CN110040991A - A method of quickly preparing short cylinder sulfate hemihydrate calcium material using calcium sulphate dihydrate - Google Patents
A method of quickly preparing short cylinder sulfate hemihydrate calcium material using calcium sulphate dihydrate Download PDFInfo
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- CN110040991A CN110040991A CN201910373883.3A CN201910373883A CN110040991A CN 110040991 A CN110040991 A CN 110040991A CN 201910373883 A CN201910373883 A CN 201910373883A CN 110040991 A CN110040991 A CN 110040991A
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- Prior art keywords
- calcium
- sulphate dihydrate
- calcium sulphate
- water
- short cylinder
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B11/00—Calcium sulfate cements
- C04B11/02—Methods and apparatus for dehydrating gypsum
- C04B11/028—Devices therefor characterised by the type of calcining devices used therefor or by the type of hemihydrate obtained
- C04B11/032—Devices therefor characterised by the type of calcining devices used therefor or by the type of hemihydrate obtained for the wet process, e.g. dehydrating in solution or under saturated vapour conditions, i.e. to obtain alpha-hemihydrate
Abstract
The invention belongs to field of inorganic nonmetallic material, disclose a kind of method that short cylinder sulfate hemihydrate calcium material is quickly prepared using calcium sulphate dihydrate, recrystallization process occurs for common calcium sulphate dihydrate original structure after processing, crystal growth is complete, without Shrinkage Problem, the short cylinder sulfate hemihydrate calcium material use value with higher prepared.Calcium sulphate dihydrate controls the dissolution and recrystallization speed of crystal face according to the difference of each crystal face energy by the difference of energy possessed by crystal difference crystal face under different solutions system, and then completes the growth behavior control of short cylinder material.This method be calcium sulphate dihydrate is ground, the reaction of ingredient, hydrothermal solution, separation and the processes composition such as dry.The problems such as present invention can not only effectively solve the easy dusting of calcium sulphate dihydrate, intensity difference and stability are low, can also extend the application field of calcium sulfate, have important practical significance to efficient utilize of China's flue gas desulfurization product and gypsum resource.
Description
Technical field
The invention belongs to field of inorganic nonmetallic material, it is related to a kind of quickly preparing short cylinder half using calcium sulphate dihydrate
The method of H 2 O calcium sulphate material.
Background technique
Inorganic material oriented growth control technology is most important in inorganic non-metallic material technology of preparing, not only influences
To crystal structure performance, and also relate to its application field.Short cylinder sulfate hemihydrate calcium material is as a kind of high-intensity inorganic
Crystalline material, because its performance is stablized, intensity is high, can significantly improve the comprehensive mechanical property of cement preparation, to concrete and builds
The application market of the raising and gypsum of building material property all has important function.
With the rapid development of our country's economy, environment and land occupation are not only polluted in the increase year by year of solid waste,
And huge waste is caused to resource.2018, China only industrial waste gypsum resource discharge amount just more than 100,000,000 tons or more.I
The annual gypsum materials demand amount of state is huge, and the exploitation of one side natural gypsum mineral is not only caused by land reclamation vegetation
Destruction be easy to cause the safe gypsum of class that caves in and due to gypsoide springy texture；Another aspect China waste gypsum
Stock number is huge.Therefore, in view of China's waste gypsum current resources situation, if calcium sulphate dihydrate can be prepared into short cylinder material half
Water gypsum material will have great importance to the higher value application of the large waste gypsum resource in China.
Calcium sulphate dihydrate usually exists under field conditions (factors) with lamellar form, and the particle of flake superposition composition
Calcium sulphate dihydrate is often accompanied by a large amount of defects in additive process and exists in shape object, especially Industrial Solid Waste, so short cylinder material
The preparation of material half-H 2 O calcium sulphate crystal is particularly important, and it is steady that the result of study of this patent not only can solve calcium sulphate dihydrate
Qualitative difference and easy pulverizing problem, can also significantly improve the comprehensive mechanical property of calcium sulfate.
Chinese patent (Publication No. CN107721220A) describes for gypsum to be added to the water, and is configured to slurry,
The aqueous solution of medium crystallization agent is added into slurry, is stirred evenly under room temperature, obtains reaction system；Wherein, medium crystallization agent be band phenyl ring or
The polybasic carboxylic acid of hexatomic ring, the polycarboxylate with phenyl ring or hexatomic ring or be the multi-anhydride with phenyl ring or hexatomic ring；
Reaction system is moved into hydrothermal reaction kettle, hydro-thermal reaction is carried out；It is cooling after hydro-thermal reaction, to obtained suspension mistake
Filter, drying, obtain short cylinder αsemiwatergypsum.The difference of this patent and the patent (CN107721220A) is the reaction time
It significantly reduces, 20~40min is foreshortened to by minimum 3h~6h；Additive is by the polybasic carboxylic acid with phenyl ring or hexatomic ring, band phenyl ring
Or hexatomic ring polycarboxylate or be that the multi-anhydride type organic with phenyl ring or hexatomic ring is changed to magnesium chloride and lemon
Sour calcium compound, calcium chloride and magnesium citrate mixture, magnesium chloride and gluconic acid calcium compound and calcium chloride and glucose
Sour magnesium compound class nontoxicity environment-friendly type substance, this cleans and innoxious peace short cylinder half-H 2 O calcium sulphate crystalline material
Full production has important practical significance.
Summary of the invention
The present invention provides a kind of method that short cylinder sulfate hemihydrate calcium material is quickly prepared using calcium sulphate dihydrate, places
Recrystallization process occurs for common calcium sulphate dihydrate original structure after reason, and crystal growth is complete, no Shrinkage Problem, and for preparing is short
Column sulfate hemihydrate calcium material use value with higher.Calcium sulphate dihydrate is under different solutions system by crystal difference
Energy possessed by crystal face is different, according to the difference of each crystal face energy, controls the dissolution and recrystallization speed of crystal face, in turn
Complete the growth behavior control of short cylinder material.
The technical solution adopted by the invention is as follows:
A method of quickly preparing short cylinder sulfate hemihydrate calcium material using calcium sulphate dihydrate, including the following steps:
(1) calcium sulphate dihydrate is placed in the ball grinder of planetary ball mill, planetary ball mill revolution be 50~
Under conditions of 200r/min, 30~60min is ground；Calcium sulphate dihydrate granularity after grinding is controlled at≤5 μm, with additive and
Water mixing, is placed in high-pressure bottle, and 20~40min is kept the temperature at 120~160 DEG C, and pressure is 0.1~2MPa.Wherein add
Agent is one of following: magnesium chloride and calcium citrate mixture, calcium chloride and magnesium citrate mixture, magnesium chloride and grape
Saccharic acid calcium compound and calcium chloride and gluconic acid magnesium compound；
(2) to separate after reaction, the solid product isolated is placed in 120 DEG C of blast drier and is dried
10~30min is handled, the liquid phase circulation after separation uses.
The solid-to-liquid ratio of the calcium sulphate dihydrate and water is 1:6~1:14, and the mass ratio of additive and water is 1:40~1:
100。
The consersion unit used for titanium system is rapidly heated autoclave or enamel is rapidly heated autoclave, is increased to from 20 DEG C
160 DEG C of time is 1~3h.
The present invention can prepare short cylinder sulfate hemihydrate calcium material, belong to by (002), (200), (110) and (1-10)
Crystal face and its symmetrical crystal face, which enclose, forms short cylinder crystalline material, and longitudinal length and lateral length ratio are 1~3.It is preparing
Three-waste free discharge in the process, solution use closed cycle, non-environmental-pollution problem, meet China develop a circular economy and energy conservation
The target of emission reduction.The problems such as present invention can not only effectively solve the easy dusting of calcium sulphate dihydrate, intensity difference and stability are low, also
The application field that calcium sulfate can be extended shows China's flue gas desulfurization product and the efficient of gypsum resource using with important
Sincere justice.
Specific embodiment
Specific embodiments of the present invention are described in detail below in conjunction with technical solution.
Embodiment 1:
Calcium sulphate dihydrate is placed in the ball grinder of planetary ball mill, is 200r/min's in planetary ball mill revolution
Under the conditions of, grind 30min；Calcium sulphate dihydrate granularity after grinding is controlled at≤5 μm, with additive (calcium chloride and magnesium citrate
Ratio 1:1) and water mixing, wherein the mass ratio of additive and water is 1:40, and the solid-to-liquid ratio of calcium sulphate dihydrate and water is 1:6, is put
It is placed in high-pressure bottle, the time that 120 DEG C are increased to from 20 DEG C is 1h, pressure 1MPa, and keeps the temperature 40min at 120 DEG C；
To separate after reaction, the solid product isolated is placed in 120 DEG C of blast drier and 30min is dried, point
Liquid phase circulation from after uses.Prepared short cylinder sulfate hemihydrate calcium material belongs to by (002), (200), (110) and (1-
10) crystal face and its symmetrical crystal face, which enclose, forms short cylinder crystalline material, and longitudinal length and lateral length ratio are 3 or so.
Embodiment 2:
Calcium sulphate dihydrate is placed in the ball grinder of planetary ball mill, in the item that planetary ball mill revolution is 50r/min
Under part, 60min is ground；Calcium sulphate dihydrate granularity after grinding is controlled at≤5 μm, is mixed with additive and water, wherein additive
It is 1:100 with the mass ratio of water, wherein additive is calcium chloride and magnesium citrate mixture (1:1), calcium sulphate dihydrate and water
Solid-to-liquid ratio is 1:14, is placed in high-pressure bottle, and the time that 160 DEG C are increased to from 20 DEG C is 3h, pressure 2MPa, and 160
20min is kept the temperature at DEG C；To separate after reaction, the solid product isolated is placed in 120 DEG C of blast drier and is done
Dry processing 10min, the liquid phase circulation after separation use.Prepared short cylinder sulfate hemihydrate calcium material, belong to by (002),
(200), (110) and (1-10) crystal face and its symmetrical crystal face, which enclose, forms short cylinder crystalline material, longitudinal length and laterally length
Spending ratio is 1 or so.
Embodiment 3:
Calcium sulphate dihydrate is placed in the ball grinder of planetary ball mill, is 180r/min's in planetary ball mill revolution
Under the conditions of, grind 30min；Calcium sulphate dihydrate granularity after grinding is controlled at≤5 μm, is mixed with additive and water, wherein adding
The mass ratio of agent and water is 1:90, and wherein additive is calcium chloride and magnesium citrate mixture (1:1), calcium sulphate dihydrate and water
Solid-to-liquid ratio be 1:12, be placed in high-pressure bottle, be increased to from 20 DEG C 150 DEG C time be 2.5h, pressure 1.5MPa,
And 25min is kept the temperature at 150 DEG C；To separate after reaction, the solid product isolated is placed in 120 DEG C of blast drier
In 15min is dried, liquid phase circulation after separation uses.Prepared short cylinder sulfate hemihydrate calcium material, belong to by
(002), (200), (110) and (1-10) crystal face and its symmetrical crystal face, which enclose, forms short cylinder crystalline material, longitudinal length with
Lateral length ratio is 2 or so.
Embodiment 4:
Calcium sulphate dihydrate is placed in the ball grinder of planetary ball mill, is 160r/min's in planetary ball mill revolution
Under the conditions of, grind 35min；Calcium sulphate dihydrate granularity after grinding is controlled at≤5 μm, is mixed with additive and water, wherein adding
The mass ratio of agent and water is 1:80, and wherein additive is calcium chloride and magnesium citrate mixture (1:1), calcium sulphate dihydrate and water
Solid-to-liquid ratio be 1:11, be placed in high-pressure bottle, be increased to from 20 DEG C 160 DEG C time be 2h, pressure 1.2MPa, and
30min is kept the temperature at 160 DEG C；To separate after reaction, the solid product isolated is placed in 120 DEG C of blast drier
20min is dried, the liquid phase circulation after separation uses.Prepared short cylinder sulfate hemihydrate calcium material, belong to by
(002), (200), (110) and (1-10) crystal face and its symmetrical crystal face, which enclose, forms short cylinder crystalline material, longitudinal length with
Lateral length ratio is 1.5 or so.
Embodiment 5:
Calcium sulphate dihydrate is placed in the ball grinder of planetary ball mill, is 140r/min's in planetary ball mill revolution
Under the conditions of, grind 40min；Calcium sulphate dihydrate granularity after grinding is controlled at≤5 μm, is mixed with additive and water, wherein adding
The mass ratio of agent and water is 1:70, and wherein additive is calcium chloride and magnesium citrate mixture (1:1), calcium sulphate dihydrate and water
Solid-to-liquid ratio be 1:10, be placed in high-pressure bottle, be increased to from 20 DEG C 140 DEG C time be 1.5h, pressure 1MPa, and
35min is kept the temperature at 140 DEG C；To separate after reaction, the solid product isolated is placed in 120 DEG C of blast drier
25min is dried, the liquid phase circulation after separation uses.Prepared short cylinder sulfate hemihydrate calcium material, belong to by
(002), (200), (110) and (1-10) crystal face and its symmetrical crystal face, which enclose, forms short cylinder crystalline material, longitudinal length with
Lateral length ratio is 1 or so.
Embodiment 6:
Calcium sulphate dihydrate is placed in the ball grinder of planetary ball mill, is 120r/min's in planetary ball mill revolution
Under the conditions of, grind 45min；Calcium sulphate dihydrate granularity after grinding is controlled at≤5 μm, is mixed with additive and water, wherein adding
The mass ratio of agent and water is 1:60, and wherein additive is calcium chloride and magnesium citrate mixture (1:1), calcium sulphate dihydrate and water
Solid-to-liquid ratio be 1:9, be placed in high-pressure bottle, be increased to from 20 DEG C 130 DEG C time be 1h, pressure 0.8MPa, and
40min is kept the temperature at 130 DEG C；To separate after reaction, the solid product isolated be placed in 120 DEG C of blast drier into
Row is dried 30min, and the liquid phase circulation after separation uses.Prepared short cylinder sulfate hemihydrate calcium material, belong to by
(002), (200), (110) and (1-10) crystal face and its symmetrical crystal face, which enclose, forms short cylinder crystalline material, longitudinal length with
Lateral length ratio is 3 or so.
Embodiment 7:
Calcium sulphate dihydrate is placed in the ball grinder of planetary ball mill, is 100r/min's in planetary ball mill revolution
Under the conditions of, grind 50min；Calcium sulphate dihydrate granularity after grinding is controlled at≤5 μm, is mixed with additive and water, wherein adding
The mass ratio of agent and water is 1:50, and wherein additive is calcium chloride and magnesium citrate mixture (1:1), calcium sulphate dihydrate and water
Solid-to-liquid ratio be 1:8, be placed in high-pressure bottle, be increased to from 20 DEG C 150 DEG C time be 2h, pressure 16MPa, and
20min is kept the temperature at 150 DEG C；To separate after reaction, the solid product isolated be placed in 120 DEG C of blast drier into
Row is dried 15min, and the liquid phase circulation after separation uses.Prepared short cylinder sulfate hemihydrate calcium material, belong to by
(002), (200), (110) and (1-10) crystal face and its symmetrical crystal face, which enclose, forms short cylinder crystalline material, longitudinal length with
Lateral length ratio is 2 or so.
Embodiment 8:
Calcium sulphate dihydrate is placed in the ball grinder of planetary ball mill, in the item that planetary ball mill revolution is 80r/min
Under part, 55min is ground；Calcium sulphate dihydrate granularity after grinding is controlled at≤5 μm, is mixed with additive and water, wherein additive
It is 1:45 with the mass ratio of water, wherein additive is calcium chloride and magnesium citrate mixture (1:1), calcium sulphate dihydrate and water
Solid-to-liquid ratio is 1:7, is placed in high-pressure bottle, is increased to 130 DEG C of time from 20 DEG C as 2.5h, pressure 1.8MPa, and
30min is kept the temperature at 130 DEG C；To separate after reaction, the solid product isolated be placed in 120 DEG C of blast drier into
Row is dried 20min, and the liquid phase circulation after separation uses.Prepared short cylinder sulfate hemihydrate calcium material, belong to by
(002), (200), (110) and (1-10) crystal face and its symmetrical crystal face, which enclose, forms short cylinder crystalline material, longitudinal length with
Lateral length ratio is 3 or so.
Embodiment 9:
Calcium sulphate dihydrate is placed in the ball grinder of planetary ball mill, in the item that planetary ball mill revolution is 60r/min
Under part, 60min is ground；Calcium sulphate dihydrate granularity after grinding is controlled at≤5 μm, is mixed with additive and water, wherein additive
It is 1:90 with the mass ratio of water, wherein additive is calcium chloride and magnesium citrate mixture (1:1), calcium sulphate dihydrate and water
Solid-to-liquid ratio is 1:13, is placed in high-pressure bottle, is increased to 120 DEG C of time from 20 DEG C as 2h, pressure 0.1MPa, and
40min is kept the temperature at 120 DEG C；To separate after reaction, the solid product isolated be placed in 120 DEG C of blast drier into
Row is dried 30min, and the liquid phase circulation after separation uses.Prepared short cylinder sulfate hemihydrate calcium material, belong to by
(002), (200), (110) and (1-10) crystal face and its symmetrical crystal face, which enclose, forms short cylinder crystalline material, longitudinal length with
Lateral length ratio is 1.5 or so.
Embodiment 10:
Calcium sulphate dihydrate is placed in the ball grinder of planetary ball mill, is 200r/min's in planetary ball mill revolution
Under the conditions of, grind 30min；Calcium sulphate dihydrate granularity after grinding is controlled at≤5 μm, is mixed with additive and water, wherein adding
The mass ratio of agent and water is 1:75, and wherein additive is magnesium chloride and calcium citrate mixture (1:1), calcium sulphate dihydrate and water
Solid-to-liquid ratio be 1:8, be placed in high-pressure bottle, be increased to from 20 DEG C 140 DEG C time be 2.5h, pressure 1.6MPa, and
10min is kept the temperature at 140 DEG C；To separate after reaction, the solid product isolated is placed in 120 DEG C of blast drier
25min is dried, the liquid phase circulation after separation uses.Prepared short cylinder sulfate hemihydrate calcium material, belong to by
(002), (200), (110) and (1-10) crystal face and its symmetrical crystal face, which enclose, forms short cylinder crystalline material, longitudinal length with
Lateral length ratio is 1 or so.
Embodiment 11:
Calcium sulphate dihydrate is placed in the ball grinder of planetary ball mill, in the item that planetary ball mill revolution is 50r/min
Under part, 60min is ground；Calcium sulphate dihydrate granularity after grinding is controlled at≤5 μm, is mixed with additive and water, wherein additive
It is 1:65 with the mass ratio of water, wherein additive is magnesium chloride and calcium citrate mixture (1:1), calcium sulphate dihydrate and water
Solid-to-liquid ratio is 1:12, is placed in high-pressure bottle, is increased to 130 DEG C of time from 20 DEG C as 1.5h, pressure 0.4MPa, and
30min is kept the temperature at 130 DEG C；To separate after reaction, the solid product isolated is placed in 120 DEG C of blast drier
30min is dried, the liquid phase circulation after separation uses.Prepared short cylinder sulfate hemihydrate calcium material, belong to by
(002), (200), (110) and (1-10) crystal face and its symmetrical crystal face, which enclose, forms short cylinder crystalline material, longitudinal length with
Lateral length ratio is 2.5 or so.
Embodiment 12:
Calcium sulphate dihydrate is placed in the ball grinder of planetary ball mill, is 130r/min's in planetary ball mill revolution
Under the conditions of, grind 30min；Calcium sulphate dihydrate granularity after grinding is controlled at≤5 μm, is mixed with additive and water, wherein adding
The mass ratio of agent and water is 1:45, and wherein additive is magnesium chloride and calcium citrate mixture (1:1), calcium sulphate dihydrate and water
Solid-to-liquid ratio be 1:9, be placed in high-pressure bottle, be increased to from 20 DEG C 160 DEG C time be 2h, pressure 1.5MPa, and
20min is kept the temperature at 160 DEG C；To separate after reaction, the solid product isolated be placed in 120 DEG C of blast drier into
Row is dried 10min, and the liquid phase circulation after separation uses.Prepared short cylinder sulfate hemihydrate calcium material, belong to by
(002), (200), (110) and (1-10) crystal face and its symmetrical crystal face, which enclose, forms short cylinder crystalline material, longitudinal length with
Lateral length ratio is 3 or so.
Embodiment 13:
Calcium sulphate dihydrate is placed in the ball grinder of planetary ball mill, is 150r/min's in planetary ball mill revolution
Under the conditions of, grind 35min；Calcium sulphate dihydrate granularity after grinding is controlled at≤5 μm, is mixed with additive and water, wherein adding
The mass ratio of agent and water is 1:80, and wherein additive is magnesium chloride and calcium citrate mixture (1:1), calcium sulphate dihydrate and water
Solid-to-liquid ratio be 1:10, be placed in high-pressure bottle, be increased to from 20 DEG C 140 DEG C time be 2.5h, pressure 2MPa, and
10min is kept the temperature at 140 DEG C；To separate after reaction, the solid product isolated is placed in 120 DEG C of blast drier
10min is dried, the liquid phase circulation after separation uses.Prepared short cylinder sulfate hemihydrate calcium material, belong to by
(002), (200), (110) and (1-10) crystal face and its symmetrical crystal face, which enclose, forms short cylinder crystalline material, longitudinal length with
Lateral length ratio is 1 or so.
Embodiment 14:
Calcium sulphate dihydrate is placed in the ball grinder of planetary ball mill, is 170r/min's in planetary ball mill revolution
Under the conditions of, grind 45min；Calcium sulphate dihydrate granularity after grinding is controlled at≤5 μm, is mixed with additive and water, wherein adding
The mass ratio of agent and water is 1:60, and wherein additive is magnesium chloride and calcium citrate mixture (1:1), calcium sulphate dihydrate and water
Solid-to-liquid ratio be 1:11, be placed in high-pressure bottle, be increased to from 20 DEG C 150 DEG C time be 2h, pressure 1MPa, and
30min is kept the temperature at 150 DEG C；To separate after reaction, the solid product isolated be placed in 120 DEG C of blast drier into
Row is dried 30min, and the liquid phase circulation after separation uses.Prepared short cylinder sulfate hemihydrate calcium material, belong to by
(002), (200), (110) and (1-10) crystal face and its symmetrical crystal face, which enclose, forms short cylinder crystalline material, longitudinal length with
Lateral length ratio is 2.5 or so.
Embodiment 15:
Calcium sulphate dihydrate is placed in the ball grinder of planetary ball mill, in the item that planetary ball mill revolution is 90r/min
Under part, 45min is ground；Calcium sulphate dihydrate granularity after grinding is controlled at≤5 μm, is mixed with additive and water, wherein additive
It is 1:95 with the mass ratio of water, wherein additive is magnesium chloride and calcium citrate mixture (1:1), calcium sulphate dihydrate and water
Solid-to-liquid ratio is 1:12, is placed in high-pressure bottle, and the time that 120 DEG C are increased to from 20 DEG C is 3h, pressure 2MPa, and 120
20min is kept the temperature at DEG C；To separate after reaction, the solid product isolated is placed in 120 DEG C of blast drier and is done
Dry processing 10min, the liquid phase circulation after separation use.Prepared short cylinder sulfate hemihydrate calcium material, belong to by (002),
(200), (110) and (1-10) crystal face and its symmetrical crystal face, which enclose, forms short cylinder crystalline material, longitudinal length and laterally length
Spending ratio is 2 or so.
Embodiment 16:
Calcium sulphate dihydrate is placed in the ball grinder of planetary ball mill, in the item that planetary ball mill revolution is 70r/min
Under part, 30min is ground；Calcium sulphate dihydrate granularity after grinding is controlled at≤5 μm, is mixed with additive and water, wherein additive
It is 1:60 with the mass ratio of water, wherein additive is magnesium chloride and calcium citrate mixture (1:1), calcium sulphate dihydrate and water
Solid-to-liquid ratio is 1:10, is placed in high-pressure bottle, is increased to 150 DEG C of time from 20 DEG C as 1.5h, pressure 1MPa, and
30min is kept the temperature at 150 DEG C；To separate after reaction, the solid product isolated be placed in 120 DEG C of blast drier into
Row is dried 30min, and the liquid phase circulation after separation uses.Prepared short cylinder sulfate hemihydrate calcium material, belong to by
(002), (200), (110) and (1-10) crystal face and its symmetrical crystal face, which enclose, forms short cylinder crystalline material, longitudinal length with
Lateral length ratio is 3 or so.
Embodiment 17:
Calcium sulphate dihydrate is placed in the ball grinder of planetary ball mill, is 110r/min's in planetary ball mill revolution
Under the conditions of, grind 40min；Calcium sulphate dihydrate granularity after grinding is controlled at≤5 μm, is mixed with additive and water, wherein adding
The mass ratio of agent and water is 1:50, and wherein additive is magnesium chloride and calcium citrate mixture (1:1), calcium sulphate dihydrate and water
Solid-to-liquid ratio be 1:7, be placed in high-pressure bottle, be increased to from 20 DEG C 160 DEG C time be 1h, pressure 0.8MPa, and
30min is kept the temperature at 160 DEG C；To separate after reaction, the solid product isolated be placed in 120 DEG C of blast drier into
Row is dried 20min, and the liquid phase circulation after separation uses.Prepared short cylinder sulfate hemihydrate calcium material, belong to by
(002), (200), (110) and (1-10) crystal face and its symmetrical crystal face, which enclose, forms short cylinder crystalline material, longitudinal length with
Lateral length ratio is 2 or so.
Embodiment 18:
Calcium sulphate dihydrate is placed in the ball grinder of planetary ball mill, is 190r/min's in planetary ball mill revolution
Under the conditions of, grind 60min；Calcium sulphate dihydrate granularity after grinding is controlled at≤5 μm, is mixed with additive and water, wherein adding
The mass ratio of agent and water is 1:60, and wherein additive is magnesium chloride and calcium citrate mixture (1:1), calcium sulphate dihydrate and water
Solid-to-liquid ratio be 1:8, be placed in high-pressure bottle, be increased to from 20 DEG C 140 DEG C time be 1.5h, pressure 0.5MPa, and
20min is kept the temperature at 140 DEG C；To separate after reaction, the solid product isolated is placed in 120 DEG C of blast drier
30min is dried, the liquid phase circulation after separation uses.Prepared short cylinder sulfate hemihydrate calcium material, belong to by
(002), (200), (110) and (1-10) crystal face and its symmetrical crystal face, which enclose, forms short cylinder crystalline material, longitudinal length with
Lateral length ratio is 1.5 or so.
Embodiment 19:
Calcium sulphate dihydrate is placed in the ball grinder of planetary ball mill, is 200r/min's in planetary ball mill revolution
Under the conditions of, grind 30min；Calcium sulphate dihydrate granularity after grinding is controlled at≤5 μm, with additive (calcium chloride and gluconic acid
Magnesium ratio 1:1) and water mixing, wherein the mass ratio of additive and water is 1:40, and the solid-to-liquid ratio of calcium sulphate dihydrate and water is 1:6,
It is placed in high-pressure bottle, the time that 120 DEG C are increased to from 20 DEG C is 3h, pressure 0.1MPa, and is kept the temperature at 120 DEG C
40min；To separate after reaction, the solid product isolated is placed in 120 DEG C of blast drier and is dried
30min, the liquid phase circulation after separation use.Prepared short cylinder sulfate hemihydrate calcium material, belong to by (002), (200),
(110) it encloses with (1-10) crystal face and its symmetrical crystal face and forms short cylinder crystalline material, longitudinal length and lateral length ratio
It is 3 or so.
Embodiment 20:
Calcium sulphate dihydrate is placed in the ball grinder of planetary ball mill, in the item that planetary ball mill revolution is 50r/min
Under part, 60min is ground；Calcium sulphate dihydrate granularity after grinding is controlled at≤5 μm, is mixed with additive and water, wherein additive
Mass ratio with water is 1:100, and wherein additive is calcium chloride and gluconic acid magnesium compound (1:1), calcium sulphate dihydrate and water
Solid-to-liquid ratio be 1:14, be placed in high-pressure bottle, be increased to from 20 DEG C 160 DEG C time be 3h, pressure 1.2MPa, and
20min is kept the temperature at 160 DEG C；To separate after reaction, the solid product isolated is placed in 120 DEG C of blast drier
10min is dried, the liquid phase circulation after separation uses.Prepared short cylinder sulfate hemihydrate calcium material, belong to by
(002), (200), (110) and (1-10) crystal face and its symmetrical crystal face, which enclose, forms short cylinder crystalline material, longitudinal length with
Lateral length ratio is 1 or so.
Embodiment 21:
Calcium sulphate dihydrate is placed in the ball grinder of planetary ball mill, is 180r/min's in planetary ball mill revolution
Under the conditions of, grind 30min；Calcium sulphate dihydrate granularity after grinding is controlled at≤5 μm, is mixed with additive and water, wherein adding
The mass ratio of agent and water is 1:90, and wherein additive is calcium chloride and gluconic acid magnesium compound (1:1), calcium sulphate dihydrate with
The solid-to-liquid ratio of water is 1:12, is placed in high-pressure bottle, and the time that 150 DEG C are increased to from 20 DEG C is 2.5h, and pressure is
1.5MPa, and 25min is kept the temperature at 150 DEG C；To separate after reaction, the solid product isolated is placed in 120 DEG C of air blast
15min is dried in drier, the liquid phase circulation after separation uses.Prepared short cylinder sulfate hemihydrate calcium material,
Belong to and is enclosed by (002), (200), (110) and (1-10) crystal face and its symmetrical crystal face into short cylinder crystalline material, longitudinal direction
Length and lateral length ratio are 3 or so.
Embodiment 22:
Calcium sulphate dihydrate is placed in the ball grinder of planetary ball mill, is 160r/min's in planetary ball mill revolution
Under the conditions of, grind 35min；Calcium sulphate dihydrate granularity after grinding is controlled at≤5 μm, is mixed with additive and water, wherein adding
The mass ratio of agent and water is 1:80, and wherein additive is calcium chloride and gluconic acid magnesium compound (1:1), calcium sulphate dihydrate with
The solid-to-liquid ratio of water be 1:11, be placed in high-pressure bottle, be increased to from 20 DEG C 160 DEG C time be 2h, pressure 1.2MPa,
And 30min is kept the temperature at 160 DEG C；To separate after reaction, the solid product isolated is placed in 120 DEG C of blast drier
In 20min is dried, liquid phase circulation after separation uses.Prepared short cylinder sulfate hemihydrate calcium material, belong to by
(002), (200), (110) and (1-10) crystal face and its symmetrical crystal face, which enclose, forms short cylinder crystalline material, longitudinal length with
Lateral length ratio is 2 or so.
Embodiment 23:
Calcium sulphate dihydrate is placed in the ball grinder of planetary ball mill, is 140r/min's in planetary ball mill revolution
Under the conditions of, grind 40min；Calcium sulphate dihydrate granularity after grinding is controlled at≤5 μm, is mixed with additive and water, wherein adding
The mass ratio of agent and water is 1:70, and wherein additive is calcium chloride and gluconic acid magnesium compound (1:1), calcium sulphate dihydrate with
The solid-to-liquid ratio of water be 1:10, be placed in high-pressure bottle, be increased to from 20 DEG C 140 DEG C time be 1.5h, pressure 1MPa,
And 35min is kept the temperature at 140 DEG C；To separate after reaction, the solid product isolated is placed in 120 DEG C of blast drier
In 25min is dried, liquid phase circulation after separation uses.Prepared short cylinder sulfate hemihydrate calcium material, belong to by
(002), (200), (110) and (1-10) crystal face and its symmetrical crystal face, which enclose, forms short cylinder crystalline material, longitudinal length with
Lateral length ratio is 1 or so.
Embodiment 24:
Calcium sulphate dihydrate is placed in the ball grinder of planetary ball mill, is 120r/min's in planetary ball mill revolution
Under the conditions of, grind 45min；Calcium sulphate dihydrate granularity after grinding is controlled at≤5 μm, is mixed with additive and water, wherein adding
The mass ratio of agent and water is 1:60, and wherein additive is calcium chloride and gluconic acid magnesium compound (1:1), calcium sulphate dihydrate with
The solid-to-liquid ratio of water is 1:9, is placed in high-pressure bottle, is increased to 130 DEG C of time from 20 DEG C as 1h, pressure 0.8MPa, and
40min is kept the temperature at 130 DEG C；To separate after reaction, the solid product isolated is placed in 120 DEG C of blast drier
30min is dried, the liquid phase circulation after separation uses.Prepared short cylinder sulfate hemihydrate calcium material, belong to by
(002), (200), (110) and (1-10) crystal face and its symmetrical crystal face, which enclose, forms short cylinder crystalline material, longitudinal length with
Lateral length ratio is 1.5 or so.
Embodiment 25:
Calcium sulphate dihydrate is placed in the ball grinder of planetary ball mill, is 100r/min's in planetary ball mill revolution
Under the conditions of, grind 50min；Calcium sulphate dihydrate granularity after grinding is controlled at≤5 μm, is mixed with additive and water, wherein adding
The mass ratio of agent and water is 1:50, and wherein additive is calcium chloride and gluconic acid magnesium compound (1:1), calcium sulphate dihydrate with
The solid-to-liquid ratio of water is 1:8, is placed in high-pressure bottle, is increased to 150 DEG C of time from 20 DEG C as 2h, pressure 1.6MPa, and
20min is kept the temperature at 150 DEG C；To separate after reaction, the solid product isolated is placed in 120 DEG C of blast drier
15min is dried, the liquid phase circulation after separation uses.Prepared short cylinder sulfate hemihydrate calcium material, belong to by
(002), (200), (110) and (1-10) crystal face and its symmetrical crystal face, which enclose, forms short cylinder crystalline material, longitudinal length with
Lateral length ratio is 2 or so.
Embodiment 26:
Calcium sulphate dihydrate is placed in the ball grinder of planetary ball mill, in the item that planetary ball mill revolution is 80r/min
Under part, 55min is ground；Calcium sulphate dihydrate granularity after grinding is controlled at≤5 μm, is mixed with additive and water, wherein additive
Mass ratio with water is 1:45, and wherein additive is calcium chloride and gluconic acid magnesium compound (1:1), calcium sulphate dihydrate and water
Solid-to-liquid ratio be 1:7, be placed in high-pressure bottle, be increased to from 20 DEG C 130 DEG C time be 2.5h, pressure 1.8MPa, and
30min is kept the temperature at 130 DEG C；To separate after reaction, the solid product isolated is placed in 120 DEG C of blast drier
20min is dried, the liquid phase circulation after separation uses.Prepared short cylinder sulfate hemihydrate calcium material, belong to by
(002), (200), (110) and (1-10) crystal face and its symmetrical crystal face, which enclose, forms short cylinder crystalline material, longitudinal length with
Lateral length ratio is 3 or so.
