CN101570343B - Method for preparing nanometer calcium carbonate special for water soluble ink by wet method - Google Patents
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Abstract
The invention relates to a method for preparing nanometer calcium carbonate, in particular to a method for preparing nanometer calcium carbonate special for water soluble ink by a wet method. The method comprises the following steps: calcining and smashing limestone to prepare calcium oxide, classifying the calcium oxide, choosing fine quality calcium oxide to be slaked in a gyratory slaker, be aged twice and carbonized twice to prepare calcium carbonate. The method is characterized in that the calcium oxide undergoes slaking in the gyratory slaker and first aging, is added with a crystal control agent, undergoes second aging after undergoing first bubbling carbonation and is added with a material looseness modifier and a surface treatment agent to carry out second modification. The methodfarthest utilizes the low-grade limestone to prepare the nanometer calcium carbonate product special for water-based ink, with mean grain size of 10-40nm and specific surface of 40-70m<2>/g and enhances the transparency and cohesive force of the ink.
Description
Technical field
The present invention relates to a kind of preparation method of nanometer grade calcium carbonate, relate to a kind of method of utilizing preparing nanometer calcium carbonate special for water soluble ink by wet method specifically.
Technical background
Nano-calcium carbonate is meant the superfine powder of particle diameter less than 100nm, is widely used in fields such as plastics, rubber, glue paste, coating, printing ink, is the functional mineral filler of a kind of novel high-grade.
At present, the technology for preparing ultrafine calcium class inorganic powder in the world is representative with European countries such as the process control technology of Japan and Germany to add auxiliary agent.
Before a kind of kinetics and thermodynamic principles of technical basis calcium carbonate reaction process, the variation of processing parameters such as the temperature by the conditioned reaction process, solid concentration, gas flow, thus reach the purpose of control carburizing reagent speed.According to the different steps in the calcium carbonate crystal process, control its different speed of response, the primary particle size of lime carbonate is reached below the 100nm, and guarantee that the crystal interface growth is complete, have good dispersing property.
A kind of technology in back is to rely on to add various organic or inorganic auxiliary agents, improves CO in carbonation reaction
2Solubleness, thereby improve CO in the liquid phase
3 2-Degree of supersaturation, impel in the crystallisation process nucleus formation speed to accelerate, help the generation of Nano particles of calcium carbonate; Or auxiliary agents such as interpolation inorganic electrolyte, tensio-active agent, " steric effect " by " electrostatic double layer " and organic adsorption layer disperses calcium carbonate crystal, suppress crystal and grow up, finally form the uniform nanoparticle of size distribution, and have good dispersing property.
Domestic enterprise adopts a kind of technology in back more substantially based on these two kinds of technology.There is bigger difference in two kinds of technology on technology, preceding a kind of technology is comparatively complicated, and facility investment is big, and production cost is low, and quality product is comparatively stable; A kind of technology in back is simple, increases a certain amount of auxiliary agent cost, the difficult control of quality.Along with the continuous development of lime carbonate industry, two kinds of technology will constantly merge, and carbonization technique has more diversity, and the function of product also can be segmented thereupon, and kind will be more.
Along with the continuous change and progress of calcium carbonate applications industry, function to nano-calcium carbonate is had higher requirement, impel the main content of nano-calcium carbonate also changing gradually, people have risen to new height to the understanding of nano-calcium carbonate simultaneously, progressively it are considered as a kind of composite type modified material and are applied.High-grade filler during nano-calcium carbonate is produced as oil-based ink has excellent dispersiveness, the transparency, gloss in printing ink, ink absorption that in press shows and high drying property make it become one of main stuffing in the present oil-based ink production.
Oil-based ink contains a large amount of organic solvents, human body and atmospheric environment are caused great infringement, and each country all makes laws and rules, the quantity discharged of restriction VOC, in order to meet the requirement of VOC law, a lot of companies all require to adopt water color ink as printing-ink.Water color ink, it is mainly processed through multiple grinding by water soluble resin, pigment dyestuff, solvent and relevant auxiliary agent.Because it is that water replaces accounting for 30～70 poisonous organic solvent in traditional printing ink, makes no longer to contain volatile organic solvent in the printing ink.In printing process, workers'health is had no adverse effects, also pollution-free to atmospheric environment, eliminated the inflammable and explosive hidden danger in working space, improved security.More and more be subjected to printing the favor on boundary in the world, development rapidly.Disabled at the aromatic solvent of some similar toluene of developed country in food packaging ink;
Constantly develop the more product of compliance with environmental protection requirements---use printing ink replaces solvent type ink to become the inexorable trend of Printing Industry Development.Aqueous, environmental protective printing ink in successful Application at intaglio printing press, offset press, screen process press.
The present nano-calcium carbonate of producing, the restriction of reasons such as condition difference when synthetic and surface treatment, can only be used for traditional solvent type ink, when being used for water color ink, because intermiscibility is bad, whiteness is not enough, bubbles, shortcomings such as easy migration, the nano-calcium carbonate of therefore developing a kind of water color ink special use has crucial meaning and economic benefit.
Summary of the invention
The objective of the invention is to utilize low-grade limestone, adopt wet-process activation to prepare particle diameter in the 10-40nm scope, have controlled mean sizes and distribution thereof, the method for superfine function calcium class inorganic powder nano-particle material.
The technical solution adopted in the present invention is:
1, calcining and broken: low-grade limestone is calcined with broken, made calcium oxide;
2, sizing screening: the poor slightly calcium oxide of a part of quality grinds into middle-grade calcium oxide product by high speed kneader or ring roller, another part calcium oxide of fine quality then enters the production that next process carries out calcium hydroxide, lime carbonate, then is used for the production of green building material air-entrained concrete building block at last for second-rate calcium oxide;
3, get calcium oxide of fine quality through being incubated the digestion of revolution digestion machine, the first time ageing, add crystal control agent, after carrying out the bubbling carbonizing first time, again through the ageing second time and carbonization for the second time, add material loosening conditioning agent and surface treatment agent and carry out secondary modification, through filter-press dehydration, filter cake directly uses to the user again, or uses to the user through secondary drying, pulverizing, packing.
Of the present invention Wingdale is calcined, adopted environment-friendly and energy-efficient steel shaft kiln that low-grade limestone is calcined, calcining temperature is controlled between 950～1050 ℃, calcination time 18～30 hours.
Digestion lime of the present invention, its process is after calcining, and the calcium oxide of fine quality of sizing screening is broken into fritter, its size is in 100mm, be sent to lime slaking machine by travelling belt, used water temp is controlled between 60～70 ℃ during ashing, and the consumption of water is 5～7 times of lime quality.Once slurry contains the thick slag of part, and calcium hydroxide concentration adopts the method for spinning liquid separation and vibration screening to remove indigested living calcined lime, silicon-dioxide, magnesium oxide and other impurity between 8～10%, obtains refining.
The ageing first time of the present invention is meant thick slurry through removing the refining that obtains behind the impurity, and the waste heat when utilizing ashing is incubated ageing, and the aged time is 24～48 hours, then makes by converting water that calcium hydroxide concentration drops to 6～8% in the refining, makes ripe slurry.
Described crystal control agent is: carbohydrate, sulfuric acid based, phosphoric acid class, acetate class or lemon acids.Wherein carbohydrate refers to one or more mixtures in sucrose, lactose, beet sugar, fructose, the glucose; Sulfuric acid based refers to sulfuric acid, Tai-Ace S 150 or sodium sulfate; The phosphoric acid class refers to ammonium phosphate, phosphoric acid, sodium phosphate; The acetate class refers to acetate or sodium acetate; The lemon acids refers to: citric acid, trisodium citrate or Trisodium Citrate.
Described crystal control agent is most preferably: beet sugar, sodium sulfate, sodium phosphate or trisodium citrate.The add-on of crystal control agent is 0.5～3.0% of a lime carbonate solid content.
