CN104562209A - Preparation method of alpha-calcium sulfate hemihydrate crystal whisker by one-step autocatalysis and application thereof - Google Patents

Preparation method of alpha-calcium sulfate hemihydrate crystal whisker by one-step autocatalysis and application thereof Download PDF

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Publication number
CN104562209A
CN104562209A CN201410755484.0A CN201410755484A CN104562209A CN 104562209 A CN104562209 A CN 104562209A CN 201410755484 A CN201410755484 A CN 201410755484A CN 104562209 A CN104562209 A CN 104562209A
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calcium sulfate
crystal whisker
sulfate crystal
autocatalysis
solution
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于翔
王延伟
迟长龙
田银彩
杨柳
魏媛
辛长征
李思雨
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Henan Institute of Engineering
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    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
    • C30B29/62—Whiskers or needles
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10—Inorganic compounds or compositions
    • C30B29/46—Sulfur-, selenium- or tellurium-containing compounds
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
    • C30B7/14—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions the crystallising materials being formed by chemical reactions in the solution

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)

Abstract

The invention provides a preparation method of an alpha-calcium sulfate hemihydrate crystal whisker by one-step autocatalysis, belonging to the field of materials. The method comprises the following steps: reacting calcium chloride and anhydrous sodium sulfate to obtain calcium sulfate dihydrate; and by using the byproduct sodium chloride in the reaction as a catalyst (crystal transforming agent) to accelerate the next reaction, carrying out normal-temperature hydrothermal reaction under the condition of high-speed stirring under the action of sodium chloride to remove 1.5-molecule crystalline water, thereby obtaining the alpha-calcium sulfate hemihydrate crystal whisker. The alpha-calcium sulfate hemihydrate crystal whisker has uniform particle size. The reaction process is an autocatalysis process without adding any additional crystal transforming agent, thereby effectively solving the problems of complex reaction system, higher cost and difficulty in operation in the alpha-calcium sulfate hemihydrate crystal whisker production process. The method is convenient for production and application, has the characteristics of low vacuum, low energy consumption and low pollution, conforms to the material synthesis requirements by the soft processing mode, and has wide application prospects.

