CN105568387A - Preparation method of calcium sulfate whiskers - Google Patents
Preparation method of calcium sulfate whiskers Download PDFInfo
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- CN105568387A CN105568387A CN201610125599.0A CN201610125599A CN105568387A CN 105568387 A CN105568387 A CN 105568387A CN 201610125599 A CN201610125599 A CN 201610125599A CN 105568387 A CN105568387 A CN 105568387A
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- preparation
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- calcium sulfate
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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
-
- 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
- C30B7/12—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by electrolysis
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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)
- Electrochemistry (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention provides a preparation of calcium sulfate whiskers. The preparation method comprises the following steps of dividing a reaction vessel into a cathode chamber and an anode chamber by using an anion exchange membrane; adding a cathode plate to the cathode chamber; adding an anode plate to the anode chamber; adding a soluble sulfate water solution into the cathode chamber; adding a soluble calcium salt water solution into the anode chamber; switching on a direct-current power supply; obtaining needle-shaped calcium sulfate whiskers in the cathode chamber after regulating pH (Potential of Hydrogen) and applying voltage.
Description
Technical field
The invention belongs to calcium sulfate crystal whiskers preparation field, particularly use the method for ion-exchange film preparation calcium sulfate crystal whiskers.
Background technology
Calcium sulfate crystal whiskers can as the inorganic fillings in matrix material, the intensity of material can be increased and have fire-retardant effect, environmental protection is pollution-free, apply very extensive, production method industrial at present has: (1) water autoclave process: raw material is obtained suspension with certain proportioning, under the conditions such as certain temperature, pressure, pH value, be placed in autoclave and complete preparation process, can calcium sulfate whiskers be obtained.(2) normal pressure acidization: after gypsum raw material is normally sized mixing by normal pressure acidization, under the conditions such as certain temperature, pH value, can obtain the higher crystal whisker products of purity through acidification.(3) micro emulsion method: raw material is made into certain density solution respectively, adds certain tensio-active agent, catalyzer etc. in the solution, by solution mixing ageing, can obtain crystal whisker products after filtration.(4) ion exchange method: zinc sulfate and ion exchange resin are raw material, using D113 type calcium type Zeo-karb as original template, by after pre-treatment with solution of zinc sulfate hybrid reaction, filter after be separated can obtain calcium sulfate crystal whiskers and zinc-type Zeo-karb.Zinc-type Zeo-karb, can recycle in the basic conditions through calcium salt process.The shortcomings such as current hydrothermal method is industrial conventional method, but existing method has facility investment large, and production cost is high, the invention provides that a kind of cost is low, the production method of the simple calcium sulfate crystal whiskers of reduced investment, operational condition.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of method adopting ion-exchange membrane to produce calcium sulfate crystal whiskers.
The principle that the present invention adopts is: with ion-exchange membrane, reaction vessel is divided into cathode compartment and anolyte compartment, soluble sulphate is added as aqueous sodium persulfate solution in cathode compartment, anolyte compartment adds soluble calcium salt as calcium chloride water, apply DC electric field, allow the sulfate radical in cathode compartment enter anolyte compartment under electric drive, with calcium binding, generate calcium sulfate, by strength of solution, voltage and pH regulator, obtain acicular calcium sulfate whisker at cathode compartment.
A preparation method for calcium sulfate crystal whiskers, its step is as follows:
A, with anion-exchange membrane, reaction vessel is divided into two portions: cathode compartment and anolyte compartment, cathode compartment adds negative plate, and anolyte compartment adds positive plate;
Add the soluble sulphate aqueous solution in B, cathode compartment, anolyte compartment adds solubility calcium salt brine solution, and room, two pole all adds stirring;
C, connection direct supply, regulate pH;
Acicular calcium sulfate whisker is obtained at cathode compartment after D, making alive.
Described preparation method, preferably, for ensureing the consistence of calcium sulfate crystal whiskers, constantly can fill into calcium ion in anode room, filling into sulfate ion, and add stirring at cathode compartment and anolyte compartment to cathode compartment.
Described preparation method, preferably, soluble sulphate can be sodium sulfate, potassium sulfate etc.
Described preparation method, preferably, soluble sulphate salt concn used is 0.5-30%, preferred 2-10%.
