CN106115762A - A kind of preparation method of cauliflower form calcium sulfite microgranule - Google Patents
A kind of preparation method of cauliflower form calcium sulfite microgranule Download PDFInfo
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- CN106115762A CN106115762A CN201610421796.7A CN201610421796A CN106115762A CN 106115762 A CN106115762 A CN 106115762A CN 201610421796 A CN201610421796 A CN 201610421796A CN 106115762 A CN106115762 A CN 106115762A
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- sulfite
- calcium chloride
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/48—Sulfites
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/50—Agglomerated particles
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The present invention relates to the preparation method of a kind of cauliflower form calcium sulfite microgranule, with calcium chloride and sodium sulfite as raw material, it is configured to certain density calcium chloride solution and sodium sulfite solution respectively with water, and with membrane filtration and collect filtrate, a certain amount of citric acid is joined in calcium chloride solution and regulates pH=10 with sodium hydroxide solution, sodium sulfite solution is slowly added in calcium chloride solution, stir while adding, finally the calcium sulfite precipitation generated is filtered, centrifugal, and with after redistilled water and water-ethanol alternately washing, it is dried at 60 DEG C, obtain cauliflower form calcium sulfite.Product pattern obtained by the present invention is cauliflower form, and size, in 5 ~ 10 μm, is evenly distributed, and preparation process is simple, and with low cost, materials safety is nontoxic, has the biggest using value in the peace and quiet field of sugarcane juice.
Description
Technical field
The present invention relates to the preparation method of a kind of cauliflower form calcium sulfite microgranule, belong to field of inorganic chemical engineering.
Background technology
Calcium sulfite is the crystalline powder of a kind of white, contains 0.5 molecular crystalline water (CaSO at ambient temperature3·
0.5H2O), at 360-390 DEG C, heating can lose water of crystallization, is decomposed into calcium oxide and sulfur dioxide, is insoluble at 650 DEG C
Water, for calcic-plastic composite material, cellulosics bleaching antichlor, food preservative and fermentation antibacterial, especially in sugar industry
Have a wide range of applications.Lime cream or calcium chloride can be passed into by sulfur dioxide and sodium sulfite reaction prepares.
Newborn calcium sulfite application in sugar industry be mainly reflected in sugarcane juice peace and quiet during.Pass through Calx
Generate calcium sulfite microgranule with sulfur dioxide or calcium chloride and sodium sulfite reaction, simultaneously the phenols in absorption sugarcane juice,
The non-sugars such as colloid, protein and pigment, reach the purpose of peace and quiet syrup.Therefore, calcium sulfite particle morphology and structure are to sugar
The peace and quiet effect of juice has strong influence.
At present, about preparation and the application of calcium sulfite microgranule, it is concentrated mainly on flue gas desulfurization and prepares desulfurated plaster side
Face.Chinese patent (CN102701618A) utilizes calcium sulfite desulfurated plaster to produce high-strength environment-friendly brushing gypsum；Chinese patent
(CN101712484A) a kind of a diameter of 0.5 ~ 8mm of preparation, surface has been covered with the column calcium sulfite particles of many fine holes, has made
Obtain calcium sulfite to be more fully contacted with water, improve dechlorination effect.Chinese patent (CN101921084A) is with calcium sulfite
For primary raw material, and it is mixed and made into a kind of calcium sulfite skin beautifying ball with organic acid, anion powder, adhesive, has made water quality have
Antibiosis antibacterial characteristics, promotes skin pore to receive thin, supplements skin moisture, thus reach moisturizing skin, prevent skin aging, whitening
The effect of skin protection.But, the research being applied in clarifying syrup by the calcium sulfite of different-shape the most but rarely has report.
Summary of the invention
The technical problem to be solved in the present invention is: provide the preparation method of a kind of cauliflower form calcium sulfite microgranule, the method
Obtained product pattern is cauliflower form, and size, in 5 ~ 10 μm, is evenly distributed, and preparation process is simple, with low cost, raw material
Safety non-toxic, has the biggest using value in the peace and quiet field of sugarcane juice.
The technical scheme solving above-mentioned technical problem is: the preparation method of a kind of cauliflower form calcium sulfite microgranule, with chlorination
Calcium and sodium sulfite are raw material, are configured to 0.1～0.3mol/L calcium chloride solution and 0.1～0.3mol/L sulfurous acid with water respectively
Sodium solution, and with membrane filtration, citric acid joined in calcium chloride solution and regulate pH=9.5～10 with sodium hydroxide solution,
The addition of citric acid is pressed 1mol calcium chloride and is added 3.5～4g citrometers, then presses calcium chloride molal quantity: sodium sulfite mole
Number is 1: 1～1.1 meters, is slowly added in calcium chloride solution by sodium sulfite solution, stirs while adding, finally by generation
Calcium sulfite precipitation filters, is centrifuged, and with after redistilled water and water-ethanol alternately washing, is dried, obtains at 55～65 DEG C
Cauliflower form calcium sulfite.
The further technical scheme of the present invention is: described filter membrane is 0.45 μm filter membrane.
The cauliflower form calcium sulfite footpath grain size obtained is 5～10 μm.
The calcium chloride solution of preparation is identical with sodium sulfite solution concentration.
The present invention, first under conditions of not adding other controlling agents, prepares the calcium sulfite microgranule of cauliflower form, grain
Footpath size is in 5 ~ 10 μm.The present invention is simple to operate, raw material environmental protection, safety non-toxic, and has the biggest application in sugar industry
It is worth.
Accompanying drawing explanation
Fig. 1 be cauliflower form calcium sulfite magnification ratio prepared by the present invention less time scanning electron microscope (SEM) photograph.
Fig. 2 be cauliflower form calcium sulfite magnification ratio prepared by the present invention bigger time scanning electron microscope (SEM) photograph.
Detailed description of the invention
Embodiment 1: respectively with calcium chloride solution and the Asia of 0.1mol/L of water preparation 0.1mol/L in 100ml beaker
Metabisulfite solution, calcium chloride solution and sodium sulfite solution filter with 0.45 μm filter membrane respectively, remove undissolved impurity,
Collecting filtrate, the citric acid then taking 0.038g is dissolved in 100ml calcium chloride solution, and molten with the sodium hydroxide of 0.5mol/L
Liquid regulation calcium chloride solution pH=10 so that it is fully deprotonation.Sodium sulfite solution is slowly added into isopyknic chlorination again
In calcium solution, and it is slowly stirred.Finally the calcium sulfite precipitation generated is filtered, centrifugal, and by redistilled water and anhydrous second
After alcohol alternately washs three times, the driest under the conditions of 60 DEG C.Having obtained particle diameter and be distributed as 5 ~ 10 μm, be evenly distributed, pattern is
The calcium sulfite microgranule of cauliflower form.
Embodiment 2: prepare the calcium chloride water of 0.2mol/L and the sulfurous acid of 0.2mol/L in 100ml beaker respectively
Sodium water solution, then filters with 0.45 μm filter membrane, removes undissolved impurity, and the citric acid then taking 0.076g is dissolved in
In 100ml calcium chloride solution, and regulate calcium chloride solution pH=10 with the sodium hydroxide solution of 0.5mol/L so that it is fully go matter
Sonization.Again sodium sulfite solution is slowly added in isopyknic calcium chloride solution, and is slowly stirred.The Asia that finally will generate
Calcium sulfate precipitation filters, centrifugal, and after alternately washing three times with redistilled water and dehydrated alcohol, the most dry under the conditions of 60 DEG C
Dry.Having obtained particle diameter and be distributed as 5 ~ 10 μm, be evenly distributed, pattern is the calcium sulfite microgranule of cauliflower form.
Embodiment 3: respectively with calcium chloride solution and the sulfurous of 0.3mol/L of water preparation 0.3mol/L in 100ml beaker
Acid sodium solution, then filters with 0.45 μm filter membrane, removes undissolved impurity, and the citric acid then taking 0.11g is dissolved in
In 100ml calcium chloride solution, and regulate calcium chloride solution pH=10 with the sodium hydroxide solution of 0.5mol/L so that it is fully go matter
Sonization.Again sodium sulfite solution is slowly added in isopyknic calcium chloride solution, and is slowly stirred.The Asia that finally will generate
Calcium sulfate precipitation filters, centrifugal, and after alternately washing three times with redistilled water and dehydrated alcohol, the most dry under the conditions of 60 DEG C
Dry.Having obtained particle diameter and be distributed as 5 ~ 10 μm, be evenly distributed, pattern is the calcium sulfite microgranule of cauliflower form.