Description

The preparation method of one step autocatalysis α-hemihydrate calcium sulfate crystal whisker and application
Technical field
The invention belongs to field of material technology, be specifically related to a kind of preparation method and application thereof of a step autocatalysis α-hemihydrate calcium sulfate crystal whisker.
Background technology
The crystalline fibers of α-hemihydrate calcium sulfate crystal whisker to be a kind of single crystal of needle-like be a kind of perfect condition, length-to-diameter ratio is larger, its atomic arrangement high-sequential during crystallization, hardly containing defect (crystal boundary, dislocation, hole etc.) existing in usual material, its physical strength equals to face and connects valence f., therefore, the physical strength of α-hemihydrate calcium sulfate crystal whisker and modulus are close to the theoretical value of perfect crystal material, and its mechanical property is far above other chopped strand and particulate filler.Based on the performance that these are excellent, α-hemihydrate calcium sulfate crystal whisker is often used in enhancing, the friction field such as fire retardant material, environmental engineering of matrix material.
At present, the common method preparing α-hemihydrate calcium sulfate crystal whisker mainly contains following three kinds: pressurized thermal water method, autoclave method, normal pressure salt solustion mehtod.Pressurized thermal water method refers to terra alba to be raw material, high pressure autoclave method is adopted to prepare α-hemihydrate calcium sulfate crystal whisker (No. 201110123932.1st, Chinese invention patent application), whisker length-to-diameter ratio prepared by this method is larger, but this method reaction times is long, if put into production, the production cycle is longer.Autoclave method adopts terra alba to be raw material, α-hemihydrate calcium sulfate crystal whisker (No. 200610029067.3rd, Chinese invention patent application) is prepared as reaction vessel with autoclave, but the shortcoming that this method exists needs reactor, equipment is comparatively complicated, and production cost is too high, be not suitable for scale operation.Normal pressure salt solustion mehtod is a kind of most widely used method preparing α-hemihydrate calcium sulfate crystal whisker now, it take terra alba as raw material, crystal modifier is added in reaction process, the water being sloughed 1.5 molecules by hydro-thermal reaction method terra alba under the effect of crystal modifier generates α-hemihydrate calcium sulfate crystal whisker (No. 03142607.7th, Chinese invention patent application), the advantage of this method is that reaction carries out at ambient pressure, reaction conditions is gentleer, but this method also also exists certain shortcoming, need before reaction to prepare terra alba raw material in advance, extend the production cycle, in addition, reaction process needs to add extra crystal modifier, add production cost, be unfavorable for industrialized production.
Summary of the invention
Technical problem to be solved by this invention prepares α-hemihydrate calcium sulfate crystal whisker for traditional method to need to add extra crystal modifier, in preparation process, system is complicated, the problem that cost is higher, provides a kind of preparation method and application of a step autocatalysis α-hemihydrate calcium sulfate crystal whisker, directly with CaCl 2and Na 2sO 4for raw material, utilizing the by product in reaction to be crystal modifier, without the need to adding extra crystal modifier, greatly reducing production cost, the α obtained-hemihydrate calcium sulfate crystal whisker size uniform.
For solving the problems of the technologies described above, the present invention by the following technical solutions:
A preparation method for one step autocatalysis α-hemihydrate calcium sulfate crystal whisker, step is as follows:
(1) by CaCl 2and Na 2sO 4be dissolved in respectively in deionized water, obtain the CaCl that concentration is 1 ~ 5mol/L 2solution and concentration are the Na of 1 ~ 3mol/L 2sO 4solution;
(2) by Na 2sO 4solution joins in reaction vessel, dropwise by CaCl under churned mechanically condition 2solution is added drop-wise in reaction vessel, after dropping completely, and mechanical stirring 25 ~ 35min, wherein Na 2sO 4with CaCl 2the ratio of amount of substance be 1:1 ~ 3:1;
(3) in reaction vessel, drip acid solution, the PH controlling solution is 4 ~ 6, then raised temperature to 100 ~ 110 DEG C, mechanic whirl-nett reaction 4 ~ 8h;
(4) after reaction terminates, filter, washing, is drying to obtain α-hemihydrate calcium sulfate crystal whisker.
CaCl in described step (2) 2drop rate be 5 ~ 10mL/min.
Acid solution in described step (3) is acetum or dilute hydrochloric acid solution.