Described preparation method, preferably, soluble calcium salt used can be calcium chloride, nitrocalcite etc.
Described preparation method, preferably, solubility calcium salt concn used is 0.5-30%, preferred 1-5%.
Described preparation method, preferably, also comprise step e, disconnect direct supply, continue to stir, whisker continued growth, obtains the calcium sulfate crystal whiskers that length-to-diameter ratio is greater than 100.
Feature of the present invention is:
(1) equipment is simple, does not need High Temperature High Pressure;
(2) available starting material are easy to get;
(3) operational condition is gentle, simple to operate.
Accompanying drawing explanation
Accompanying drawing 1 is the process diagram of a kind of preparation method of calcium sulfate crystal whiskers.
Accompanying drawing 2 is calcium sulfate crystal whiskers figure prepared by present method.
Wherein 1-positive plate; 2-negative plate; 3-anion-exchange membrane; 4-anolyte compartment; 5-cathode compartment; 6-calcium sulfate crystal whiskers.
Specific implementation method
Describe technical scheme of the present invention in detail below in conjunction with embodiment, but protection domain is not limited thereto.Apparatus of the present invention and material all can be bought from market.The extraordinary hyposmosis EDI film that such as described anion-exchange membrane can be produced with gold autumn environmental protection, upperization, Ya Sitong etc., hyposmosis separatory membrane, electrolytic film etc.
The preparation method of embodiment 1 one kinds of calcium sulfate crystal whiskers, comprises the following steps:
A, with anion-exchange membrane, reaction vessel is divided into two portions: cathode compartment and anolyte compartment.
Aqueous sodium persulfate solution is added, concentration 5% (quality) in B, cathode compartment; Anolyte compartment adds calcium chloride water, concentration 2% (quality), and room, two pole all adds stirring.
C, connection direct supply, voltage 4V, electric current 0.25A, pH regulator is 3,
D, making alive obtained acicular calcium sulfate whisker at cathode compartment after 2.5 hours.
E, disconnection direct supply, continue to stir, whisker continued growth, obtains the calcium sulfate crystal whiskers that length-to-diameter ratio is greater than 100.
Accompanying drawing 1 is the process diagram of a kind of preparation method of calcium sulfate crystal whiskers.Accompanying drawing 2 is calcium sulfate crystal whiskers figure prepared by present method, Calcium Sulfate Whiskers 0.6-1.2 micron prepared by analysis, length 180-300 micron.
The preparation method of embodiment 2 one kinds of calcium sulfate crystal whiskers, step is as follows:
A, with anion-exchange membrane, reaction vessel is divided into two portions: cathode compartment and anolyte compartment, cathode compartment adds negative plate, and anolyte compartment adds positive plate;
Add the soluble sulphate aqueous solution (potassium sulfate, mass concentration 10%) in B, cathode compartment, anolyte compartment adds solubility calcium salt brine solution (nitrocalcite, mass concentration 30%), and room, two pole all adds stirring; For ensureing the consistence of calcium sulfate crystal whiskers, constantly can fill into calcium ion in anode room, filling into sulfate ion to cathode compartment, and all add stirring at cathode compartment and anolyte compartment.
C, connection direct supply, regulate pH;
Acicular calcium sulfate whisker is obtained at cathode compartment after D, making alive.
Certainly, the above embodiment of the present invention is only and example of the present invention is described, and is not the restriction to the specific embodiment of the present invention.For those of ordinary skill in the field, other multi-form change or variations can also be done in the basis of above-mentioned citing.Here cannot all embodiments be illustrated in detail.Every belong to technical scheme of the present invention the apparent change of amplifying out or variation be still in the row of protection scope of the present invention.
Claims (7)
1. a preparation method for calcium sulfate crystal whiskers, is characterized in that, step is as follows:
A, with anion-exchange membrane, reaction vessel is divided into two portions: cathode compartment and anolyte compartment, cathode compartment adds negative plate, and anolyte compartment adds positive plate;
Add the soluble sulphate aqueous solution in B, cathode compartment, anolyte compartment adds solubility calcium salt brine solution, and room, two pole all adds stirring;
C, connection direct supply, regulate pH;
Acicular calcium sulfate whisker is obtained at cathode compartment after D, making alive.
2. preparation method according to claim 1, is characterized in that, for ensureing the consistence of calcium sulfate crystal whiskers, constantly can fill into calcium ion in anode room, filling into sulfate ion, and all add stirring at cathode compartment and anolyte compartment to cathode compartment.
3. preparation method according to claim 1, is characterized in that, soluble sulphate can be sodium sulfate, potassium sulfate etc.
4. according to preparation method according to claim 3, it is characterized in that, soluble sulphate salt concn used is 0.5-30%, preferred 2-10%.
5. preparation method according to claim 1, is characterized in that, soluble calcium salt used can be calcium chloride, nitrocalcite etc.
6. according to preparation method according to claim 5, it is characterized in that, solubility calcium salt concn used is 0.5-30%, preferred 1-5%.
7. preparation method according to claim 1, is characterized in that, also comprises step e, disconnects direct supply, and continue to stir, whisker continued growth, obtains the calcium sulfate crystal whiskers that length-to-diameter ratio is greater than 100.
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| CN201610125599.0A CN105568387B (en) | 2016-02-26 | 2016-02-26 | A kind of preparation method of calcium sulfate crystal whiskers |
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| CN201610125599.0A CN105568387B (en) | 2016-02-26 | 2016-02-26 | A kind of preparation method of calcium sulfate crystal whiskers |
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| CN105568387A true CN105568387A (en) | 2016-05-11 |
| CN105568387B CN105568387B (en) | 2019-03-26 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108503887A (en) * | 2018-04-27 | 2018-09-07 | 福州大学 | A kind of acicular calcium sulfate and preparation method thereof prepared using desulfurization gypsum powder |
| CN113882021A (en) * | 2021-10-12 | 2022-01-04 | 贵州大学 | Method for preparing calcium sulfate whisker by phosphogypsum high-temperature high-pressure method |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1683594A (en) * | 2005-03-14 | 2005-10-19 | 新疆大学 | Process for preparing super fine metal oxide |
| CN101168852A (en) * | 2007-08-31 | 2008-04-30 | 武善东 | Mass production method for calcium sulfate whisker |
| CN104261449A (en) * | 2014-09-22 | 2015-01-07 | 四川大学 | Method for preparing high-purity carbonate by using calcium and magnesium-rich solution to mineralize CO2 |
| CN204714911U (en) * | 2015-06-17 | 2015-10-21 | 黑龙江科技大学 | New device prepared by nano cerium dioxide powder |
-
2016
- 2016-02-26 CN CN201610125599.0A patent/CN105568387B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1683594A (en) * | 2005-03-14 | 2005-10-19 | 新疆大学 | Process for preparing super fine metal oxide |
| CN101168852A (en) * | 2007-08-31 | 2008-04-30 | 武善东 | Mass production method for calcium sulfate whisker |
| CN104261449A (en) * | 2014-09-22 | 2015-01-07 | 四川大学 | Method for preparing high-purity carbonate by using calcium and magnesium-rich solution to mineralize CO2 |
| CN204714911U (en) * | 2015-06-17 | 2015-10-21 | 黑龙江科技大学 | New device prepared by nano cerium dioxide powder |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108503887A (en) * | 2018-04-27 | 2018-09-07 | 福州大学 | A kind of acicular calcium sulfate and preparation method thereof prepared using desulfurization gypsum powder |
| CN113882021A (en) * | 2021-10-12 | 2022-01-04 | 贵州大学 | Method for preparing calcium sulfate whisker by phosphogypsum high-temperature high-pressure method |
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| CN105568387B (en) | 2019-03-26 |
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Effective date of registration: 20181217 Address after: 265200 No. 79 Changjiang Road, Laiyang Economic Development Zone, Yantai City, Shandong Province Applicant after: Yantai Far East Fine Chemical Co., Ltd. Address before: 264005, Qingquan Road, Laishan District, Shandong, Yantai, 32 Applicant before: Yantai University |
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Denomination of invention: A preparation method of calcium sulfate whisker Effective date of registration: 20220616 Granted publication date: 20190326 Pledgee: Rizhao Bank Co.,Ltd. Yantai Zhifu sub branch Pledgor: Yantai Far East Fine Chemical Co.,Ltd. Registration number: Y2022980007840 |