CN109112635A - A method of quickly preparing semi-hydrated gypsum whisker and anhydrous gypsum whisker using ardealite - Google Patents
A method of quickly preparing semi-hydrated gypsum whisker and anhydrous gypsum whisker using ardealite Download PDFInfo
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- CN109112635A CN109112635A CN201810906420.4A CN201810906420A CN109112635A CN 109112635 A CN109112635 A CN 109112635A CN 201810906420 A CN201810906420 A CN 201810906420A CN 109112635 A CN109112635 A CN 109112635A
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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
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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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- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a kind of methods that semi-hydrated gypsum whisker Yu anhydrous gypsum whisker are quickly prepared using ardealite, include the following steps, the by-product ardealite that phosphoric acid by wet process " two water laws " technique obtains is mixed with phosphoric acid,diluted, the concentrated sulfuric acid, the free SO of control liquid phase is then added4 2‑Concentration is 9%~15%, the crystal modifier of phosphoric acid quality score 0.3%~2% is added, convert 3~10min, slurry is transferred to after room temperature is aged 10~30min in ageing tank and is filtered under diminished pressure, filter cake fast dewatering under the conditions of 150~200 DEG C of temperature, semi-hydrated gypsum crystal whisker products can be obtained, mother liquor is Ke Xunhuanliyong.Anhydrous gypsum crystal whisker products are can be obtained into after 550~700 DEG C of high temperature furnace high temperature calcining in obtained semi-hydrated gypsum crystal whisker products.Present invention process process is simple, and transformation time is short, and production capacity is big, strong operability, it is easy to accomplish industrialization, moreover it is possible to which a large amount of consumption by-product ardealites realize ardealite high value added utilization.
Description
Technical field
The present invention relates to ardealites, and the side of crystal whisker of gypsum is prepared especially with the industry by-product gypsum containing various impurity
Method.
Background technique
Ardealite is phosphoric acid by wet process industrial by-product, 1 ton of P of every production2O54-5 tons of ardealites are about generated, at present the master of ardealite
Purposes is wanted to have Sulphuric acid co-production cement, Thistle board, building gypsum plaster, gypsum wallboard, plastering gupsum mortar and Sulphuric acid
Coproducing ammonium lime etc., wherein ardealite is maximum in the consumption of building trade.Ester exchange at phosphorus has excellent mechanical property, resistance to
The features such as high temperature, high acid and alkali-resistance and cost performance, has relatively broad purposes, ardealite in the enhancing and modification of composite material
Whisker is prepared instead of the natural gypsum, the high added value of waste ardealite may be implemented.Form that there are three types of ester exchange at phosphorus, two
Water crystal whisker of gypsum, semi-hydrated gypsum whisker and anhydrous gypsum whisker, wherein half water and anhydrous gypsum whisker are common two kinds of forms,
Anhydrous gypsum whisker is most stable.
Ester exchange at phosphorus is white fibrous monocrystal, is under the microscope acicular crystal, draw ratio is greater than
10, the preparation process of ester exchange at phosphorus substantially converts the two of threadiness for the granular calcium sulphate dihydrate in ardealite
Water or hemihydrate calcium sulfate crystal whisker.Chinese patent CN 105603505A discloses that " a kind of ardealite hydro-thermal prepares high length-diameter ratio sulfuric acid
The method of calcium pyroborate ", the ardealite concentration 1%~7% of patent configuration, carries out transformation of crystal, conversion temperature under high pressure hydro-thermal
110~170 DEG C, 4~10h of time, this method process flow is long, and working condition is harsh and production capacity is low, is industrially difficult to answer
With.Normal pressure solwution method can be realized ardealite crystal form without condition of high voltage and be converted from sheet to crystal whisker-shaped, Chinese patent CN
104562180A discloses " a method of with preparing calcium sulphate whiskers from ardealite ", and this method dissolves by heating phosphorus stone using diluted acid
It is filtered after cream, prepares dihydrate gypsum whisker by the way of filtrate crystallisation precipitation, since solubility is very low in diluted acid for calcium sulfate,
In order to be completely dissolved calcium sulfate, required liquid-solid ratio is very high, and production capacity is very low, and economy is poor.Present invention process skill
The targets such as art is easy to get from raw material, production capacity is big, process flow is short, production cost is low are started with, dense with phosphoric acid,diluted to pulp density
The influence to the crystal whisker of gypsum draw ratio of preparation such as selection, sulfuric acid dosage, conversion temperature and time of degree all carried out repeatedly
Grope, optimize and verify, has obtained a kind of method that ardealite low cost quickly prepares crystal whisker of gypsum, through consulting pertinent literature,
There is presently no similar production methods to report in pertinent literature and patent.
Summary of the invention
The purpose of the present invention is to provide a kind of, which quickly to prepare semi-crystal using ardealite, to lead to the method for anhydrous whisker
It crosses crystal whisker of gypsum draw ratio made from this method and reaches 30~50.
A kind of technical solution of the present invention: side quickly preparing semi-hydrated gypsum whisker Yu anhydrous gypsum whisker using ardealite
Method, it is characterised in that its preparation step is as follows:
(1) it weighs a certain amount of phosphoric acid,diluted to be added into reactor, phosphoric acid,diluted mass concentration is 15%~25%, opens stirring dress
It sets, 300~350r/min of revolving speed is gradually added into ardealite and the concentrated sulfuric acid, phosphoric acid,diluted and ardealite after being warming up to 95~100 DEG C
The liquid-solid ratio of (butt) is 2.5~5:1, controls liquid phase SO4 2-Concentration is 9%~15%, compound modifying agent is added, dosage is phosphoric acid
The 0.3%~2% of quality；
(2) slurry is continuously heating to 105~120 DEG C, maintains to convert 3~10min at such a temperature, slurry is transferred to ageing
Room temperature is filtered under diminished pressure after being aged 10~30min in slot；
(3) filtered filter cake is placed in fast dewatering in the drying box for be warming up in advance 150~200 DEG C, can be obtained after drying
To semi-hydrated gypsum crystal whisker products, filtered mother liquor be can be recycled；High temperature furnace by semi-hydrated gypsum whisker at 550~700 DEG C
Anhydrous gypsum crystal whisker products can be obtained in middle calcining.
The above-mentioned semi-crystal that quickly prepared using ardealite must be with the method for anhydrous whisker, phosphoric acid,diluted described in step (1)
One of industrial phosphoric acid, fertilizer phosphoric acid or phosphoric acid purification process by-product raffinate.
The above-mentioned semi-crystal that quickly prepared using ardealite must be with the method for anhydrous whisker, phosphoric acid,diluted and phosphorus stone in step (1)
The liquid-solid ratio range of cream is 3~3.5:1；Liquid phase SO4 2-Concentration is 11%~12%.
The above-mentioned semi-crystal that quickly prepared using ardealite must be with the method for anhydrous whisker, and compound modifying agent is in step (1)
One of magnesium chloride and magnesium sulfate.
The above-mentioned semi-crystal that quickly prepared using ardealite must be with the method for anhydrous whisker, and slurry temperature is 110 in step (2)
~115 DEG C, heating method used is heat transfer oil electric heating, and transformation time is 5~6min.
The above-mentioned semi-crystal that quickly prepared using ardealite must be with the method for anhydrous whisker, filter cake fast dewatering in step (3)
Dry, drying temperature is 180 DEG C, and the cycle-index of mother liquor is 3~5 times.
The above-mentioned semi-crystal that quickly prepared using ardealite must prepare anhydrous gypsum in (3) with the method for anhydrous whisker, step
Calcination temperature when whisker is 600~650 DEG C.
Key of the invention is the additional amount of sulfuric acid, cannot get semi-hydrated gypsum whisker when liquid phase sulfuric acid concentration is less than 9%,
It secondly is conversion temperature, temperature cannot get semi-hydrated gypsum whisker when being lower than 95 DEG C, whisker is long when conversion temperature is 95 DEG C~100 DEG C
Diameter need to reach 2h or more than small and transformation time, and the time greatly extends, and at 105 DEG C of conversion temperature or more, convert 10min or less
The biggish crystal whisker of gypsum of draw ratio can be obtained.Crystal whisker of gypsum technique is prepared compared to existing ardealite, the present invention has following excellent
Gesture:
A) is using phosphoric acid,diluted as transformation of crystal medium, and sulfuric acid is as compound modifying agent.Phosphoric acid,diluted and sulfuric acid are that common industry is former
Material, it is from a wealth of sources, it is at low cost；
B) ardealite pulp density is greater than 20%, and production capacity is big, the filtered all semi-hydrated gypsum whiskers of filter cake, and yield is
100%；
C) the entire conversion process of carries out under normal pressure, and transformation time only needs 3~10min, and process flow is short, and high degree mentions
High production capacity；
D) the crystal whisker of gypsum purity of preparation has reached 93.5% or more, and semi-hydrated gypsum whisker draw ratio 30~50, whiteness is greater than 85,
Anhydrous gypsum whisker draw ratio 30~50, whiteness are greater than 92.
Figure of description
Fig. 1 is the semi-hydrated gypsum whisker microscopic optical structure figure that the present invention obtains；Fig. 2 is the anhydrous gypsum whisker that the present invention obtains
Microscopic optical structure figure.
Specific embodiment
Embodiment 1
Crystallization conversion medium uses wet phosphoric acid purifying process by-product raffinate, P2O5Initial concentration is 47.2%, content of MgO
3.5%, it is diluted with water to 16.5%, the raffinate 3000g after weighing dilution is added to 6L stainless steel circular-cylindrical jacket reactor
In, reactor and agitating paddle are nonstandard production, there is hydraulic barrier in reactor, and heating device uses hotline heater, will extract
Spent acid is warming up to 95 DEG C, opens stirring, speed of agitator 350r/min.
Ardealite raw material 1500g, 98% industrial sulphuric acid 420g are weighed, ardealite is added simultaneously with the concentrated sulfuric acid in 10min
Into raffinate, crystal form modifying agent epsom salt 11g is added.Slurry is warming up to 110 DEG C after charging, speed of agitator tune
To 280r/min, slurry is transferred in the reactive tank of 5L after converting 8min, revolving speed 250r/min is aged 15min at room temperature, subtracts
Press filtration.
Filtered mother liquor can be used as the utilization of ardealite transformation of crystal medium circulation, and filter cake is in the drying box at 200 DEG C
Quick dewatering drying obtains semi-hydrated gypsum crystal whisker products, average aspect ratio 42, half-H 2 O calcium sulphate purity 94.1%, whiteness after cooling
85.1.High temperature furnace high temperature of the obtained semi-hydrated gypsum whisker at 550 DEG C is calcined into 1.5h, anhydrous gypsum crystalline substance is obtained after cooling
Must, average aspect ratio 40, anhydrous gypsum whisker purity 93.6%, whiteness 92.
Embodiment 2
Raffinate P2O5Initial concentration is 47.2%, and content of MgO 3.5% is diluted with water to 20%, the raffinate after weighing dilution
3000g is added in 6L stainless steel circular-cylindrical jacket reactor, and raffinate is warming up to 100 DEG C, opens stirring, speed of agitator
For 350r/min, ardealite raw material 1250g, 98% industrial sulphuric acid 400g are weighed, in 10min simultaneously by ardealite and the concentrated sulfuric acid
It is added in raffinate.Crystal form modifying agent magnesium chloride 10g is added.
Slurry is warming up to 105 DEG C after charging, speed of agitator is adjusted to 280r/min, turns slurry after converting 10min
It moves in the reactive tank of 5L, revolving speed 250r/min is aged 30min at room temperature, is filtered under diminished pressure.
Filtered mother liquor can be used as the utilization of ardealite transformation of crystal medium circulation, and filter cake is in the drying box at 150 DEG C
Quick dewatering drying obtains semi-hydrated gypsum crystal whisker products, average aspect ratio 38, half-H 2 O calcium sulphate purity 94.2%, whiteness after cooling
86.5.High temperature furnace high temperature of the obtained semi-hydrated gypsum whisker at 700 DEG C is calcined into 1.5h, anhydrous gypsum crystalline substance is obtained after cooling
Must, average aspect ratio 37, anhydrous gypsum whisker purity 93.7%, whiteness 94.2.
Embodiment 3
Crystallization conversion medium uses fertilizer phosphoric acid, P2O5Initial concentration is 26.1%, and content of MgO 0.82% is diluted with water to 18%,
Fertilizer phosphoric acid 3000g after weighing dilution, is added in 6L stainless steel circular-cylindrical jacket reactor, fertilizer phosphoric acid is warming up to 97
DEG C, stirring is opened, speed of agitator 350r/min weighs ardealite raw material 1350g, 98% industrial sulphuric acid 435g, in 10min
Ardealite and the concentrated sulfuric acid are added to simultaneously in fertilizer phosphoric acid.Crystal form modifying agent epsom salt 30g is added.
Slurry is warming up to 120 DEG C after charging, and speed of agitator is adjusted to 280r/min, slurry is shifted after converting 4min
Into the reactive tank of 5L, revolving speed 250r/min is aged 20min at room temperature, is filtered under diminished pressure.
Filtered mother liquor can be used as the utilization of ardealite transformation of crystal medium circulation, and filter cake is in the drying box at 180 DEG C
Quick dewatering drying obtains semi-hydrated gypsum crystal whisker products, average aspect ratio 46, half-H 2 O calcium sulphate purity 94.5%, whiteness after cooling
86.6.High temperature furnace high temperature of the obtained semi-hydrated gypsum whisker at 650 DEG C is calcined into 1.5h, anhydrous gypsum crystalline substance is obtained after cooling
Must, average aspect ratio 44, anhydrous gypsum whisker purity 93.9%, whiteness 94.3.
Embodiment 4
Crystallization conversion medium uses industrial phosphoric acid, P2O5Initial concentration is 61.2%, and content of MgO 0.02% is diluted with water to 18%,
Industrial phosphoric acid 3000g after weighing dilution, is added in 6L stainless steel circular-cylindrical jacket reactor, industrial phosphoric acid is warming up to 97
DEG C, stirring is opened, speed of agitator 350r/min weighs ardealite raw material 1350g, 98% industrial sulphuric acid 435g, in 10min
Ardealite and the concentrated sulfuric acid are added to simultaneously in fertilizer phosphoric acid.Crystal form modifying agent epsom salt 30g is added.
Slurry is warming up to 120 DEG C after charging, and speed of agitator is adjusted to 280r/min, slurry is shifted after converting 4min
Into the reactive tank of 5L, revolving speed 250r/min is aged 20min at room temperature, is filtered under diminished pressure.
Filtered mother liquor can be used as the utilization of ardealite transformation of crystal medium circulation, and filter cake is in the drying box at 180 DEG C
Quick dewatering drying obtains semi-hydrated gypsum crystal whisker products, average aspect ratio 46, half-H 2 O calcium sulphate purity 95.6%, whiteness after cooling
88.2.High temperature furnace high temperature of the obtained semi-hydrated gypsum whisker at 650 DEG C is calcined into 1.5h, anhydrous gypsum crystalline substance is obtained after cooling
Must, average aspect ratio 44, anhydrous gypsum whisker purity 96.4%, whiteness 96.2.
Claims (7)
1. a kind of method for quickly preparing semi-hydrated gypsum whisker Yu anhydrous gypsum whisker using ardealite, it is characterised in that it is prepared
Steps are as follows:
(1) it weighs a certain amount of phosphoric acid,diluted to be added into reactor, phosphoric acid,diluted mass concentration is 15%~25%, opens stirring dress
It sets, 300~350r/min of revolving speed, is gradually added into ardealite and the concentrated sulfuric acid after being warming up to 95~100 DEG C, phosphoric acid,diluted and ardealite
Liquid-solid ratio is 2.5~5:1, controls liquid phase SO4 2-Concentration is 9%~15%, and compound modifying agent is added, and dosage is phosphoric acid quality
0.3%~2%；
(2) slurry is continuously heating to 105~120 DEG C, maintains to convert 3~10min at such a temperature, slurry is transferred to ageing
Room temperature is filtered under diminished pressure after being aged 10~30min in slot；
(3) filtered filter cake is placed in fast dewatering in the drying box for be warming up in advance 150~200 DEG C, can be obtained after drying
To semi-hydrated gypsum crystal whisker products, filtered mother liquor be can be recycled；High temperature furnace by semi-hydrated gypsum whisker at 550~700 DEG C
Anhydrous gypsum crystal whisker products can be obtained in middle calcining.
2. a kind of method that semi-hydrated gypsum whisker Yu anhydrous gypsum whisker are quickly prepared using ardealite according to right 1,
It is characterized in that phosphoric acid,diluted described in step (1) is in industrial phosphoric acid, fertilizer phosphoric acid or phosphoric acid purification process by-product raffinate
One kind.
3. a kind of method that semi-hydrated gypsum whisker Yu anhydrous gypsum whisker are quickly prepared using ardealite according to right 1,
It is characterized in that the liquid-solid ratio range of phosphoric acid,diluted and ardealite is 3~3.5:1 in step (1)；Liquid phase SO4 2-Concentration be 11%~
12%。
4. a kind of method that semi-hydrated gypsum whisker Yu anhydrous gypsum whisker are quickly prepared using ardealite according to right 1,
It is characterized in that compound modifying agent is one of magnesium chloride and magnesium sulfate in step (1).
5. a kind of method that semi-hydrated gypsum whisker Yu anhydrous gypsum whisker are quickly prepared using ardealite according to right 1,
It is characterized in that slurry temperature is 110~115 DEG C in step (2), heating method used is heat transfer oil electric heating, transformation time
For 5~6min.
6. a kind of method that semi-hydrated gypsum whisker Yu anhydrous gypsum whisker are quickly prepared using ardealite according to right 1,
It is characterized in that filter cake quick dewatering drying in step (3), drying temperature is 180 DEG C, and the cycle-index of mother liquor is 3~5 times.
7. a kind of method that semi-hydrated gypsum whisker Yu anhydrous gypsum whisker are quickly prepared using ardealite according to right 1,
It is characterized in that calcination temperature when preparing anhydrous gypsum whisker in step (3) is 600~650 DEG C.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114506872A (en) * | 2022-01-05 | 2022-05-17 | 中国科学院大学 | Method for preparing anhydrous gypsum at normal temperature and pressure |
| CN114538811A (en) * | 2021-11-12 | 2022-05-27 | 天宝动物营养科技股份有限公司 | Method for preparing high-strength gypsum from phosphogypsum |
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| US20130288887A1 (en) * | 2012-04-28 | 2013-10-31 | Zhejiang University | Method for preparing a nano-calcium carbonate slurry from waste gypsum as calcium source, the product and use thereof |
| CN103757705A (en) * | 2013-12-20 | 2014-04-30 | 淮南市明月环保科技有限责任公司 | Preparation method of anhydrous calcium sulfate whisker |
| CN105154979A (en) * | 2015-09-18 | 2015-12-16 | 金正大诺泰尔化学有限公司 | Method for producing wet-process phosphoric acid and coproducing alpha-semi-hydrated gypsum whisker and high-purity high-whiteness alpha-semi-hydrated gypsum whisker |
| CN105776303A (en) * | 2016-01-30 | 2016-07-20 | 瓮福（集团）有限责任公司 | Production method of alpha-hemihydrate gypsum |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US20130288887A1 (en) * | 2012-04-28 | 2013-10-31 | Zhejiang University | Method for preparing a nano-calcium carbonate slurry from waste gypsum as calcium source, the product and use thereof |
| CN103757705A (en) * | 2013-12-20 | 2014-04-30 | 淮南市明月环保科技有限责任公司 | Preparation method of anhydrous calcium sulfate whisker |
| CN105154979A (en) * | 2015-09-18 | 2015-12-16 | 金正大诺泰尔化学有限公司 | Method for producing wet-process phosphoric acid and coproducing alpha-semi-hydrated gypsum whisker and high-purity high-whiteness alpha-semi-hydrated gypsum whisker |
| CN105776303A (en) * | 2016-01-30 | 2016-07-20 | 瓮福（集团）有限责任公司 | Production method of alpha-hemihydrate gypsum |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114538811A (en) * | 2021-11-12 | 2022-05-27 | 天宝动物营养科技股份有限公司 | Method for preparing high-strength gypsum from phosphogypsum |
| CN114506872A (en) * | 2022-01-05 | 2022-05-17 | 中国科学院大学 | Method for preparing anhydrous gypsum at normal temperature and pressure |
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