In described step (2) and step (3), churned mechanically speed is 800 ~ 1800rpm.
Drying temperature in described step (4) is 80 ~ 105 DEG C, and time of drying is 4 ~ 8h.
The described application of α-hemihydrate calcium sulfate crystal whisker in matrix material enhancing.
Beneficial effect of the present invention: (1) present method is directly with CaCl 2and Na 2sO 4for raw material, obtain terra alba, the generation that side product chlorinated sodium in reaction will promote next step to react as catalyzer (crystal modifier), without the need to adding extra crystal modifier, greatly reduce production cost, the crystal water sloughing 1.5 molecules by normal-temperature water thermal response method under the effect of sodium-chlor under the condition of high-speed stirring can obtain α-hemihydrate calcium sulfate crystal whisker, the α obtained-hemihydrate calcium sulfate crystal whisker size uniform; (2) the method effectively solves system complexity in the preparation process of α-hemihydrate calcium sulfate crystal whisker, the problem that cost is higher, is specially adapted to matrix material and strengthens and macromolecular material filling flame retardant area; (3) the method production cycle is shorter, is conducive to suitability for industrialized production, and application prospect is comparatively wide; (4) reaction is carried out at ambient pressure, and mild condition, environmental protection, operates easy to implement, for suitability for industrialized production and application provide good technical support.
figure of description
Fig. 1 is α-hemihydrate calcium sulfate crystal whisker XRD spectra prepared by the embodiment of the present invention 1 one step autocatalytic method.
Fig. 2 is α-hemihydrate calcium sulfate crystal whisker SEM image prepared by the embodiment of the present invention 1 one step autocatalytic method.
Embodiment
Embodiment 1
The preparation method of the one step autocatalysis α-hemihydrate calcium sulfate crystal whisker of the present embodiment, step is as follows:
Weigh 27.5g CaCl 2(0.25mol) be dissolved in 100mL deionized water, be mixed with the CaCl of 2.5mol/L 2solution, weighs 35.5g Na 2sO 4(0.25mol) be dissolved in 200mL deionized water, be mixed with the Na of 1.25mol/L 2sO 4then two kinds of solution are filtered by solution respectively.
By above-mentioned Na 2sO 4pour in there-necked flask, mechanical stirring, then with the speed of 5mL/min by CaCl 2join in there-necked flask, treat CaCl 2after solution drips completely, continue to stir 0.5h.Then by solution warms to 104 DEG C, mechanical stirring speed is 1500rpm, keeps the temperature of churned mechanically speed and solution to continue reaction 4h.After reacting completely, reacting liquor while hot is filtered, then carries out washing 5 times with 100 DEG C of hot water, then use washing with alcohol three times.The product obtained after reaction is obtained α-hemihydrate calcium sulfate crystal whisker as dry 6h in 80 DEG C of baking ovens, sieves, preserve.
α-hemihydrate calcium sulfate crystal whisker embodiment 1 obtained carries out XRD scanning, and the α-hemihydrate calcium sulfate crystal whisker taken a morsel carries out SEM observation, as depicted in figs. 1 and 2.XRD result shows, the position consistency at the crystal formation of the α-hemihydrate calcium sulfate crystal whisker obtained and the peak of standard spectrogram.SEM result shows, and α-hemihydrate calcium sulfate crystal whisker particle diameter is comparatively even.
Embodiment 2
The preparation method of the one step autocatalysis α-hemihydrate calcium sulfate crystal whisker of the present embodiment, step is as follows:
Weigh 55.0g CaCl 2(0.5mol) be dissolved in 200mL deionized water, be mixed with the CaCl of 2.5mol/L 2solution, weighs 35.5g Na 2sO 4(0.25mol) be dissolved in 200mL deionized water, be mixed with the Na of 1.25mol/L 2sO 4then two kinds of solution are filtered by solution respectively;
By above-mentioned Na 2sO 4pour in there-necked flask, mechanical stirring, then with the speed of 10mL/min by CaCl 2join in there-necked flask, treat CaCl 2after solution drips completely, continue to stir 0.5h.Then by solution warms to 104 DEG C, mechanical stirring speed is 1800rpm, keeps the temperature of churned mechanically speed and solution to continue reaction 4h.After reacting completely, reacting liquor while hot is filtered, then carries out washing 5 times with 100 DEG C of hot water, then use washing with alcohol three times.The product obtained after reaction is obtained α-hemihydrate calcium sulfate crystal whisker as dry 4h in 100 DEG C of baking ovens, sieves, preserve.
Embodiment 3
The preparation method of the one step autocatalysis α-hemihydrate calcium sulfate crystal whisker of the present embodiment, step is as follows:
Weigh 27.5g CaCl 2(0.25mol) be dissolved in 100mL deionized water, be mixed with the CaCl of 2.5mol/L 2solution, weighs 35.5g Na 2sO 4(0.25mol) be dissolved in 200mL deionized water, be mixed with the Na of 1.25mol/L 2sO 4then two kinds of solution are filtered by solution respectively;
By above-mentioned Na 2sO 4pour in there-necked flask, mechanical stirring, then with the speed of 5mL/min by CaCl 2join in there-necked flask, treat CaCl 2after solution drips completely, continue to stir 0.5h.Then by solution warms to 104 DEG C, mechanical stirring speed is 800rpm, keeps the temperature of churned mechanically speed and solution to continue reaction 8h.After reacting completely, reacting liquor while hot is filtered, then carries out washing 5 times with 100 DEG C of hot water, then use washing with alcohol three times.The product obtained after reaction is obtained α-hemihydrate calcium sulfate crystal whisker as dry 4h in 100 DEG C of baking ovens, sieves, preserve.
Embodiment 4
The preparation method of the one step autocatalysis α-hemihydrate calcium sulfate crystal whisker of the present embodiment, step is as follows:
(1) by 110gCaCl 2(1mol) be dissolved in 1000mL deionized water and obtain the CaCl that concentration is 1mol/L 2solution, by 142gNa 2sO 4(1mol) be dissolved in 1000mL deionized water and obtain the Na that concentration is 1mol/L 2sO 4solution;
(2) by Na 2sO 4solution joins in reaction vessel, dropwise by CaCl under rotating speed is the churned mechanically condition of 800rpm 2solution is added drop-wise in reaction vessel, CaCl 2drop rate be 5mL/min, after dropping completely, mechanical stirring 25min;
(3) in reaction vessel, drip acetum, the PH controlling solution is 4, and then raised temperature to 100 DEG C is under the condition of 800rpm in speed, mechanic whirl-nett reaction 8h;
(4) after reaction terminates, filter, washing, under the condition of 80 DEG C, namely dry 8h obtains α-hemihydrate calcium sulfate crystal whisker.
Embodiment 5
The preparation method of the one step autocatalysis α-hemihydrate calcium sulfate crystal whisker of the present embodiment, step is as follows:
(1) by 165gCaCl 2(1.5mol) be dissolved in 300mL deionized water and obtain the CaCl that concentration is 5mol/L 2solution, by 71gNa 2sO 4(0.5mol) be dissolved in 166.67mL deionized water and obtain the Na that concentration is 3mol/L 2sO 4solution;
(2) by Na 2sO 4solution joins in reaction vessel, dropwise by CaCl under rotating speed is the churned mechanically condition of 1800rpm 2solution is added drop-wise in reaction vessel, CaCl 2drop rate be 10mL/min, after dropping completely, mechanical stirring 35min;
(3) in reaction vessel, drip dilute hydrochloric acid solution, the PH controlling solution is 6, and then raised temperature to 110 DEG C is under the condition of 1800rpm in speed, mechanic whirl-nett reaction 4h;
(4) after reaction terminates, filter, washing, under the condition of 105 DEG C, namely dry 4h obtains α-hemihydrate calcium sulfate crystal whisker.
Embodiment 6
The preparation method of the one step autocatalysis α-hemihydrate calcium sulfate crystal whisker of the present embodiment, step is as follows:
(1) 55.0g CaCl 2(0.5mol) be dissolved in 200mL deionized water, be mixed with the CaCl of 2.5mol/L 2solution, weighs 35.5g Na 2sO 4(0.25mol) be dissolved in 125mL deionized water, be mixed with the Na of 2mol/L 2sO 4solution;
(2) by Na 2sO 4solution joins in reaction vessel, dropwise by CaCl under rotating speed is the churned mechanically condition of 1000rpm 2solution is added drop-wise in reaction vessel, CaCl 2drop rate be 6mL/min, after dropping completely, mechanical stirring 30min;
(3) in reaction vessel, drip dilute hydrochloric acid solution, the PH controlling solution is 5, and then raised temperature to 105 DEG C is under the condition of 1000rpm in speed, mechanic whirl-nett reaction 5h;
(4) after reaction terminates, filter, washing, under the condition of 90 DEG C, namely dry 5h obtains α-hemihydrate calcium sulfate crystal whisker.
The application of α-hemihydrate calcium sulfate crystal whisker in matrix material enhancing:
By embodiment 1 ~ 6 prepare α-hemihydrate calcium sulfate crystal whisker with 1% ratio and polypropylene (PP) carry out melt blending with twin screw extruder, the testing bar universal tensile machine then carrying out being injection molded into dumbbell shape carries out tension test.Carry out tension test test with virgin pp (PP), result is as shown in table 1.
Add the polypropylene tensile strength test chart of 1% α-hemihydrate calcium sulfate crystal whisker
Result shows, the tensile strength of pure PP is 25.5MPa, after adding the α-hemihydrate calcium sulfate crystal whisker of 1%, the tensile strength of PP can reach 44.6MPa, and the intensity of PP adds 74.9%, and it is quite significant for describing α-hemihydrate calcium sulfate crystal whisker for the reinforced effects of polymkeric substance.

