CN104911688B - The preparation method of anhydrous calcium sulfate whisker - Google Patents
The preparation method of anhydrous calcium sulfate whisker Download PDFInfo
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- CN104911688B CN104911688B CN201510309296.XA CN201510309296A CN104911688B CN 104911688 B CN104911688 B CN 104911688B CN 201510309296 A CN201510309296 A CN 201510309296A CN 104911688 B CN104911688 B CN 104911688B
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- calcium sulfate
- anhydrous calcium
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Abstract
The invention belongs to whisker preparing technical field, more particularly to a kind of method that one step hydro thermal method prepares anhydrous calcium sulfate whisker, including step：A, gypsum is placed in water, is configured to the first suspension, add crystal control agent thereto under agitation, form slurry；Wherein, the solid mass ratio of the liquid of water and gypsum is 5.5~30:1；The mol ratio of crystal control agent and gypsum is 0.7~5:1；B, slurry is transferred in hydrothermal reaction kettle, under agitation hydro-thermal reaction 2h~10h, obtains the second suspension；Wherein, the setting temperature of hydrothermal reaction kettle is 170 DEG C~220 DEG C；C, by the second suspension separation of solid and liquid, filter cake and filtrate are obtained, filter cake is scrubbed, drying obtains anhydrous calcium sulfate whisker.Anhydrous calcium sulfate whisker can be prepared using one step hydro thermal method in the preparation method, and method is simple；Meanwhile the problem of purity is not high is not only avoid, the method using high temperature sintering is also avoided, reduces production cost.
Description
Technical field
The invention belongs to whisker preparing technical field, specifically, is related to a kind of one step hydro thermal method and prepares dead plaster
The method of whisker.
Background technology
Calcium sulfate crystal whiskers are also known as crystal whisker of gypsum, have high intensity, high-modulus, high tenacity, high-insulativity, abrasion performance, resistance to height
Temperature, acid and alkali-resistance, anticorrosive, infrared reflectivity are good, be easy to surface treatment, easily compound, nontoxic etc. many excellent with polymer
Wuli-Shili-Renli system approach and mechanical performance.As new function material, it is widely used in plastics, rubber, bonding agent, friction
Make strengthening and toughening agent or functional form filler in material, papermaking, pitch, coating, paint, light building material and encapsulant；Can also be straight
Connect the high insulating materials as filtering material, insulation material, fire-resistant heat insulating material, infrared light reflecting material and covered electric cable.Sulphur
Sour calcium pyroborate is the new material that a kind of application field is relatively wide, market prospects are extremely wide because its cost performance is higher, and mesh
It is preceding receive much concern in the world, extremely promising inorganic carbon sources material.
Calcium sulfate crystal whiskers can be divided into Dihydrate gypsum whiskers (CaSO according to crystallization water difference4·2H2O), half-H 2 O calcium sulphate is brilliant
Must (CaSO4·0.5H2) and anhydrous calcium sulfate whisker (CaSO O4).Wherein, anhydrous calcium sulfate whisker intensity highest；Sulfate dihydrate
Calcium pyroborate must use under conditions of less than 110 DEG C, otherwise just not have the humidification of whisker, therefore prospects for commercial application
It is small；Anhydrous calcium sulfate whisker and hemihydrate calcium sulfate crystal whisker then have higher intensity and use value.Hemihydrate calcium sulfate crystal whisker exists
Hydration reaction can occur under wet environment, destroy crystal structure and performance；Therefore, to keep its stability hemihydrate calcium sulfate crystal whisker
Need the calcination at 600 DEG C~700 DEG C to handle, generate insoluble anhydrous calcium sulfate whisker, this just causes industrial production cost
The problem of higher.
Patent CN 201210452856.3 discloses a kind of method that low cost prepares calcium sulfate crystal whiskers, methods described bag
Include procedure below：Raw material powdered whiting and anhydrite crush, by the calcium carbonate mineral after crushing and anhydrite ore sulfuric acid
After solution processing, add crystalline form growth regulator and mixed liquor is made, being generated at high temperature under high pressure through hydrothermal synthesis method has higher major diameter
The hemihydrate calcium sulfate crystal whisker of ratio, hemihydrate calcium sulfate crystal whisker is filtered, washing, high temperature take off crystallization water step to obtain high-quality anhydrous
Calcium sulfate whiskers.Though calcination at 600 DEG C~700 DEG C is not needed to handle in this technique, wherein by hemihydrate calcium sulfate crystal whisker
The high temperature at 250 DEG C~300 DEG C is still needed to during changing to anhydrous calcium sulfate whisker and takes off crystallization water operation, therefore industrial cost
It is still higher.
