CN102674425A - Production technique of nano calcium carbonate by normal temperature method - Google Patents
Production technique of nano calcium carbonate by normal temperature method Download PDFInfo
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- CN102674425A CN102674425A CN2012101587165A CN201210158716A CN102674425A CN 102674425 A CN102674425 A CN 102674425A CN 2012101587165 A CN2012101587165 A CN 2012101587165A CN 201210158716 A CN201210158716 A CN 201210158716A CN 102674425 A CN102674425 A CN 102674425A
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- normal temperature
- carbonization
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- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 title claims abstract description 102
- 229910000019 calcium carbonate Inorganic materials 0.000 title claims abstract description 76
- 238000000034 method Methods 0.000 title claims abstract description 46
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 21
- 239000013078 crystal Substances 0.000 claims abstract description 30
- 238000001035 drying Methods 0.000 claims abstract description 26
- 238000010000 carbonizing Methods 0.000 claims abstract description 11
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 30
- 238000003763 carbonization Methods 0.000 claims description 28
- 230000015572 biosynthetic process Effects 0.000 claims description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 19
- 239000000292 calcium oxide Substances 0.000 claims description 15
- 235000012255 calcium oxide Nutrition 0.000 claims description 15
- 238000007670 refining Methods 0.000 claims description 15
- 239000003795 chemical substances by application Substances 0.000 claims description 14
- 239000000243 solution Substances 0.000 claims description 13
- 239000002512 suppressor factor Substances 0.000 claims description 12
- 239000012065 filter cake Substances 0.000 claims description 10
- 235000013336 milk Nutrition 0.000 claims description 10
- 239000008267 milk Substances 0.000 claims description 10
- 210000004080 milk Anatomy 0.000 claims description 10
- 239000011259 mixed solution Substances 0.000 claims description 10
- 239000001569 carbon dioxide Substances 0.000 claims description 9
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 9
- 238000000746 purification Methods 0.000 claims description 9
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 claims description 8
- 230000018044 dehydration Effects 0.000 claims description 8
- 238000006297 dehydration reaction Methods 0.000 claims description 8
- 230000005587 bubbling Effects 0.000 claims description 6
- 239000012535 impurity Substances 0.000 claims description 5
- 238000004381 surface treatment Methods 0.000 claims description 5
- 239000000725 suspension Substances 0.000 claims description 5
- MOMKYJPSVWEWPM-UHFFFAOYSA-N 4-(chloromethyl)-2-(4-methylphenyl)-1,3-thiazole Chemical compound C1=CC(C)=CC=C1C1=NC(CCl)=CS1 MOMKYJPSVWEWPM-UHFFFAOYSA-N 0.000 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 4
- 150000003016 phosphoric acids Chemical class 0.000 claims description 4
- 235000019983 sodium metaphosphate Nutrition 0.000 claims description 4
- 239000001488 sodium phosphate Substances 0.000 claims description 4
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical group [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 4
- 229910000406 trisodium phosphate Inorganic materials 0.000 claims description 4
- 235000019801 trisodium phosphate Nutrition 0.000 claims description 4
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 4
- 229960001763 zinc sulfate Drugs 0.000 claims description 4
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 4
- 229920002472 Starch Polymers 0.000 claims description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- 239000001913 cellulose Substances 0.000 claims description 2
- 229920002678 cellulose Polymers 0.000 claims description 2
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 2
- 239000004310 lactic acid Substances 0.000 claims description 2
- 235000014655 lactic acid Nutrition 0.000 claims description 2
- 239000008107 starch Substances 0.000 claims description 2
- 235000019698 starch Nutrition 0.000 claims description 2
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 239000002245 particle Substances 0.000 abstract description 3
- 239000004033 plastic Substances 0.000 abstract description 3
- 229920003023 plastic Polymers 0.000 abstract description 3
- 239000012847 fine chemical Substances 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- 239000000853 adhesive Substances 0.000 abstract 1
- 230000001070 adhesive effect Effects 0.000 abstract 1
- 238000003889 chemical engineering Methods 0.000 abstract 1
- 239000003973 paint Substances 0.000 abstract 1
- 239000000047 product Substances 0.000 description 5
- 238000005255 carburizing Methods 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000007710 freezing Methods 0.000 description 3
- 230000008014 freezing Effects 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 2
- 238000007639 printing Methods 0.000 description 2
- 238000004513 sizing Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 235000011089 carbon dioxide Nutrition 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
Landscapes
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Abstract
The invention discloses a production technique of nano calcium carbonate by a normal temperature method, belonging to the technical field of fine chemical engineering. The production technique comprises the following steps: proportioning, carbonizing, treating, dehydrating, primary drying, secondary drying and depolymerizing. The invention has the characteristics of low equipment investment, low energy consumption, low production cost and the like, can implement production under normal temperature conditions, and can control the particle size and crystal form. The nano calcium carbonate produced by the technique disclosed by the invention can be used as a filling material in plastics industry, rubber industry, paint industry, paper manufacturing industry, ink industry, adhesive industry and other industries.
Description
Technical field
The present invention relates to the fine chemical technology field, particularly a kind of normal temperature method nanometer grade calcium carbonate production technique.
Background technology
Nanometer grade calcium carbonate is claimed super fine calcium carbonate again, is mainly used in plastics industry, rubber industry, coatings industry, paper industry, printing ink industry and sizing agent industry etc.The working method of nanometer grade calcium carbonate mainly is a carborization; The main mode of production of nanometer grade calcium carbonate carbonization at present is a low-temperature freezing; As: band stirs bubbling carborization, hypergravity carborization etc., and these production technique all must be equipped with the freezing device, thereby; Its facility investment is bigger, and energy consumption and production cost are all very high.
Summary of the invention
The purpose of this invention is to provide that a kind of facility investment is few, energy consumption and production cost is lower, can under normal temperature condition, produce, and can control particle diameter, also can control the nanometer grade calcium carbonate production technique of crystal formation.
The technical scheme that the present invention taked is a kind of normal temperature method nanometer grade calcium carbonate production technique of invention, and its technical process is:
A, batching: aqua calcis through the suspension separator, is removed impurity, and add quicklime concentration content in the water adjustment solution, become refining aqua calcis at 6-10%, subsequent use;
B, carbonization: subsequent use refining aqua calcis is placed carbonating tower; The dioxide gas (generally, carbonic acid gas volume content wherein is 20-40%) that feeds after purifying carries out bubbling carbonizing, and adds crystal formation directed agents and the crystal formation suppressor factor that accounts for quicklime weight 1-3% in the refining aqua calcis; Under 20-65 ℃ of temperature, carry out carbonizing treatment;, the pH value in the solution can stop carbonization when reaching 6.5-7.5, the nano-calcium carbonate milk sap after the collection carbonization, and subsequent use;
Used crystal formation directed agents and crystal formation suppressor factor are that a kind of in vitriol, phosphoric acid, phosphoric acid salt, Hydrocerol A, lactic acid, ROHM, ZX-I, starch, the Mierocrystalline cellulose or two kinds are multiple or whole; When adopting two kinds when multiple or whole, the proportioning of each component can adopt single-candidate, also can adopt other ratio;
C, processing: subsequent use nano-calcium carbonate milk sap is heated to 60-80 ℃, adds the StNa that accounts for quicklime weight 2-2.5%, carry out surface treatment, become and handle the nano-calcium carbonate mixed solution, subsequent use;
D, dehydration: subsequent use processing nano-calcium carbonate mixed solution is carried out processed, let its water cut reduce to 40-60%, collect the nano-calcium carbonate filter cake after dewatering, subsequent use;
E, one-level drying: subsequent use nano-calcium carbonate filter cake is carried out the drying first time, let its water cut reduce to 10-20%, become dried nano-calcium carbonate just, subsequent use;
F, secondary drying: subsequent use first dried nano-calcium carbonate is carried out redrying handle, let its water cut reduce to below 0.5%, become the work in-process nano-calcium carbonate, subsequent use;
G, depolymerization: subsequent use work in-process nano-calcium carbonate is pulverized depolymerization, promptly become nanometer grade calcium carbonate.
In the carburising step in B step, the interpolation time of crystal formation directed agents and crystal formation suppressor factor is for feeding before the purification of carbon dioxide gas or when feeding purification of carbon dioxide gas or feed purification of carbon dioxide gas carbonization mid-term afterwards.
In the B carburising step in step, its carbonization temperature is 35-55 ℃.
In the B carburising step in step, its carbonization temperature is 45 ℃.
In the B carburising step in step, described vitriol is calcium sulfate or zinc sulfate, and described phosphoric acid salt is trisodium phosphate or sodium-metaphosphate.
Normal temperature method nanometer grade calcium carbonate production technique of the present invention owing to selected suitable crystal formation directed agents and crystal formation suppressor factor for use, passivation its susceptibility to carbonization temperature, make that its carbonization temperature can be in the normal temperature scope; Simultaneously, as required, the crystal formation directed agents, the suppressor factor that add different amounts can make the particle diameter of product be controlled at the 20-100 nanometer, and selecting the crystal formation of different crystal formation directed agents and suppressor factor may command product for use is cubes, spherule, mixed crystal type; In addition, abandoned the freezing process in the traditional technology, so, both reduced the investment of refrigerating apparatus, also reduced the energy consumption that the operation because of refrigerating apparatus consumes, thereby, its production cost reduced.
Embodiment:
Below in conjunction with embodiment, the present invention is done further explanation.Following explanation is the mode to give an example, but protection scope of the present invention is not limited thereto.
Embodiment one:
The technical process of present embodiment is:
A, batching: aqua calcis through the suspension separator, is removed impurity, and add quicklime concentration content in the water adjustment solution, become refining aqua calcis 10%, subsequent use;
B, carbonization: subsequent use refining aqua calcis is placed carbonating tower; The dioxide gas that feeds after purifying carries out bubbling carbonizing; And (both proportionings are single-candidate to add the zinc sulfate account for quicklime weight 3% in the refining aqua calcis and trisodium phosphate mixture; Also can be other ratio) as crystal formation directed agents and crystal formation suppressor factor, under the normal temperature scope of 20-65 ℃ of temperature, carry out initial carbonizing treatment (in whole carbonization process, the heat that carburizing reagent produced; The temperature of solution though can raise, but still need not take cooling measure); , the pH value in the solution can stop carbonization when reaching 7.0, the nano-calcium carbonate milk sap after the collection carbonization, and subsequent use; The interpolation time of zinc sulfate and trisodium phosphate is to feed before the purification of carbon dioxide gas;
C, processing: subsequent use nano-calcium carbonate milk sap is heated to 70 degree, adds the StNa that accounts for quicklime weight 2% and carry out surface treatment, become and handle the nano-calcium carbonate mixed solution, subsequent use;
D, dehydration: subsequent use processing nano-calcium carbonate mixed solution is carried out processed (can adopt plate-and-frame filter press or other dehydration equipment), let its water cut reduce to 40%, collect the nano-calcium carbonate filter cake after dewatering, subsequent use;
E, one-level drying: subsequent use nano-calcium carbonate filter cake is carried out the first time dry (adopting duplex drying machine or chain-plate type drying machine), let its water cut reduce to 20%, become dried nano-calcium carbonate just, subsequent use;
F, secondary drying: subsequent use first dried nano-calcium carbonate is carried out redrying handle (can adopt board-like drying machine or flash dryer or other drying plant), let its water cut reduce to below 0.5%, become the work in-process nano-calcium carbonate, subsequent use;
G, depolymerization: subsequent use work in-process nano-calcium carbonate is pulverized depolymerization (can adopt high speed powder mill or other disintegrating apparatus), promptly become nanometer grade calcium carbonate.
The nanometer grade calcium carbonate product that this scheme is produced, through detecting, its crystal formation is a spherule, median size is the 40-80 nanometer.
Embodiment two:
The technical process of present embodiment is:
A, batching: aqua calcis through the suspension separator, is removed impurity, and add quicklime concentration content in the water adjustment solution, become refining aqua calcis 8%, subsequent use;
B, carbonization: subsequent use refining aqua calcis is placed carbonating tower; The dioxide gas that feeds after purifying carries out bubbling carbonizing; And (both proportionings are single-candidate to add the calcium sulfate account for quicklime weight 1% in the refining aqua calcis and ZX-I mixture; Also can be other ratio) as crystal formation directed agents and crystal formation suppressor factor, under the normal temperature scope of 20-65 ℃ of temperature, carry out initial carbonizing treatment (in whole carbonization process, the heat that carburizing reagent produced; The temperature of solution though can raise, but still need not take cooling measure); , the pH value in the solution can stop carbonization when reaching 7.0, the nano-calcium carbonate milk sap after the collection carbonization, and subsequent use; The interpolation time of calcium sulfate and ZX-I is when feeding purification of carbon dioxide gas;
C, processing: subsequent use nano-calcium carbonate milk sap is heated to 70 degree, adds the StNa that accounts for quicklime weight 2% and carry out surface treatment, become and handle the nano-calcium carbonate mixed solution, subsequent use;
D, dehydration: subsequent use processing nano-calcium carbonate mixed solution is carried out processed (can adopt plate-and-frame filter press or other dehydration equipment), let its water cut reduce to 50%, collect the nano-calcium carbonate filter cake after dewatering, subsequent use;
E, one-level drying: subsequent use nano-calcium carbonate filter cake is carried out the first time dry (adopting duplex drying machine or chain-plate type drying machine), let its water cut reduce to 15%, become dried nano-calcium carbonate just, subsequent use;
F, secondary drying: subsequent use first dried nano-calcium carbonate is carried out redrying handle (can adopt board-like drying machine or flash dryer or other drying plant), let its water cut reduce to below 0.5%, become the work in-process nano-calcium carbonate, subsequent use;
G, depolymerization: subsequent use work in-process nano-calcium carbonate is pulverized depolymerization (can adopt high speed powder mill or other disintegrating apparatus), promptly become nanometer grade calcium carbonate.
The nanometer grade calcium carbonate product that this scheme is produced, through detecting, its crystal formation is a mixed crystal shape, median size is the 80-100 nanometer.
Embodiment three:
The technical process of present embodiment is:
A, batching: aqua calcis through the suspension separator, is removed impurity, and add quicklime concentration content in the water adjustment solution, become refining aqua calcis 6%, subsequent use;
B, carbonization: subsequent use refining aqua calcis is placed carbonating tower; The dioxide gas that feeds after purifying carries out bubbling carbonizing; And (both proportionings are single-candidate to add the sodium-metaphosphate account for quicklime weight 1% in the refining aqua calcis and ROHM mixture; Also can be other ratio) as crystal formation directed agents and crystal formation suppressor factor, under the normal temperature scope of 20-65 ℃ of temperature, carry out initial carbonizing treatment (in whole carbonization process, the heat that carburizing reagent produced; The temperature of solution though can raise, but still need not take cooling measure); , the pH value in the solution can stop carbonization when reaching 7.0, the nano-calcium carbonate milk sap after the collection carbonization, and subsequent use: sodium-metaphosphate and polyacrylic interpolation time are the carbonization mid-term after the feeding purification of carbon dioxide gas, that is: the centre in whole carbon period;
C, processing: subsequent use nano-calcium carbonate milk sap is heated to 70 degree, adds the StNa that accounts for quicklime weight 2.5% and carry out surface treatment, become and handle the nano-calcium carbonate mixed solution, subsequent use;
D, dehydration: subsequent use processing nano-calcium carbonate mixed solution is carried out processed (can adopt plate-and-frame filter press or other dehydration equipment), let its water cut reduce to 60%, collect the nano-calcium carbonate filter cake after dewatering, subsequent use;
E, one-level drying: subsequent use nano-calcium carbonate filter cake is carried out the first time dry (adopting duplex drying machine or chain-plate type drying machine), let its water cut reduce to 10%, become dried nano-calcium carbonate just, subsequent use;
F, secondary drying: subsequent use first dried nano-calcium carbonate is carried out redrying handle (can adopt board-like drying machine or flash dryer or other drying plant), let its water cut reduce to below 0.5%, become the work in-process nano-calcium carbonate, subsequent use;
G, depolymerization: subsequent use work in-process nano-calcium carbonate is pulverized depolymerization (can adopt high speed powder mill or other disintegrating apparatus), promptly become nanometer grade calcium carbonate.
The nanometer grade calcium carbonate product that this scheme is produced, through detecting, its crystal formation is a cubes, median size is the 60-80 nanometer.
Use the nanometer grade calcium carbonate that the present invention produces, can be used as the packing material of industries such as plastics industry, rubber industry, coatings industry, paper industry, printing ink industry and sizing agent industry.
Claims (5)
1. normal temperature method nanometer grade calcium carbonate production technique is characterized in that technical process is:
A, batching: aqua calcis through the suspension separator, is removed impurity, and add quicklime concentration content in the water adjustment solution, become refining aqua calcis at 6-10%, subsequent use;
B, carbonization: subsequent use refining aqua calcis is placed carbonating tower; The dioxide gas that feeds after purifying carries out bubbling carbonizing; And add crystal formation directed agents and the crystal formation suppressor factor that accounts for quicklime weight 1-3% in the refining aqua calcis, and under 20-65 ℃ of temperature, carry out carbonizing treatment,, the pH value in the solution can stop carbonization when reaching 6.5-7.5; Nano-calcium carbonate milk sap after the collection carbonization, subsequent use;
Used crystal formation directed agents and crystal formation suppressor factor are that a kind of in vitriol, phosphoric acid, phosphoric acid salt, Hydrocerol A, lactic acid, ROHM, ZX-I, starch, the Mierocrystalline cellulose or two kinds are multiple or whole;
C, processing: subsequent use nano-calcium carbonate milk sap is heated to 60-80 ℃, adds the StNa that accounts for quicklime weight 2-2.5% and carry out surface treatment, become and handle the nano-calcium carbonate mixed solution, subsequent use;
D, dehydration: subsequent use processing nano-calcium carbonate mixed solution is carried out processed, let its water cut reduce to 40-60%, collect the nano-calcium carbonate filter cake after dewatering, subsequent use;
E, one-level drying: subsequent use nano-calcium carbonate filter cake is carried out the drying first time, let its water cut reduce to 10-20%, become dried nano-calcium carbonate just, subsequent use;
F, secondary drying: subsequent use first dried nano-calcium carbonate is carried out redrying handle, let its water cut reduce to below 0.5%, become the work in-process nano-calcium carbonate, subsequent use;
G, depolymerization: subsequent use work in-process nano-calcium carbonate is pulverized depolymerization, promptly become nanometer grade calcium carbonate.
2. normal temperature method nanometer grade calcium carbonate production technique according to claim 1; It is characterized in that: in the B carburising step in step; The interpolation time of crystal formation directed agents and crystal formation suppressor factor is for feeding before the purification of carbon dioxide gas or when feeding purification of carbon dioxide gas or feed the carbonization mid-term after the purification of carbon dioxide gas.
3. normal temperature method nanometer grade calcium carbonate production technique according to claim 1 and 2 is characterized in that: in the B carburising step in step, its carbonization temperature is 35-55 ℃.
4. normal temperature method nanometer grade calcium carbonate production technique according to claim 3 is characterized in that: in the B carburising step in step, its carbonization temperature is 45 ℃.
5. normal temperature method nanometer grade calcium carbonate production technique according to claim 4 is characterized in that: in the B carburising step in step, described vitriol is calcium sulfate or zinc sulfate, and described phosphoric acid salt is trisodium phosphate or sodium-metaphosphate.
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