the following steps: the molar ratio of the sulfate to the calcium salt is 1: 2-4; both the sulfate and calcium salts were analytically pure.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011415169.5A CN112429759B (en) | 2020-12-07 | 2020-12-07 | Micron-sized flower-shaped alpha-CaSO4·0.5H2Method for producing O crystal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011415169.5A CN112429759B (en) | 2020-12-07 | 2020-12-07 | Micron-sized flower-shaped alpha-CaSO4·0.5H2Method for producing O crystal |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN112429759A true CN112429759A (en) | 2021-03-02 |
| CN112429759B CN112429759B (en) | 2022-11-01 |
Family
ID=74692001
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011415169.5A Active CN112429759B (en) | 2020-12-07 | 2020-12-07 | Micron-sized flower-shaped alpha-CaSO4·0.5H2Method for producing O crystal |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112429759B (en) |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3848070A (en) * | 1971-10-05 | 1974-11-12 | Kureha Chemical Ind Co Ltd | Method for producing calcium sulfite semihydrate |
| US4226636A (en) * | 1977-12-30 | 1980-10-07 | Tokuyama Soda Kabushiki Kaisha | Production of calcium silicate having high specific bulk volume and calcium silicate-gypsum composite |
| US20120093771A1 (en) * | 2010-10-19 | 2012-04-19 | National Cheng Kung University | Method for preparing a hardened calcium sulfate dihydrate block and use thereof |
| CN103723757A (en) * | 2012-10-10 | 2014-04-16 | 深圳兰度生物材料有限公司 | Preparation method of medical grade alpha-calcium sulfate hemihydrate |
| CN103922379A (en) * | 2014-03-31 | 2014-07-16 | 北京工业大学 | Preparation method of bunch-shaped calcium sulphate dihydrate |
| CN106395879A (en) * | 2016-08-29 | 2017-02-15 | 安徽六国化工股份有限公司 | Preparation method of large particle size calcium sulphate dihydrate in wet-process phosphoric acid technology |
| CN108314074A (en) * | 2018-03-28 | 2018-07-24 | 湘潭大学 | A kind of preparation method of gypsum micro-sphere material |
| CN110422868A (en) * | 2019-05-17 | 2019-11-08 | 湖北民族大学 | Crystal modifier, medical sheet α-half-H 2 O calcium sulphate and preparation method thereof |
-
2020
- 2020-12-07 CN CN202011415169.5A patent/CN112429759B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3848070A (en) * | 1971-10-05 | 1974-11-12 | Kureha Chemical Ind Co Ltd | Method for producing calcium sulfite semihydrate |
| US4226636A (en) * | 1977-12-30 | 1980-10-07 | Tokuyama Soda Kabushiki Kaisha | Production of calcium silicate having high specific bulk volume and calcium silicate-gypsum composite |
| US20120093771A1 (en) * | 2010-10-19 | 2012-04-19 | National Cheng Kung University | Method for preparing a hardened calcium sulfate dihydrate block and use thereof |
| CN103723757A (en) * | 2012-10-10 | 2014-04-16 | 深圳兰度生物材料有限公司 | Preparation method of medical grade alpha-calcium sulfate hemihydrate |
| CN103922379A (en) * | 2014-03-31 | 2014-07-16 | 北京工业大学 | Preparation method of bunch-shaped calcium sulphate dihydrate |
| CN106395879A (en) * | 2016-08-29 | 2017-02-15 | 安徽六国化工股份有限公司 | Preparation method of large particle size calcium sulphate dihydrate in wet-process phosphoric acid technology |
| CN108314074A (en) * | 2018-03-28 | 2018-07-24 | 湘潭大学 | A kind of preparation method of gypsum micro-sphere material |
| CN110422868A (en) * | 2019-05-17 | 2019-11-08 | 湖北民族大学 | Crystal modifier, medical sheet α-half-H 2 O calcium sulphate and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| QIAOSHAN CHEN ET AL.: "A facile method to control the structure and morphology of α-calcium sulfate hemihydrate", 《CRYSTENGCOMM》 * |
| XIANGBIN SUN ET AL.: "Aspect ratio-controlled preparation of a CaSO4$0.5H2O from phosphogypsum in potassium tartrate aqueous solution", 《RSC ADVANCES》 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN112429759B (en) | 2022-11-01 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US7700066B1 (en) | Process for preparing alpha calcium sulfate hemihydrate | |
| NZ575529A (en) | Process for manufacturing ultra low consistency alpha - and beta - blend stucco | |
| CN107746195B (en) | Method for efficiently producing α type semi-hydrated gypsum | |
| KR102070380B1 (en) | Method for producing synthetic hectorite at low temperature and atmospheric pressure | |
| CN101550344B (en) | Method for preparing magnesium hydroxide/silicon dioxide composite inorganic flame retardant | |
| CN112777579B (en) | Method for preparing short columnar alpha-CaSO4.0.5H2O by crystallization through one-step dihydrate-semi-hydrate wet phosphoric acid process | |
| CN111825111B (en) | Preparation method for improving thermal stability of magnesium-aluminum hydrotalcite | |
| CN109052446B (en) | Method for preparing calcium-aluminum hydrotalcite by using industrial waste residues as raw materials | |
| CN112429759B (en) | Micron-sized flower-shaped alpha-CaSO4·0.5H2Method for producing O crystal | |
| CN110407220B (en) | Rapid preparation method of SAPO-34 molecular sieve with large specific surface area | |
| CN107473244B (en) | A kind of method that spodumene prepares lithium carbonate by-product potassium type zeolite | |
| CN105236780A (en) | Method for preparation of high strength alpha-semi-hydrated gypsum by self-curing modification steam pressurization | |
| CN102167300A (en) | Method for preparing hexagonal micro powder hydroxyapatite material | |
| CN116903020A (en) | Method for preparing alpha-hemihydrate gypsum stable under normal pressure | |
| CN102351207B (en) | Method for preparing nano attapulgite by solvothermal process | |
| CN114349039B (en) | Method for regulating and controlling morphology and granularity of alpha-hemihydrate gypsum crystal in solution system | |
| CN1724479A (en) | Method of comprehensive utilization of phophogypsum | |
| CN110422868B (en) | Crystal transformation agent, medical flaky alpha-calcium sulfate hemihydrate and preparation method thereof | |
| CN114907036A (en) | Calcium carbonate gel, preparation method and application | |
| CN107572542B (en) | Method for preparing nano kaolinite by using muscovite powder | |
| CN113292092A (en) | Preparation method of high-magnesium calcite | |
| CN114751440B (en) | Simple green template-free method for preparing anhydrous CaSO 4 Method for preparing micro/nano crystal and product | |
| CN112811449A (en) | Novel method for preparing magnesium-aluminum hydrotalcite | |
| KR20180054057A (en) | Method for producing synthetic hectorite at low temperature and atmospheric pressure | |
| CN115196664B (en) | Calcium sulfate dihydrate containing only eutectic phosphorus 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 | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |