CN105401219A - Normal pressure acidification method for preparing anhydrous calcium sulfate whiskers - Google Patents
Normal pressure acidification method for preparing anhydrous calcium sulfate whiskers Download PDFInfo
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- CN105401219A CN105401219A CN201511028199.XA CN201511028199A CN105401219A CN 105401219 A CN105401219 A CN 105401219A CN 201511028199 A CN201511028199 A CN 201511028199A CN 105401219 A CN105401219 A CN 105401219A
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- Prior art keywords
- calcium sulfate
- anhydrous calcium
- hydrochloric acid
- normal pressure
- sulfate whisker
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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
- C30B29/10—Inorganic compounds or compositions
- C30B29/46—Sulfur-, selenium- or tellurium-containing compounds
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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
- 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 normal pressure acidification method for preparing anhydrous calcium sulfate whiskers. The method comprises the following steps: mixing concentrated hydrochloric acid and CaSO4.2H2O according to a liquid-solid ratio of 5 to 20 so as to obtain slurry; subjecting the slurry to a stirring reaction in a water bath with a constant temperature of 60 to 100 DEG C so as to obtain turbid liquid; and subjecting the turbid liquid to solid-liquid separation so as to obtain a filter cake and filtrate and drying the filter cake so as to obtain the anhydrous calcium sulfate whiskers. According to the invention, the highly concentrated hydrochloric acid is used as a medium; the process of calcination is not needed; and the anhydrous calcium sulfate whiskers can be directly synthesized by using the normal pressure acidification method, so the problem of hydration of the calcium sulfate whiskers is overcome, preparation links are reduced, and preparation cost for the whiskers is lowered.
Description
Technical field
The present invention relates to crystal preparing technology field, especially a kind of normal pressure acidization prepares the method for anhydrous calcium sulfate whisker.
Background technology
Calcium sulfate crystal whiskers is also known as crystal whisker of gypsum, be a kind of monocrystalline staple fibre of excellent performance, there is high strength, high-modulus, high tenacity, high-insulativity, abrasion performance, high temperature resistant, acid and alkali-resistance, anticorrosive, infrared reflectivity good, be easy to surface treatment, easily and polymkeric substance compound, the Wuli-Shili-Renli system approach of many excellences such as nontoxic and mechanical property.It integrates fortifying fibre and the advantage both ultra-fine inorganic filler, is widely used in plastics, rubber, caking agent, friction materials, papermaking, pitch, coating, paint, light building material and sealing material and makes strengthening and toughening agent or functional type filler; Again can directly as the high insulating material of filtering material, lagging material, fire-resistant heat insulating material, infrared light reflecting material and covered electric cable.Calcium sulfate crystal whiskers is higher due to its cost performance, is the type material that a kind of Application Areas is comparatively wide, market outlook are very wide, be also receive much concern in the world at present, extremely rising inorganic carbon sources material.
Calcium sulfate crystal whiskers comprises two water, Ban Shui, anhydrous calcium sulfate whisker three kinds, and wherein Dihydrate gypsum whiskers dehydration temperaturre is lower, mechanical property is poor, and prospects for commercial application is little; Can hydration reaction be there is after hemihydrate calcium sulfate crystal whisker contacts with water, cause the destruction of its crystalline structure and performance.With regard to preparation link, the existing technology of preparing of hemihydrate calcium sulfate crystal whisker is the most ripe, and researchist has carried out a large amount of work for the stability of calcium sulfate crystal whiskers.Research finds that the basic reason of calcium sulfate crystal whiskers aquation is that whisker internal gutter and surfactivity point exist calcium ion and surface hydroxyl, attracts water molecules to enter the gap of lattice, impels calcium sulphate hemihydrate to change terra alba into.Adopt the stablizers such as sodium phosphate, sodium oleate, sodium stearate, Trisodium Citrate, reduce the extent of hydration of hemihydrate calcium sulfate crystal whisker to a certain extent, but internal crystal framework duct cannot be eliminated, aquation is inevitable; And anhydrous dead roasting calcium sulfate crystal whiskers needs first to prepare hemihydrate calcium sulfate crystal whisker, then in the high-temperature calcination of 600-700 degree, complex steps and the problem causing production cost too high.
Summary of the invention
For overcoming the deficiencies in the prior art, the invention provides a kind of method that normal pressure acidization prepares anhydrous calcium sulfate whisker, comprising the steps:
By concentrated acid and CaSO
42H
2o is 5 ~ 20 be mixed to form slip according to liquid-solid ratio;
By described slip stirring reaction 1 ~ 6h in the water bath with thermostatic control of 60 ~ 100 DEG C, obtain suspension liquid;
Described suspension liquid is carried out solid-liquid separation and obtain filter cake and filtrate, described filter cake obtains described anhydrous calcium sulfate whisker after drying.
Wherein, described concentrated acid is the one in the vitriol oil, concentrated nitric acid, concentrated hydrochloric acid, strong phosphoric acid.
Wherein, when adopting concentrated acid to be concentrated hydrochloric acid, the concentration of concentrated hydrochloric acid is 6.50mol/L ~ 10.83mol/L.