Embodiment 27:
Calcium sulphate dihydrate is placed in the ball grinder of planetary ball mill, in the item that planetary ball mill revolution is 60r/min
Under part, 60min is ground；Calcium sulphate dihydrate granularity after grinding is controlled at≤5 μm, is mixed with additive and water, wherein additive
Mass ratio with water is 1:90, and wherein additive is calcium chloride and gluconic acid magnesium compound (1:1), calcium sulphate dihydrate and water
Solid-to-liquid ratio be 1:13, be placed in high-pressure bottle, be increased to from 20 DEG C 120 DEG C time be 2h, pressure 1.5MPa, and
20min is kept the temperature at 120 DEG C；To separate after reaction, the solid product isolated is placed in 120 DEG C of blast drier
30min is dried, the liquid phase circulation after separation uses.Prepared short cylinder sulfate hemihydrate calcium material, belong to by
(002), (200), (110) and (1-10) crystal face and its symmetrical crystal face, which enclose, forms short cylinder crystalline material, longitudinal length with
Lateral length ratio is 2.5 or so.
Embodiment 28:
Calcium sulphate dihydrate is placed in the ball grinder of planetary ball mill, is 200r/min's in planetary ball mill revolution
Under the conditions of, grind 30min；Calcium sulphate dihydrate granularity after grinding is controlled at≤5 μm, with additive (magnesium chloride and gluconic acid
Ca proportion 1:1) and water mixing, wherein the mass ratio of additive and water is 1:40, and the solid-to-liquid ratio of calcium sulphate dihydrate and water is 1:6,
It is placed in high-pressure bottle, the time that 120 DEG C are increased to from 20 DEG C is 1h, pressure 0.1MPa, and is kept the temperature at 120 DEG C
40min；To separate after reaction, the solid product isolated is placed in 120 DEG C of blast drier and is dried
30min, the liquid phase circulation after separation use.Prepared short cylinder sulfate hemihydrate calcium material, belong to by (002), (200),
(110) it encloses with (1-10) crystal face and its symmetrical crystal face and forms short cylinder crystalline material, longitudinal length and lateral length ratio
It is 3 or so.
Embodiment 29:
Calcium sulphate dihydrate is placed in the ball grinder of planetary ball mill, in the item that planetary ball mill revolution is 50r/min
Under part, 60min is ground；Calcium sulphate dihydrate granularity after grinding is controlled at≤5 μm, is mixed with additive and water, wherein additive
Mass ratio with water is 1:100, and wherein additive is magnesium chloride and gluconic acid calcium compound (1:1), calcium sulphate dihydrate and water
Solid-to-liquid ratio be 1:14, be placed in high-pressure bottle, be increased to from 20 DEG C 160 DEG C time be 3h, pressure 2MPa, and
20min is kept the temperature at 160 DEG C；To separate after reaction, the solid product isolated be placed in 120 DEG C of blast drier into
Row is dried 10min, and the liquid phase circulation after separation uses.Prepared short cylinder sulfate hemihydrate calcium material, belong to by
(002), (200), (110) and (1-10) crystal face and its symmetrical crystal face, which enclose, forms short cylinder crystalline material, longitudinal length with
Lateral length ratio is 1 or so.
Embodiment 30:
Calcium sulphate dihydrate is placed in the ball grinder of planetary ball mill, is 180r/min's in planetary ball mill revolution
Under the conditions of, grind 30min；Calcium sulphate dihydrate granularity after grinding is controlled at≤5 μm, is mixed with additive and water, wherein adding
The mass ratio of agent and water is 1:90, and wherein additive is magnesium chloride and gluconic acid calcium compound (1:1), calcium sulphate dihydrate with
The solid-to-liquid ratio of water is 1:12, is placed in high-pressure bottle, and the time that 150 DEG C are increased to from 20 DEG C is 2.5h, and pressure is
1.5MPa, and 25min is kept the temperature at 150 DEG C；To separate after reaction, the solid product isolated is placed in 120 DEG C of air blast
15min is dried in drier, the liquid phase circulation after separation uses.Prepared short cylinder sulfate hemihydrate calcium material,
Belong to and is enclosed by (002), (200), (110) and (1-10) crystal face and its symmetrical crystal face into short cylinder crystalline material, longitudinal direction
Length and lateral length ratio are 2 or so.
Embodiment 31:
Calcium sulphate dihydrate is placed in the ball grinder of planetary ball mill, is 160r/min's in planetary ball mill revolution
Under the conditions of, grind 35min；Calcium sulphate dihydrate granularity after grinding is controlled at≤5 μm, is mixed with additive and water, wherein adding
The mass ratio of agent and water is 1:80, and wherein additive is magnesium chloride and gluconic acid calcium compound (1:1), calcium sulphate dihydrate with
The solid-to-liquid ratio of water be 1:11, be placed in high-pressure bottle, be increased to from 20 DEG C 160 DEG C time be 2h, pressure 1.2MPa,
And 30min is kept the temperature at 160 DEG C；To separate after reaction, the solid product isolated is placed in 120 DEG C of blast drier
In 20min is dried, liquid phase circulation after separation uses.Prepared short cylinder sulfate hemihydrate calcium material, belong to by
(002), (200), (110) and (1-10) crystal face and its symmetrical crystal face, which enclose, forms short cylinder crystalline material, longitudinal length with
Lateral length ratio is 3 or so.
Embodiment 32:
Calcium sulphate dihydrate is placed in the ball grinder of planetary ball mill, is 140r/min's in planetary ball mill revolution
Under the conditions of, grind 40min；Calcium sulphate dihydrate granularity after grinding is controlled at≤5 μm, is mixed with additive and water, wherein adding
The mass ratio of agent and water is 1:70, and wherein additive is magnesium chloride and gluconic acid calcium compound (1:1), calcium sulphate dihydrate with
The solid-to-liquid ratio of water be 1:10, be placed in high-pressure bottle, be increased to from 20 DEG C 140 DEG C time be 1.5h, pressure 1MPa,
And 35min is kept the temperature at 140 DEG C；To separate after reaction, the solid product isolated is placed in 120 DEG C of blast drier
In 25min is dried, liquid phase circulation after separation uses.Prepared short cylinder sulfate hemihydrate calcium material, belong to by
(002), (200), (110) and (1-10) crystal face and its symmetrical crystal face, which enclose, forms short cylinder crystalline material, longitudinal length with
Lateral length ratio is 1 or so.
