A kind of bouquet shape terra alba preparation method
Technical field
The invention belongs to materials chemistry inorganic materials preparing technical field, more specifically to a kind of preparation method of bouquet shape terra alba.
Background technology
The structure of crystal is controlled in crystal engineering research and is full of challenge, and causes different field scientific worker's broad interest always.
Terra alba, claims again gypsum.As the time-honored mineral starting material of one, unique and be easy to processing to eco-friendly, physicals because of it, more and more there is wide exploitation and application prospect in fields such as environment, health, buildings.The nearly more than ten years, gypsum is mainly concentrated on to crystal transition and stabilization research aspect both at home and abroad, by the aquation process of doping metals inorganic salt, inorganic molecules or organic polymer molecular Control plaster of Paris, and then the impact of its hardenite microstructure change of research gypsum intensity.M.M.Rashad has studied the spectrum change that organic/inorganic additive forms gypsum crystal in phosphoric acid solution simulated environment; St é phane Veesler has studied in dissimilar carboxylic acid environment semi-hydrated gypsum to the transforming relationship of dihydrate gypsum; Peng Jiahui studies the impact of plaster of Paris aquation process with gelatine, tripoly phosphate sodium STPP etc., has proposed the slow setting mechanism of additive to plaster of Paris; Yuan Zhitao is proposing the adsorption of stablizer to whisker surface aspect double water crystal whisker of gypsum stabilization treatment of research plurality of stable agent.But, so far, about in the aqueous solution, introduce lower concentration thickening material on dihydrate gypsum mineralising after the report of crystal morphology impact little.
As the fine etherate of a kind of carboxymethyl cellulose of obtaining through chemical modification, Xylo-Mucine (CMC) has than other thickening material and the more excellent performance of stablizer, has a wide range of applications in fields such as food, health, medicine, daily use chemicals.As everyone knows, the influence factor of gypsum product performance has grade of gypsum, time of coagulation, demould time, adulterant kind etc.Different varieties Additive can cause the microstructure change of gypsum, and then affects the performance of plastering.Therefore select the adulterant of adapted varieties to prepare the gypsum of special appearance particularly important.
Summary of the invention
For solving prior art problem, the invention provides a kind of bouquet shape terra alba preparation method.From the replacement(metathesis)reaction of calcium halide and vitriol, and then the synthetic calcium sulfate that contains two crystal water, be finally prepared into a kind of bouquet shape terra alba, synthetic route is simple, easy to operate, and productive rate is higher, the kind that further increases gypsum product, is expected to as building material product.
The technical solution adopted in the present invention is as follows:
A preparation method for bouquet shape terra alba, it comprises following steps:
A. calcium halide solution preparation: thickening material is stirred in the reactor adding containing deionized water to stirring, ultrasonic to dissolving; Then add calcium halide, be stirred to dissolving.
B. terra alba preparation: vitriol is stirred and is added in steps A calcium halide solution, continue to be stirred to precipitation and occur, filter and obtain terra alba filter cake;
C. washing: filter the terra alba filter cake obtaining directly with ethanol and water washing, or directly add ethanol and water washing after drying;
D. dry: the terra alba of ethanol and water washing is dried to obtain bouquet shape terra alba.
The calcium halide solution that described steps A obtains refers to that in concentration be the preferred 0.2-0.4wt% of 0.1-0.5wt%() thickener soln in add equivalent concentration calcium halide, calcium halide concentration 0.1-0.5M, 25-80 DEG C stir 0.5 hour.
Described thickening material refers to Xylo-Mucine (CMC).
Described calcium halide refers to calcium chloride.
Described vitriol refers to Potassium aluminum sulfate dodecahydrate.
The washing of described step C refers to that filtering the calcium sulfate filter cake that obtains adds under ethanol and hydroecium temperature and filter drip washing, or filters after the 50-80 DEG C of oven dry of calcium sulfate filter cake obtaining and add under ethanol and hydroecium temperature and filter drip washing.
The dry of described step D refers to that washed calcium sulfate filter cake obtains bouquet shape terra alba for 3-10 hour through 50-80 DEG C of oven dry.
Specific embodiment of the invention process is:
The deionized water of certain volume is mixed with to Xylo-Mucine (CMC) solution of concentration 0.1-0.5wt%, ultrasonic at 25-80 DEG C, stirring adds the calcium chloride of equivalent concentration 0.1-0.5M after 0.5 hour, at 25-80 DEG C, continue to stir 0.5 hour, then the Potassium aluminum sulfate dodecahydrate of equivalent concentration 0.05-0.25M is stirred and is added in calcium chloride solution, at 25-80 DEG C, continue to stir 0.5 hour, filter and obtain terra alba filter cake.The calcium sulfate filter cake that filtration obtains adds under ethanol and hydroecium temperature and filters drip washing, or filters after the 50-80 DEG C of oven dry of calcium sulfate filter cake obtaining and add under ethanol and hydroecium temperature and filter drip washing.Washed calcium sulfate filter cake is dried 3-10 hour to obtain bouquet shape terra alba through 50-80 DEG C.
A kind of bouquet shape terra alba preparation method of the present invention, from the replacement(metathesis)reaction of calcium halide and vitriol, and then the synthetic calcium sulfate that contains two crystal water, finally make a kind of bouquet shape sulfate dihydrate calcium material, synthetic route is simple, easy to operate, productive rate is higher, and the bouquet shape sulfate dihydrate calcium material of gained is fan-shaped bouquet shape.