The content of the invention
To solve the above-mentioned problems of the prior art, the invention provides a kind of preparation side of anhydrous calcium sulfate whisker
Anhydrous calcium sulfate whisker can be prepared using one step hydro thermal method in method, the preparation method, and method is simple, simplifies anhydrous slufuric acid
The preparation technology of calcium pyroborate；Meanwhile the method using high temperature sintering is avoided, also significantly reduce production cost.
In order to reach foregoing invention purpose, present invention employs following technical scheme：
The preparation method of anhydrous calcium sulfate whisker, including step：A, gypsum is placed in water, it is suspended is configured to first
Liquid, crystal control agent is added into first suspension under agitation, form slurry；Wherein, the water and the gypsum
The solid mass ratio of liquid be 5.5~30:1；The mol ratio of the crystal control agent and the gypsum is 0.7~5:1；B, by described in
Slurry is transferred in hydrothermal reaction kettle, and carries out hydro-thermal reaction 2h~10h under agitation, obtains the second suspension；Wherein, it is described
The setting temperature of hydrothermal reaction kettle is 170 DEG C~220 DEG C；C, by the second suspension separation of solid and liquid, filter cake and filtrate are obtained,
The filter cake is scrubbed, drying obtains anhydrous calcium sulfate whisker.
Further, any one of the crystal control agent in calcium chloride, ammonium chloride, magnesium chloride, ammonium sulfate.
Further, the filtrate, which is back in the step A, is used as crystal control agent Recycling.
Further, in the step C, the filter cake washed through deionized water and at 80 DEG C drying obtain it is described
Anhydrous calcium sulfate whisker.
Further, in the step B, compactedness of the slurry in the hydrothermal reaction kettle be 50%~
80%.
Further, the hydrothermal reaction kettle is magnetic force reactor or homogeneous reactor.
The present invention has synthesized nothing using gypsum as raw material, and using the effect of crystal control agent by one step hydro thermal method
H 2 O calcium sulphate whisker, compared with the preparation method of anhydrous calcium sulfate whisker in the prior art, high-temperature process is avoided passing through by half water
The process that calcium sulfate crystal whiskers change to anhydrous calcium sulfate whisker, production cost can be greatly reduced；In addition, according to the anhydrous of the present invention
The preparation method of calcium sulfate crystal whiskers also has the advantages of technique is simple, easily operated.
Brief description of the drawings
The following description carried out in conjunction with the accompanying drawings, the characteristics of above and other aspect of embodiments of the invention and advantage
It will become clearer, in accompanying drawing：
Fig. 1 is the step flow chart of the preparation method of 1 anhydrous calcium sulfate whisker according to an embodiment of the invention；
Fig. 2 is the XRD of 1 anhydrous calcium sulfate whisker according to an embodiment of the invention；
Fig. 3 is the SEM figures of 1 anhydrous calcium sulfate whisker according to an embodiment of the invention；
Fig. 4 is the XRD of 4 anhydrous calcium sulfate whisker according to an embodiment of the invention；
Fig. 5 is the SEM figures of 4 anhydrous calcium sulfate whisker according to an embodiment of the invention；
Fig. 6 is the XRD of 7 anhydrous calcium sulfate whisker according to an embodiment of the invention；
Fig. 7 is the SEM figures of 7 anhydrous calcium sulfate whisker according to an embodiment of the invention；
Fig. 8 is the XRD of 8 anhydrous calcium sulfate whisker according to an embodiment of the invention；
Fig. 9 is the SEM figures of 8 anhydrous calcium sulfate whisker according to an embodiment of the invention.