Various embodiments of the present invention preparation water used by solution is redistilled water.
In various embodiments of the present invention, generate pelleting centrifugation and with redistilled water and dehydrated alcohol alternately washing, with secondary
Distilled water wash once after again with absolute ethanol washing once for alternately washing 1 time.
Claims (4)
1. the preparation method of a cauliflower form calcium sulfite microgranule, it is characterised in that: with calcium chloride and sodium sulfite as raw material, point
It is not configured to 0.1～0.3mol/L calcium chloride solution and 0.1～0.3mol/L sodium sulfite solution with water, and with membrane filtration,
Being joined by citric acid in calcium chloride solution and regulate pH=9.5～10 with sodium hydroxide solution, the addition of citric acid presses 1mol
Calcium chloride adds 3.5～4g citrometers, then by calcium chloride molal quantity: sodium sulfite molal quantity is based on 1: 1～1.1, by Asia
Metabisulfite solution is slowly added in calcium chloride solution, stirs while adding, finally by generate calcium sulfite precipitation filter, from
The heart, and with after redistilled water and water-ethanol alternately washing, be dried at 55～65 DEG C, obtain cauliflower form calcium sulfite.
The preparation method of a kind of cauliflower form calcium sulfite microgranule the most according to claim 1, it is characterised in that: described filter
Film is 0.45 μm filter membrane.
The preparation method of a kind of cauliflower form calcium sulfite microgranule the most according to claim 1 and 2, it is characterised in that: obtain
Cauliflower form calcium sulfite footpath grain size be 5～10 μm.
The preparation method of a kind of cauliflower form calcium sulfite microgranule the most according to claim 1 and 2, it is characterised in that: preparation
Calcium chloride solution identical with sodium sulfite solution concentration.
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| CN201610421796.7A CN106115762B (en) | 2016-06-14 | 2016-06-14 | A kind of preparation method of cauliflower-shaped calcium sulfite particulate |
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| CN201610421796.7A CN106115762B (en) | 2016-06-14 | 2016-06-14 | A kind of preparation method of cauliflower-shaped calcium sulfite particulate |
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| CN106115762B CN106115762B (en) | 2017-11-28 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108529660A (en) * | 2017-03-01 | 2018-09-14 | 广西科技大学 | A kind of preparation method of square calcium sulfite particle |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201284240Y (en) * | 2008-10-07 | 2009-08-05 | 刘武义 | Calcium sulfite particle |
| CN102092765A (en) * | 2010-12-01 | 2011-06-15 | 何侠 | Method for preparing roasted sulfate residues into sulfites by using chemical method |
| CN103964484A (en) * | 2014-05-27 | 2014-08-06 | 湖南恒光科技股份有限公司 | Preparation process of nano anhydrous calcium sulfate |
-
2016
- 2016-06-14 CN CN201610421796.7A patent/CN106115762B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201284240Y (en) * | 2008-10-07 | 2009-08-05 | 刘武义 | Calcium sulfite particle |
| CN102092765A (en) * | 2010-12-01 | 2011-06-15 | 何侠 | Method for preparing roasted sulfate residues into sulfites by using chemical method |
| CN103964484A (en) * | 2014-05-27 | 2014-08-06 | 湖南恒光科技股份有限公司 | Preparation process of nano anhydrous calcium sulfate |
Non-Patent Citations (3)
| Title |
|---|
| ABRAHAM COHEN ET AL.: ""STUDIES ON ALKALINE EARTH SULFITES - I. NEW CRYSTALLINE PHASES OF HYDRATED, ALCOHOLATED AND UNSOLVATED CALCIUM SULFITE"", 《INORG.NUCL.CHEM.LETTERS》 * |
| T.MATSUNO: ""GROWTH OF METASTABLE CaSO3•4H2O CYSTRAL FROM GELS WITH ORGANINC ADDITIVES"", 《JOURNAL OF CRYSTAL GROWTH》 * |
| T.MATSUNO: ""SPHERULITIC CRYSTAL GROWTh OF CaSO3 O.5H2O IN GEL"", 《JOURNAL OF CRYSTAL GROWTH》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108529660A (en) * | 2017-03-01 | 2018-09-14 | 广西科技大学 | A kind of preparation method of square calcium sulfite particle |
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