Claims (6)

1. a preparation method for a step autocatalysis α-hemihydrate calcium sulfate crystal whisker, is characterized in that step is as follows: (1) is by CaCl 2and Na 2sO 4be dissolved in respectively in deionized water, obtain the CaCl that concentration is 1 ~ 5mol/L 2solution and concentration are the Na of 1 ~ 3mol/L 2sO 4solution;
(2) by Na 2sO 4solution joins in reaction vessel, dropwise by CaCl under churned mechanically condition 2solution is added drop-wise in reaction vessel, after dropping completely, and mechanical stirring 25 ~ 35min, wherein Na 2sO 4with CaCl 2the ratio of amount of substance be 1:1 ~ 3:1;
(3) in reaction vessel, drip acid solution, the PH controlling solution is 4 ~ 6, then raised temperature to 100 ~ 110 DEG C, mechanic whirl-nett reaction 4 ~ 8h;
(4) after reaction terminates, filter, washing, is drying to obtain α-hemihydrate calcium sulfate crystal whisker.
2. the preparation method of a step autocatalysis α-hemihydrate calcium sulfate crystal whisker according to claim 1, is characterized in that: CaCl in described step (2) 2drop rate be 5 ~ 10mL/min.
3. the preparation method of a step autocatalysis α-hemihydrate calcium sulfate crystal whisker according to claim 1, is characterized in that: the acid solution in described step (3) is acetum or dilute hydrochloric acid solution.
4. the preparation method of a step autocatalysis α-hemihydrate calcium sulfate crystal whisker according to claim 1, is characterized in that: in described step (2) and step (3), churned mechanically speed is 800 ~ 1800rpm.
5. the preparation method of a step autocatalysis α-hemihydrate calcium sulfate crystal whisker according to claim 1, it is characterized in that: the drying temperature in described step (4) is 80 ~ 105 DEG C, time of drying is 4 ~ 8h.
6. the application of α-hemihydrate calcium sulfate crystal whisker according to claim 1 in matrix material enhancing.
CN201410755484.0A 2014-12-11 2014-12-11 Preparation method of alpha-calcium sulfate hemihydrate crystal whisker by one-step autocatalysis and application thereof Pending CN104562209A (en)

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CN105293557A (en) * 2015-12-07 2016-02-03 杭州易泰环保有限公司 Method for preparing and separating monodisperse nano alpha-calcium sulfate hemihydrate
CN112342624A (en) * 2020-10-26 2021-02-09 西华大学 Preparation method of alpha calcium sulfate hemihydrate crystal whisker
CN114436309A (en) * 2022-01-28 2022-05-06 山东祥生新材料科技股份有限公司 Production process of calcium sulfate dihydrate for producing alpha-type high-strength gypsum

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CN105293557A (en) * 2015-12-07 2016-02-03 杭州易泰环保有限公司 Method for preparing and separating monodisperse nano alpha-calcium sulfate hemihydrate
CN105293557B (en) * 2015-12-07 2017-05-17 杭州易泰环保有限公司 Method for preparing and separating monodisperse nano alpha-calcium sulfate hemihydrate
CN112342624A (en) * 2020-10-26 2021-02-09 西华大学 Preparation method of alpha calcium sulfate hemihydrate crystal whisker
CN112342624B (en) * 2020-10-26 2021-08-10 西华大学 Preparation method of alpha calcium sulfate hemihydrate crystal whisker
CN114436309A (en) * 2022-01-28 2022-05-06 山东祥生新材料科技股份有限公司 Production process of calcium sulfate dihydrate for producing alpha-type high-strength gypsum

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