Embodiment
Hereinafter, with reference to the accompanying drawings to embodiments of the invention are described in detail.However, it is possible to come in many different forms real
Apply the present invention, and the specific embodiment of the invention that should not be construed as limited to illustrate here.Conversely, there is provided these implementations
Example is in order to explain the principle and its practical application of the present invention, so that others skilled in the art are it will be appreciated that the present invention
Various embodiments and be suitable for the various modifications of specific intended application.
It will be appreciated that although term " first ", " second " etc. can be used to describe various intermediate products herein, still
These intermediate products should not be limited by these terms, these terms be only used for by one intermediate products of chemical classes identical with
Another intermediate products makes a distinction.
Fig. 1 is the step flow chart of the preparation method of anhydrous calcium sulfate whisker according to an embodiment of the invention.
Reference picture 1, the preparation method of anhydrous calcium sulfate whisker according to an embodiment of the invention comprise the following steps：
In step 110, gypsum is placed in water, forms the first suspension.Wherein, the liquid stereoplasm amount of water and gypsum
Than for 5.5~30:1.
In the step 120, crystal control agent is added into the first suspension, stirring forms white slurry.
Specifically, the mol ratio of crystal control agent and gypsum is 0.7~5:1；Wherein, crystal control agent may be selected from chlorination
Any one in calcium, ammonium chloride, magnesium chloride, ammonium sulfate.
In step 130, white slurry is moved in hydrothermal reaction kettle, allows white slurry to carry out hydro-thermal reaction, obtain the
Two suspensions.
Specifically, the setting temperature of hydrothermal reaction kettle is 170 DEG C~220 DEG C, and the hydro-thermal reaction time is 2h~10h.
What deserves to be explained is above-mentioned hydro-thermal reaction should be carried out in the case of stirring, the equipment that hydro-thermal reaction uses can be with
It is homogeneous reactor or magnetic force reactor, or other equipment that can realize the hydro-thermal reaction under stirring condition simultaneously.
In step 140, by the second suspension separation of solid and liquid, filter cake and filtrate are obtained, filter cake after deionized water is washed,
Drying obtains anhydrous calcium sulfate whisker at 80 DEG C.
What deserves to be explained is in step 140, the filtrate obtained through separation of solid and liquid can be recycled for use as crystal control agent；
That is only gypsum need to be added according to predetermined ratio into the filtrate, it is agitated, you can white slurry to be formed, so as to continue
Carry out hydro-thermal reaction；Or by the filtrate return to step 110, mixed with the first suspension, it is agitated, you can to form stock white
Material, so as to continue hydro-thermal reaction.
Hereinafter, the preparation method of the anhydrous calcium sulfate whisker according to the present invention will be carried out with reference to specific embodiment detailed
Description, contrasted for convenience of to the experiment parameter of each embodiment, analysis in table form contrasts each embodiment；Embodiment
Comparing result in 1-9 under different experiments parameter is as shown in table 1.
Table 1 according to an embodiment of the invention 1-9 experiment parameter contrast
In table 1, " mol ratio " refers to the ratio between amount of material of crystal control agent and gypsum.
Wherein, the hydrothermal reaction kettle used in embodiment 1,2,4,5,6,7,8,9 refers to homogeneous reactor (model：JXF-
8-200, producer：Yantai Pine Ridge Chemical Equipment Co., Ltd.), wherein, the liner volume of the reactor in homogeneous reactor is
100mL, the kettle rotary speed of reactor is 28r/min, but the present invention this is not particularly limited, usually, use this set
When standby, it is 14r/min~28r/min to control kettle rotating speed；The hydrothermal reaction kettle used in embodiment 3 is magnetic force reactor
(model：GSH-2/20, producer：Weihai Yuan Cheng Chemical Equipment Co., Ltd.s), wherein, the volume of magnetic force reactor is 2L, in it
Portion's rotating speed of agitator is 600r/min, but the present invention is also not particularly limited to this, usually, during using the equipment, in control
The mixing speed of portion's agitating paddle is 200r/min~600r/min.
In above-described embodiment 1-9, in step 130, the compactedness of white slurry is 50%~80% or so, general feelings
Under condition, controlling can be such that above-mentioned hydro-thermal reaction preferably carries out in the range of the compactedness.