Wherein, described filtrate backflow Posterior circle utilizes, and replaces described concentrated hydrochloric acid and described CaSO
42H
2o mixes.
Beneficial effect:
The object of this invention is to provide a kind of preparation method of a step normal pressure acidization synthesis anhydrous calcium sulfate whisker.Take concentrated hydrochloric acid as medium in preparation process of the present invention, do not need calcination process, directly by normal pressure acidization synthesis anhydrous calcium sulfate whisker, both can solve the aquation problem of calcium sulfate crystal whiskers, and preparation link can have been reduced simultaneously, and reduced the preparation cost of whisker.
Accompanying drawing explanation
Fig. 1 is X-ray diffraction (XRD) figure of embodiment 1 gained anhydrous calcium sulfate whisker.
Fig. 2 is the scanning electron microscope (SEM) photograph of embodiment 1 gained anhydrous calcium sulfate whisker.
Fig. 3 is X-ray diffraction (XRD) figure of embodiment 2 gained anhydrous calcium sulfate whisker.
Fig. 4 is the scanning electron microscope (SEM) photograph of embodiment 2 gained anhydrous calcium sulfate whisker.
Fig. 5 is X-ray diffraction (XRD) figure of embodiment 3 gained anhydrous calcium sulfate whisker.
Fig. 6 is the scanning electron microscope (SEM) photograph of embodiment 3 gained anhydrous calcium sulfate whisker.
Fig. 7 is X-ray diffraction (XRD) figure of embodiment 4 gained anhydrous calcium sulfate whisker.
Fig. 8 is the scanning electron microscope (SEM) photograph of embodiment 4 gained anhydrous calcium sulfate whisker.
Embodiment
Below, will be described in detail the embodiment of the present invention by reference to the accompanying drawings.
The invention provides a kind of method that normal pressure acidization prepares anhydrous calcium sulfate whisker, comprise the steps:
Step one: by concentrated acid and CaSO
42H
2o (popular name: plaster stone) is 5 ~ 20 be mixed to form slip according to liquid-solid ratio.
Wherein, described concentrated acid can be the one in the vitriol oil, concentrated nitric acid, concentrated hydrochloric acid, strong phosphoric acid.Preferably better effect is concentrated hydrochloric acid.
Wherein, because the solubleness of calcium sulfate in hydrochloric acid increases along with the rising of acid concentration, concentration of hydrochloric acid is raised to a certain degree, and the solubleness of calcium sulfate declines on the contrary.In the present invention, adopt high concentrated hydrochloric acid as medium, the lower solubleness of calcium sulfate and the lower degree of supersaturation of anhydrous calciumsulphate can be controlled, thus improve yield and the quality of product.Comprehensive, the concentration of concentrated hydrochloric acid of the present invention controls as 6.50mol/L ~ 10.83mol/L is good.
Step 2: by described slip stirring reaction 1 ~ 6h in the water bath with thermostatic control of 60 ~ 100 DEG C, obtain suspension liquid.
Step 3: filtered by described suspension liquid, obtains filter cake and filtrate after solid-liquid separation, described filter cake obtains described anhydrous calcium sulfate whisker after drying.
In order to economize on resources, protection of the environment, the described filtrate Posterior circle that can reflux utilizes, and such as, detects its concentration of hydrochloric acid still in described preferable range, described concentrated hydrochloric acid can be replaced in step one and described CaSO
42H
2o mixes.
, show feature of the present invention by several embodiment below, as shown in table 1:
Table 1 embodiment 1 ~ 5 and reaction parameter thereof
All do not pass through calcination from table 1 and composition graphs 1 ~ 8, five embodiments, normal heating just can obtain anhydrous calcium sulfate whisker in a water bath.
Because adopt high concentrated hydrochloric acid directly to prepare anhydrous calciumsulphate, do not need calcination process in preparation process, directly by normal pressure acidization synthesis anhydrous calcium sulfate whisker, can both solve the aquation problem of calcium sulfate crystal whiskers, preparation link can be reduced simultaneously, reduce the preparation cost of whisker.
Claims (4)
1. normal pressure acidization prepares a method for anhydrous calcium sulfate whisker, it is characterized in that, comprises the steps:
By concentrated acid and CaSO
42H
2o is 5 ~ 20 be mixed to form slip according to liquid-solid ratio;
By described slip stirring reaction 1 ~ 6h in the water bath with thermostatic control of 60 ~ 100 DEG C, obtain suspension liquid;
Described suspension liquid is carried out solid-liquid separation and obtain filter cake and filtrate, described filter cake obtains described anhydrous calcium sulfate whisker after drying.
2. prepare the method for anhydrous calcium sulfate whisker according to claim 1, it is characterized in that, described concentrated acid is the one in the vitriol oil, concentrated nitric acid, concentrated hydrochloric acid, strong phosphoric acid.
3. prepare the method for anhydrous calcium sulfate whisker according to claim 2, it is characterized in that, the concentration of described concentrated hydrochloric acid is 6.50mol/L ~ 10.83mol/L.