Embodiment 33:
Calcium sulphate dihydrate is placed in the ball grinder of planetary ball mill, is 120r/min's in planetary ball mill revolution
Under the conditions of, grind 45min；Calcium sulphate dihydrate granularity after grinding is controlled at≤5 μm, is mixed with additive and water, wherein adding
The mass ratio of agent and water is 1:60, and wherein additive is magnesium chloride and gluconic acid calcium compound (1:1), calcium sulphate dihydrate with
The solid-to-liquid ratio of water is 1:9, is placed in high-pressure bottle, is increased to 130 DEG C of time from 20 DEG C as 3h, pressure 0.8MPa, and
40min is kept the temperature at 130 DEG C；To separate after reaction, the solid product isolated is placed in 120 DEG C of blast drier
30min is dried, the liquid phase circulation after separation uses.Prepared short cylinder sulfate hemihydrate calcium material, belong to by
(002), (200), (110) and (1-10) crystal face and its symmetrical crystal face, which enclose, forms short cylinder crystalline material, longitudinal length with
Lateral length ratio is 3 or so.
Embodiment 34:
Calcium sulphate dihydrate is placed in the ball grinder of planetary ball mill, is 100r/min's in planetary ball mill revolution
Under the conditions of, grind 50min；Calcium sulphate dihydrate granularity after grinding is controlled at≤5 μm, is mixed with additive and water, wherein adding
The mass ratio of agent and water is 1:50, and wherein additive is magnesium chloride and gluconic acid calcium compound (1:1), calcium sulphate dihydrate with
The solid-to-liquid ratio of water is 1:8, is placed in high-pressure bottle, is increased to 150 DEG C of time from 20 DEG C as 2h, pressure 1.6MPa, and
20min is kept the temperature at 150 DEG C；To separate after reaction, the solid product isolated is placed in 120 DEG C of blast drier
15min is dried, the liquid phase circulation after separation uses.Prepared short cylinder sulfate hemihydrate calcium material, belong to by
(002), (200), (110) and (1-10) crystal face and its symmetrical crystal face, which enclose, forms short cylinder crystalline material, longitudinal length with
Lateral length ratio is 15 or so.
Embodiment 35:
Calcium sulphate dihydrate is placed in the ball grinder of planetary ball mill, in the item that planetary ball mill revolution is 80r/min
Under part, 55min is ground；Calcium sulphate dihydrate granularity after grinding is controlled at≤5 μm, is mixed with additive and water, wherein additive
Mass ratio with water is 1:45, and wherein additive is magnesium chloride and gluconic acid calcium compound (1:1), calcium sulphate dihydrate and water
Solid-to-liquid ratio be 1:7, be placed in high-pressure bottle, be increased to from 20 DEG C 130 DEG C time be 2.5h, pressure 1.8MPa, and
30min is kept the temperature at 130 DEG C；To separate after reaction, the solid product isolated is placed in 120 DEG C of blast drier
20min is dried, the liquid phase circulation after separation uses.Prepared short cylinder sulfate hemihydrate calcium material, belong to by
(002), (200), (110) and (1-10) crystal face and its symmetrical crystal face, which enclose, forms short cylinder crystalline material, longitudinal length with
Lateral length ratio is 2 or so.
Embodiment 36:
Calcium sulphate dihydrate is placed in the ball grinder of planetary ball mill, in the item that planetary ball mill revolution is 60r/min
Under part, 60min is ground；Calcium sulphate dihydrate granularity after grinding is controlled at≤5 μm, is mixed with additive and water, wherein additive
Mass ratio with water is 1:90, and wherein additive is magnesium chloride and gluconic acid calcium compound (1:1), calcium sulphate dihydrate and water
Solid-to-liquid ratio be 1:13, be placed in high-pressure bottle, be increased to from 20 DEG C 120 DEG C time be 2h, pressure 1.5MPa, and
20min is kept the temperature at 120 DEG C；To separate after reaction, the solid product isolated is placed in 120 DEG C of blast drier
30min is dried, the liquid phase circulation after separation uses.Prepared short cylinder sulfate hemihydrate calcium material, belong to by
(002), (200), (110) and (1-10) crystal face and its symmetrical crystal face, which enclose, forms short cylinder crystalline material, longitudinal length with
Lateral length ratio is 1.5 or so.
Claims (2)
1. a kind of method for quickly preparing short cylinder sulfate hemihydrate calcium material using calcium sulphate dihydrate, which is characterized in that including with
Lower step:
(1) calcium sulphate dihydrate being placed in planetary ball mill and is ground, the calcium sulphate dihydrate granularity after grinding is controlled at≤5 μm,
Mix, be placed in high-pressure bottle with additive and water, at 120~160 DEG C keep the temperature 20~40min, pressure be 0.1~
2MPa；Wherein, the additive is one of following: magnesium chloride and calcium citrate mixture, calcium chloride and magnesium citrate
Mixture, magnesium chloride and gluconic acid calcium compound, calcium chloride and gluconic acid magnesium compound；The calcium sulphate dihydrate and water
Solid-to-liquid ratio be 1:6~1:14；The mass ratio of the additive and water is 1:40~1:100；
(2) to separate after reaction, the solid product isolated is placed in 120 DEG C of blast drier and is dried 10
~30min, the liquid phase circulation after separation use.
2. a kind of side for quickly preparing short cylinder sulfate hemihydrate calcium material using calcium sulphate dihydrate according to claim 1
Method, it is characterized in that being: titanium system is rapidly heated autoclave or enamel is rapidly heated autoclave, from 20 DEG C be increased to 160 DEG C when
Between be 1~3h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112299468A (en) * | 2020-10-30 | 2021-02-02 | 山东聚鑫新材料有限公司 | Flaky calcium sulfate crystal and preparation method thereof |
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| CN112299468A (en) * | 2020-10-30 | 2021-02-02 | 山东聚鑫新材料有限公司 | Flaky calcium sulfate crystal and preparation method thereof |
| CN112299468B (en) * | 2020-10-30 | 2022-12-30 | 山东聚鑫新材料有限公司 | Flaky calcium sulfate crystal and preparation method thereof |
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