The anhydrous calcium sulfate whisker product that above-described embodiment 1-9 is prepared is determined, the measurement result such as institute of table 2
Show.
The measurement result of the anhydrous calcium sulfate whisker that 1-9 is prepared according to an embodiment of the invention of table 2
| Pattern | Length/μm | Diameter/μm | |
| Embodiment 1 | Threadiness | 40~60 | 0.5~1.5 |
| Embodiment 2 | Threadiness | 40~100 | 0.5~1.0 |
| Embodiment 3 | Threadiness | 30~90 | 0.5~1.0 |
| Embodiment 4 | Threadiness | 30~60 | 0.5~3.0 |
| Embodiment 5 | Threadiness | 20~40 | 0.5~3.0 |
| Embodiment 6 | Threadiness | 30~50 | 0.5~2.0 |
| Embodiment 7 | Threadiness | 20~40 | 0.5~2.0 |
| Embodiment 8 | Threadiness | 20~30 | 1.0~2.0 |
| Embodiment 9 | Threadiness | 40~60 | 0.5~2.0 |
Wherein, SEM (ESEM) characterization result difference for the anhydrous calcium sulfate whisker product that embodiment 1,4,7,8 obtains
As shown in Fig. 3, Fig. 5, Fig. 7 and Fig. 9；And (X ray spreads out the XRD for the anhydrous calcium sulfate whisker product that embodiment 1,4,7,8 obtains
Penetrate) characterization result is respectively as shown in Fig. 2, Fig. 4, Fig. 6 and Fig. 8.
It is worth noting that, in the prior art, with gypsum (CaSO4·2H2O it is) raw material, is prepared by hydro-thermal method
The principle of hemihydrate calcium sulfate crystal whisker, it is considered that be dissolution-crystallization mechanism.First, crystal control agent is by controlling CaSO4·
2H2O and CaSO4·0.5H2O solubility, so as to result in the difference of system degree of supersaturation；Second, hemihydrate calcium sulfate crystal whisker is
Hexagonal crystal system, crystal control agent are adsorbed in CaSO4·0.5H2On O different crystal faces, it is promoted to carry out one-dimensional growth, so as to generate
CaSO4·0.5H2O whiskers.
In the preparation method of anhydrous calcium sulfate whisker according to an embodiment of the invention, with gypsum (CaSO4·2H2O)
For raw material, anhydrous calcium sulfate whisker is prepared by hydro-thermal method, its process with above-mentioned there is larger difference.Specifically,
On the one hand, in an embodiment according to the present invention, crystal control agent is to CaSO4·2H2O and CaSO4Solubility impact,
The difference of the system degree of supersaturation is result in, so as to CaSO4Pattern be controlled by, obtain anhydrous calcium sulfate whisker；Ability
Field technique personnel will be appreciated that in the mixed system that many kinds of substance coexists, due to common-ion effect be present and effect of saltouing
The influence of effect should be waited, influence of the same material to the solubility of other materials is different, and at different temperatures, is also in
Existing complex effects；On the other hand, anhydrous calcium sulfate whisker is orthorhombic system, and anhydrous calcium sulfate whisker is being prepared by gypsum hydro-thermal
During, the crystal control agent in system is adsorbed in CaSO4Different crystal faces on, control the speed of growth of different crystal faces to occur
Difference, so as to promote its one-dimensional growth, then form anhydrous calcium sulfate whisker.Those skilled in the art also will be appreciated that
When same crystal control agent coexists from the material in different crystallographic systems, it is in CaSO4·0.5H2O and CaSO4Surface
Suction type is different, and absorption crystal face is different, therefore crystal face growth course caused by it is also by difference.Therefore, using gypsum as original
Material, anhydrous calcium sulfate whisker is prepared with hemihydrate calcium sulfate crystal whisker as two entirely different processes using hydro-thermal method；And continue with half
H 2 O calcium sulphate whisker prepares anhydrous calcium sulfate whisker, then needs high-temperature process, and energy expenditure is larger, will greatly improve production cost.