4. prepare the method for anhydrous calcium sulfate whisker according to claim 2, it is characterized in that, described filtrate backflow Posterior circle utilizes, and replaces described concentrated hydrochloric acid and described CaSO
42H
2o mixes.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201511028199.XA CN105401219B (en) | 2015-12-31 | 2015-12-31 | A kind of method that normal pressure acidization prepares anhydrous calcium sulfate whisker |
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| CN201511028199.XA CN105401219B (en) | 2015-12-31 | 2015-12-31 | A kind of method that normal pressure acidization prepares anhydrous calcium sulfate whisker |
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| CN105401219B CN105401219B (en) | 2018-03-20 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106811801A (en) * | 2017-01-24 | 2017-06-09 | 东南大学 | A kind of preparation method of modified gypsum whisker |
| CN110117813A (en) * | 2019-05-17 | 2019-08-13 | 哈尔滨工业大学（威海） | A method of preparing calcium sulfate crystal whiskers from gypsum offscum |
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|---|---|---|---|---|
| CN1598083A (en) * | 2004-08-20 | 2005-03-23 | 东北大学 | Process for preparing calcium sulfate whisker |
| CN101311337A (en) * | 2008-04-25 | 2008-11-26 | 东北大学 | Process for preparing calcium sulphate whiskers by using flue gas desulfurization gypsum |
| CN102212884A (en) * | 2011-05-04 | 2011-10-12 | 上海大学 | Method for preparing calcium sulfate crystal whisker from many kinds of industrial waste residue gypsum serving as raw materials |
| CN102352535A (en) * | 2011-09-22 | 2012-02-15 | 东莞上海大学纳米技术研究院 | Method for preparing calcium sulfate crystal whiskers from desulfurized gypsum under normal pressure |
| CN102677177A (en) * | 2012-04-13 | 2012-09-19 | 昆明理工大学 | Preparation method of calcium sulfate hemihydrate crystal whiskers high in length diameter ratio |
| CN102912445A (en) * | 2012-10-22 | 2013-02-06 | 浙江天蓝环保技术股份有限公司 | Process and device for preparing gypsum whisker by semi-dry desulfurized fly ash and waste acid |
| CN104005086A (en) * | 2014-04-04 | 2014-08-27 | 贵阳中化开磷化肥有限公司 | Method for preparing calcium sulfate dihydrate crystal whisker from phosphorus gypsum |
| CN104562180A (en) * | 2015-01-07 | 2015-04-29 | 西南科技大学 | Method for preparing calcium sulfate whisker from phosphogypsum |
| CN104911688A (en) * | 2015-06-08 | 2015-09-16 | 中国科学院青海盐湖研究所 | Preparation method of anhydrous calcium sulfate whisker |
| CN105112989A (en) * | 2015-10-14 | 2015-12-02 | 科洋环境工程（上海）有限公司 | Preparation method of calcium sulfate whisker |
-
2015
- 2015-12-31 CN CN201511028199.XA patent/CN105401219B/en active Active
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1598083A (en) * | 2004-08-20 | 2005-03-23 | 东北大学 | Process for preparing calcium sulfate whisker |
| CN101311337A (en) * | 2008-04-25 | 2008-11-26 | 东北大学 | Process for preparing calcium sulphate whiskers by using flue gas desulfurization gypsum |
| CN102212884A (en) * | 2011-05-04 | 2011-10-12 | 上海大学 | Method for preparing calcium sulfate crystal whisker from many kinds of industrial waste residue gypsum serving as raw materials |
| CN102352535A (en) * | 2011-09-22 | 2012-02-15 | 东莞上海大学纳米技术研究院 | Method for preparing calcium sulfate crystal whiskers from desulfurized gypsum under normal pressure |
| CN102677177A (en) * | 2012-04-13 | 2012-09-19 | 昆明理工大学 | Preparation method of calcium sulfate hemihydrate crystal whiskers high in length diameter ratio |
| CN102912445A (en) * | 2012-10-22 | 2013-02-06 | 浙江天蓝环保技术股份有限公司 | Process and device for preparing gypsum whisker by semi-dry desulfurized fly ash and waste acid |
| CN104005086A (en) * | 2014-04-04 | 2014-08-27 | 贵阳中化开磷化肥有限公司 | Method for preparing calcium sulfate dihydrate crystal whisker from phosphorus gypsum |
| CN104562180A (en) * | 2015-01-07 | 2015-04-29 | 西南科技大学 | Method for preparing calcium sulfate whisker from phosphogypsum |
| CN104911688A (en) * | 2015-06-08 | 2015-09-16 | 中国科学院青海盐湖研究所 | Preparation method of anhydrous calcium sulfate whisker |
| CN105112989A (en) * | 2015-10-14 | 2015-12-02 | 科洋环境工程（上海）有限公司 | Preparation method of calcium sulfate whisker |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106811801A (en) * | 2017-01-24 | 2017-06-09 | 东南大学 | A kind of preparation method of modified gypsum whisker |
| CN110117813A (en) * | 2019-05-17 | 2019-08-13 | 哈尔滨工业大学（威海） | A method of preparing calcium sulfate crystal whiskers from gypsum offscum |
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| Publication number | Publication date |
|---|---|
| CN105401219B (en) | 2018-03-20 |
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