CN105624772B - A kind of control method of semi-hydrated gypsum monocrystalline oriented growth - Google Patents
A kind of control method of semi-hydrated gypsum monocrystalline oriented growth Download PDFInfo
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- CN105624772B CN105624772B CN201610030658.6A CN201610030658A CN105624772B CN 105624772 B CN105624772 B CN 105624772B CN 201610030658 A CN201610030658 A CN 201610030658A CN 105624772 B CN105624772 B CN 105624772B
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- monocrystalline
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- gypsum
- hydrated gypsum
- ardealite
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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
- 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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- 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
Abstract
The invention discloses a kind of control method of semi-hydrated gypsum monocrystalline oriented growth, and it is that acidity regulator is added in ardealite, adds water, it is well mixed, after ageing, it is fitted into the reactor with condensation reflux unit, adds impurity stabilizer, crystal face selection adsorbent, after well mixed, heating response is carried out, while ion motion controller is added in reaction system, reaction terminates rear, cooling, filtering, dries solid, obtains the controllable semi-hydrated gypsum monocrystalline of form.The characteristics of this method technique is simple, and cost is low, it is adapted to industrialized production.
Description
Technical field
The present invention relates to gypsum, more particularly to a kind of column pattern that may be used as in building, plastics, rubber, coating
The preparation method of semi-hydrated gypsum monocrystal.
Background technology
Gypsum is sulfate mineral, and its chemical molecular formula is CaSO42H2O.Gypsum can be dehydrated to form anhydrite,
They are in a kind of metastable condition in nature, under certain condition can mutual inversion of phases.Natural gypsum chief value be it
Heated under condition of different temperatures, its calcined product takes on a different character.Start when the natural gypsum such as being heated into 65~70 DEG C
Dehydration, becomes semi-hydrated gypsum；It is heated to gradually be dehydrated within 200 DEG C, semi-hydrated gypsum partially changes into anhydrous gypsum, but contacts with water
Condense quickly and be changed into dihydrate gypsum；200~300 DEG C are heated to, mainly as anhydrous gypsum, condensation is slack-off, but intensity increases；Add
Heat is anhydrous gypsum to product at 300~450 DEG C, and condensation accelerates, but intensity is relatively low；It is heated between 400~700 DEG C, changes
Components unchanged is learned, turns into a kind of new variant --- " burning to death " gypsum, its is extremely difficult to be dissolved in water, adds also non-condensing after water；Continue to heat
During to 800 DEG C, anhydrous gypsum becomes to condense slowly and hardened；When being heated to 800~1000 DEG C, free lime is generated, is obtained just
Normal extremely valuable conventional calcination gypsum；Semi-hydrated gypsum mainly makees the prefabrication of gypsum, such as plasterboard, wall body construction, heat-insulated
Semicircular tile, building decoration product etc..Gypsum building products have fire prevention, heat-insulated, sound-absorbing, shrinkage factor is small and can follow closely, can saw, can bond and
The features such as body weight is light, anti-seismic performance is good [feature and purposes [J] the Shandong land resources of gypsum, 2005,21B：46].
Ardealite is the industrial residue discharged during Wet-process Phosphoric Acid Production, can contain two due to the difference of production procedure
Water gypsum (CaSO42H2O) and semi-hydrated gypsum (CaSO40.5H2O) are using dihydrate gypsum as Main Ingredients and Appearance.Additionally containing few
Measure the impurity such as undecomposed ground phosphate rock, free phosphoric acid, ferric phosphate, aluminum phosphate and fluosilicate；The year discharge of whole world ardealite
Amount is close to 200,000,000 tons, and the annual emissions of China's ardealite are also above 10,000,000 tons.This does not only take up a large amount of soils, and seriously
Pollute environment [comprehensive utilization [J] Environmental science and technologies of seat U.S. cloud ardealites, 2001, (3)：10~13].
What flower carries out water-washing pre-treatment when using ardealite to it, except the impurity in removing slag, to avoid impurity to gypsum
[what flower ardealites base alcohol~hydro-thermal method prepares the research of big L/D ratio wastewaters with modified calcium sulfate whiskers [J] southwest science and technology for the influence of pattern
University, 2014:17].Ardealite is handled with water, caused waste water will pollute environment.
Sun Hong is beautiful et al. to mix the phosphogypsum powder of acquisition with diluted acid, obtains calcic and the acid of sulfate ion and insoluble matter
Property mixed liquor, filtering obtains acid filtrate, the acid filtrate crystallization of acquisition crystallized, and obtains calcium sulfate crystal whiskers [Sun Hongjuan, beam
Ya Qin, Peng Tongjiang, wait a kind of with the method [P] of preparing calcium sulphate whiskers from ardealite, China, 201510007196.1].The work
Skill is extracted with sour (nitric acid or hydrochloric acid) to the utility in ardealite, and acid is readily volatilized by etching apparatus, and environment is made
Into pollution.
Calcium sulfate crystal whiskers prepared by what flower and Sun Hongjuan et al., are needle-like, pattern is uncontrollable；Easily to environment in production process
Pollute.
The content of the invention
The purpose of the present invention is the deficiency for prior art scheme, there is provided a kind of low cost, high efficiency, morphology controllable
The preparation method of semi-hydrated gypsum monocrystalline, to realize the gypsum monocrystalline morphology controllable prepared, environmentally safe purpose.