In the prior art, the preparation of anhydrous calcium sulfate whisker typically uses gypsum-hemihydrate calcium sulfate crystal whisker-anhydrous sulphur
The preparation path of sour calcium pyroborate, that is to say, that using gypsum as raw material, hemihydrate calcium sulfate crystal whisker is prepared through hydro-thermal method, so
High-temperature process is carried out to hemihydrate calcium sulfate crystal whisker afterwards, obtains anhydrous calcium sulfate whisker；The shortcomings that this method, is mainly by following two side
Face, one is obtained hemihydrate calcium sulfate crystal whisker degree of hydration during washing greatly improves, the diameter of part whisker becomes
Slightly, the calcium sulphate dihydrate of sheet is generated, then after follow-up high-temperature process, influences the purity of anhydrous calcium sulfate whisker；Secondly
It is that energy expenditure is larger during prepared by hemihydrate calcium sulfate crystal whisker high-temperature process into anhydrous calcium sulfate whisker, this will cause
Cost greatly improves.
Ground is corresponded, equally takes hydro-thermal method to make according to the preparation method of the anhydrous calcium sulfate whisker of the present invention
It is standby, but without the pilot process of hemihydrate calcium sulfate crystal whisker, but anhydrous calcium sulfate whisker has been prepared in one step hydro thermal method
Product, so as to effectively avoid intermediate products hemihydrate calcium sulfate crystal whisker because of influence of the aquation to anhydrous calcium sulfate whisker purity, separately
Outside, can also high-temperature calcination be avoided to handle, so as to significantly reduce production cost.
Although the present invention has shown and described with reference to specific embodiment, it should be appreciated by those skilled in the art that：
In the case where not departing from the spirit and scope of the present invention limited by claim and its equivalent, can carry out herein form and
Various change in details.
Claims (5)
1. a kind of preparation method of anhydrous calcium sulfate whisker, it is characterised in that including step：
A, gypsum is placed in water, is configured to the first suspension, add crystalline form control into first suspension under agitation
Preparation, form slurry；Wherein, the solid mass ratio of liquid of the water and the gypsum is 5.5~30:1；The crystal control agent with
The mol ratio of the gypsum is 0.7~5:1；The crystal control agent is in calcium chloride, ammonium chloride, magnesium chloride, ammonium sulfate
Any one；
B, the slurry is transferred in hydrothermal reaction kettle, and carries out hydro-thermal reaction 2h~10h under agitation, it is suspended to obtain second
Liquid；Wherein, the setting temperature of the hydrothermal reaction kettle is 200 DEG C~220 DEG C；
C, second suspension is subjected to separation of solid and liquid, obtains filter cake and filtrate, the filter cake is scrubbed, drying obtain it is anhydrous
Calcium sulfate crystal whiskers.
2. preparation method according to claim 1, it is characterised in that the filtrate is back in the step A as crystalline substance
Shape controlling agent Recycling.
3. preparation method according to claim 1, it is characterised in that in the step C, the filter cake is through deionized water
Wash and drying obtains the anhydrous calcium sulfate whisker at 80 DEG C.
4. preparation method according to claim 1, it is characterised in that in the step B, the slurry is in the hydro-thermal
Compactedness in reactor is 50%~80%.
5. preparation method according to claim 1, it is characterised in that the hydrothermal reaction kettle is magnetic force reactor or homogeneous
Reactor.
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| CN105401219B (en) * | 2015-12-31 | 2018-03-20 | 中国科学院青海盐湖研究所 | A kind of method that normal pressure acidization prepares anhydrous calcium sulfate whisker |
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| CN108893774A (en) * | 2018-07-27 | 2018-11-27 | 湖北工业大学 | A kind of preparation method of metal salt hydrotropy hydrothermal synthesis calcium sulfate crystal whiskers |
| CN110205679A (en) * | 2019-06-25 | 2019-09-06 | 湖南迈辉环保材料有限公司 | The manufacturing method of wgrg high strength crystal whisker gypsum |
| CN111607827B (en) * | 2019-07-16 | 2022-01-07 | 北新集团建材股份有限公司 | Post-treatment method of calcium sulfate whisker |
| CN111118606B (en) * | 2019-12-31 | 2021-12-21 | 浙江环耀环境建设有限公司 | Method for preparing calcium sulfate whiskers by using bone gelatin wastewater |
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