Brief description of the drawings
In order more to express to clear and definite the technical scheme of this inventive embodiments, below embodiment is described in the accompanying drawing that uses be briefly described.Obviously, the accompanying drawing in below describing is only some embodiments of the present invention, for this field those of ordinary skill, under the prerequisite of not paying creative work, also can obtain according to this type of accompanying drawing other accompanying drawing.
Fig. 1 is the whole synthetic route chart of a kind of bouquet shape of the present invention terra alba;
Fig. 2 is the electron scanning micrograph of a kind of bouquet shape of the present invention terra alba;
Fig. 3 is the X-ray powder diffraction pattern of a kind of bouquet shape of the present invention terra alba;
Fig. 4 is the Fourier transform infrared spectroscopy figure of a kind of bouquet shape of the present invention terra alba;
Fig. 5 is the transmission electron microscope picture of a kind of bouquet shape of the present invention terra alba.
Embodiment
For making the object, technical solutions and advantages of the present invention clearer, below in conjunction with accompanying drawing, embodiment of the present invention is described further in detail.
Embodiment 1
The deionized water of 500mL is mixed with to Xylo-Mucine (CMC) solution of 0.2wt%, ultrasonic at 30 DEG C, stir the calcium chloride that adds equivalent concentration 0.1M after 0.5 hour, continue to stir 0.5 hour at 30 DEG C; Then the Potassium aluminum sulfate dodecahydrate of equivalent concentration 0.05M is stirred and is added in calcium chloride solution, continue to be stirred to precipitation at 30 DEG C to occur, filter and obtain terra alba filter cake; The calcium sulfate filter cake obtaining adds under ethanol and hydroecium temperature and filters drip washing, or filters after the 60 DEG C of oven dry of calcium sulfate filter cake that obtain and add under ethanol and hydroecium temperature and filter drip washing; Washed calcium sulfate filter cake is dried 5 hours to obtain bouquet shape terra alba through 50 DEG C.
The above-mentioned a kind of bouquet shape terra alba thing preparing is carried out to Measurement and analysis mutually, obtain electron scanning micrograph as shown in Figure 2, as shown in Figure 2: the calcium sulphate dihydrate obtaining is bouquet shape pattern.
Fig. 3 is the X-ray powder diffraction pattern of this kind of bouquet shape terra alba, as shown in Figure 3: bouquet shape Crystallization of Gypsum degree is higher.
Fig. 4 is the Fourier transform infrared spectroscopy figure of this kind of bouquet shape terra alba, as shown in Figure 4: 3522cm
-1with 3399cm
-1near absorption band belongs to the stretching vibration of bouquet shape terra alba hydroxyl and crystal water, 1619cm
-1near absorption band belongs to the flexural vibration of bouquet shape terra alba hydroxyl, 1103cm
-1, 667cm
-1with 598cm
-1near absorption band belongs to stretching vibration and the flexural vibration of bouquet shape terra alba sulfate radical.
Fig. 5 is the transmission electron microscope picture of this kind of bouquet shape terra alba, as shown in Figure 5: bouquet shape terra alba is single crystalline structure, and preferential (021) and (041) crystal face of exposing.
Embodiment 2
The deionized water of 1000mL is mixed with to Xylo-Mucine (CMC) solution of 0.4wt%, ultrasonic at 50 DEG C, stir after 0.5 hour and add equivalent concentration 0.3M calcium chloride, continue to stir 0.5 hour at 50 DEG C; Then the Potassium aluminum sulfate dodecahydrate of equivalent concentration 0.15M is stirred and is added in calcium chloride solution, continue to be stirred to precipitation at 50 DEG C to occur, filter and obtain terra alba filter cake; The calcium sulfate filter cake obtaining adds under ethanol and hydroecium temperature and filters drip washing, or filters after the 70 DEG C of oven dry of calcium sulfate filter cake that obtain and add under ethanol and hydroecium temperature and filter drip washing; Washed calcium sulfate filter cake is dried 8 hours to obtain bouquet shape terra alba through 80 DEG C.
The above-mentioned a kind of bouquet shape terra alba thing preparing is carried out to Measurement and analysis mutually, obtain similar electron scanning micrograph as shown in Figure 2, similar X-ray powder diffraction pattern as shown in Figure 3, similar Fourier transform infrared spectroscopy figure as shown in Figure 4, similar transmission electron microscope picture as shown in Figure 5.
Embodiment 3
The deionized water of 5000mL is mixed with to Xylo-Mucine (CMC) solution of 0.5wt%, ultrasonic at 80 DEG C, stir after 0.5 hour and add equivalent concentration 0.5M calcium chloride, continue to stir 0.5 hour at 80 DEG C; Then the Potassium aluminum sulfate dodecahydrate of equivalent concentration 0.25M is stirred and is added in calcium chloride solution, continue to be stirred to precipitation at 80 DEG C to occur, filter and obtain terra alba filter cake; The calcium sulfate filter cake obtaining adds under ethanol and hydroecium temperature and filters drip washing, or filters after the 80 DEG C of oven dry of calcium sulfate filter cake that obtain and add under ethanol and hydroecium temperature and filter drip washing; Washed calcium sulfate filter cake is dried 10 hours to obtain bouquet shape terra alba through 60 DEG C.
The above-mentioned a kind of bouquet shape terra alba thing preparing is carried out to Measurement and analysis mutually, obtain similar electron scanning micrograph as shown in Figure 2, similar X-ray powder diffraction pattern as shown in Figure 3, similar Fourier transform infrared spectroscopy figure as shown in Figure 4, similar transmission electron microscope picture as shown in Figure 5.
The foregoing is only the present invention and be described further, and unrestricted the present invention, all in spiritual principles of the present invention, any amendment of making, be equal to and replace or improvement etc., all should be included in protection scope of the present invention.