To achieve the above objectives, the present invention is to adopt the following technical scheme that：
A kind of control method of semi-hydrated gypsum monocrystalline oriented growth, it is characterised in that comprise the steps successively：
A, pretreatment of raw material：Acidity regulator is added in ardealite, adds water, is well mixed, is aged 24h；It is wherein sour
Spend 1~10% that conditioning agent addition is phosphogypsum quality；The addition of water is the 100~500% of phosphogypsum quality；
B, the preparation of gypsum monocrystalline：Poured into the processing ardealite that step A is obtained in the reactor with condensation reflux unit,
Add impurity stabilizer, crystal face selection adsorbent, be well mixed after, carry out heating response, while in reaction system add from
Sub- motion controller, reaction terminate rear, cooling, filtering, dry solid, obtain semi-hydrated gypsum monocrystalline.
In the present invention：Described impurity stabilizer addition is phosphogypsum quality 100~500%；Crystal face selection adsorbent
Addition is the impurity stabilizer of phosphogypsum quality 1~10%；Acidity regulator described in step A is in calcium oxide, calcium carbonate
It is a kind of；Impurity stabilizer described in step B is one kind in sorbierite, mannitol, glycerine；Crystal face selection adsorbent is along fourth
One kind in enedioic acid, polycarboxylic acids, butanedioic acid；Ion motion controller described in step B, for one can produce alternating electric field or
The device of alternating magnetic field, its frequency-adjustable, frequency are 0.1~50HZ；Reaction temperature described in step B is 90~120 DEG C, reaction
Time is 0.5~2 hour.
This method acidity regulator, the pH value of ardealite is adjusted, it is changed into neutral from acidity, acid solution can be avoided
Corrosion to equipment.Impurity stabilizer, avoids impurity element from dissolving in the solution, avoids double of water gypsum crystal growth of impurity
Influence；The selectable particular crystal plane adsorbed in monocrystalline of crystal face selection adsorbent, so as to suppress the growth of the crystallographic direction, makes crystalline substance
Body grows along other crystallographic directions, so as to realize oriented growth；Ion motion controller, controlled by electric field or magnetic field in solution
The direction of motion and speed of ion, promote ion ordered arrangement on monocrystalline, improve single crystal growth rate.This method phosphorous chemical industry
Caused waste residue is raw material, prepares gypsum monocrystalline, and the gypsum has the characteristics of crystal development is complete, intensity is high, as plastics, rubber
The filler of glue, coating, its intensity can be improved；As gypsum sheet material, high strength gypsum sheet material also can obtain.This method has technique simple
Singly, the characteristics of cost is low, it is adapted to industrialized production.
Embodiment
The present invention is described in further detail below in conjunction with specific embodiment.
A, pretreatment of raw material：
Table 1 lists the dosage of various raw materials in 13 embodiment pretreatments of raw material that numbering is 1~13：According to table 1 not
Same embodiment determines the addition of acidity regulator (calcium oxide, calcium carbonate) and water, and is aged 24h, and ardealite raw material is entered
Row pretreatment.
Pretreatment of raw material (the unit of table 1：g)
B：The preparation of gypsum monocrystalline
Poured into the processing ardealite that step A is obtained in the reactor with condensation reflux unit, add impurity stabilizer, it is brilliant
Face selected adsorbent, after being well mixed, heating response is carried out, while ion motion controller is added in reaction system, reacted
After end, cool down, filter, drying solid, obtaining semi-hydrated gypsum monocrystalline.
Preparation (the unit of the gypsum monocrystalline of table 2：g)
Note：Alternating electric field 3000V/m, alternating magnetic field are 500 Gausses.
Embodiments of the invention can be implemented and can reach goal of the invention, obtain crystallizing preferable semi-hydrated gypsum monocrystalline, shape
Looks are short cylinder.
Claims (2)
1. a kind of control method of semi-hydrated gypsum monocrystalline oriented growth, it is characterised in that comprise the steps：
A, pretreatment of raw material：Acidity regulator is added in ardealite, adds water, is well mixed, is aged 24h；Wherein acidity is adjusted
Section agent is one kind in calcium oxide, calcium carbonate, and addition is the 1~10% of phosphogypsum quality；The addition of water is phosphogypsum quality
100~500%；
B, the preparation of gypsum monocrystalline：Pour into the reactor with condensation reflux unit, add in the processing ardealite that step A is obtained
Impurity stabilizer, crystal face selection adsorbent, after being well mixed, heating response is carried out, while transported in reaction system plus ion
Movement controller, reaction terminate rear, cooling, filtering, dry solid, obtain semi-hydrated gypsum monocrystalline；Wherein impurity stabilizer is mountain
Pears alcohol, its addition are phosphogypsum quality 100~500%；Crystal face selection adsorbent is polycarboxylic acids, and its addition is ardealite matter
Amount 1~10%；Ion motion controller is a device that can produce alternating electric field or alternating magnetic field, its frequency-adjustable, and frequency is
0.1~50Hz.
2. the control method of semi-hydrated gypsum monocrystalline oriented growth according to claim 1, it is characterised in that institute in step B
Reaction temperature is stated as 90~120 DEG C, the reaction time is 0.5~2 hour.
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| CN112442731A (en) * | 2020-11-06 | 2021-03-05 | 昆明理工大学 | Method for directionally regulating and controlling crystal transformation and growth by multiple physical fields |
| CN113046832B (en) * | 2021-03-10 | 2022-05-13 | 西安建筑科技大学 | Method for preparing calcium sulfate hemihydrate crystal whiskers through short-period low-cost hydrothermal method |
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