Described first time, bubbling carbonizing was meant that regulating the carbonization starting temperature is 17-25 ℃, feeds CO with the aged refining of process insulation
2Gas, CO
2The concentration of gas is 25～35%, and the air compressor gaseous tension is a 1.0-1.5 normal atmosphere, and carbonization is to stop carbonization at 8～9 o'clock to slurry pH value, and aeration time 30-60 minute is through stirring bubbling carbonizing intermittence, obtaining ripe slurry.
The ageing second time of the present invention is meant that ripe slurry is introduced ageing tank carries out 20～80 hours ageing, discharge section water after this, and the concentration of regulating the slurry of nano-calcium carbonate is 12-14%.
The described carbonization second time is meant discharge section water after the ageing second time, and the concentration of regulating the slurry of nano-calcium carbonate is 12-14%, feeds CO
2Gas carries out the carbonization second time, CO
2Gas concentration is 25～35%, and carbonization stops carbonization, aeration time 10-20 minute to nano-calcium carbonate slurry pH≤7 o'clock.This method is except utilizing CO
2Agitating outside the effect of rolling of gas also relies on the blade of agitator to CO
2Gas disperses to shear.Because gas is evenly distributed in reaction system, and bubble is less, is beneficial to absorption, so speed of response is very fast.
In the described secondary modification, modification for the first time is meant at first squeezes into special-purpose stirred pot with ageing after-ripening slurry by stock pump, after being heated to 50～80 ℃, add and dissolved the material loosening conditioning agent, the amount that adds is respectively 1.0～3.0% of lime carbonate solid content in the ripe slurry, modification time 15～30 minutes.
Described material loosening conditioning agent is meant one or more mixture of sodium polyacrylate, polyol, polyphosphoric acid salt, sodium polyacrylate is meant the acrylic copolymer of molecular weight at 3000-8000, and polyol is meant tartrate, amino acid, L-glutamic acid, citric acid or polysaccharide; Polyphosphoric acid salt is meant Sodium hexametaphosphate 99, tripoly phosphate sodium STPP or trisodium phosphate.
In the described secondary modification, modify for the second time and be meant after the first time, modification was finished, add surface-modifying agent, the amount of adding be in the ripe slurry lime carbonate solid content 2.0～3.5%, modification time 25～40 minutes.Surface-modifying agent is meant a kind of of cats product, water-base resin or chelating type aqueous titanic acid ester coupling agent or any multiple mixture.
Described cats product refers to: Trimethyllaurylammonium bromide, cetyl trimethylammonium bromide, octadecyl trimethylammonium bromide, Dodecyl trimethyl ammonium chloride, palmityl trimethyl ammonium chloride or octadecyl trimethyl ammonium chloride.Water-base resin refers to: one or both mixtures in water-soluble rosin modified resin, the water-borne acrylic resin.Chelating type aqueous titanic acid ester class coupling agent refers to titanate coupling agent (CT-54), hydramine alkoxyl group titanate coupling agent (TNS), hydramine lipid acid titanate coupling agent (TNF) titanate coupling agent.
Slurries filtration after coating is directly used to the user to water content 40%-50%, or will use to the user after filter cake drying, pulverizing, classification, the packing.
Drying of the present invention is meant ripe slurry through the pressure filter press filtration, adopts two blade dryers to add the drying means of pan dryer two-stage series connection again.This method is in dry mass that guarantees product and dry stability, and is less to performance impacts such as product whiteness, activation rates, improved The comprehensive performance.
Adopt the nano-calcium carbonate of method preparation of the present invention, its salient features is as follows:
Description of drawings
Fig. 1 is the TEM photo of nano-calcium carbonate of the present invention.
Embodiment
By the following examples the concrete embodiment of the present invention is narrated, but embodiment does not limit protection scope of the present invention.
Embodiment 1
Wingdale is crushed to 30 * 100mm size through jaw crusher, be sent to shaft kiln liftout bucket by travelling belt, adopt environment-friendly and energy-efficient steel shaft kiln that low-grade limestone is calcined, calcining temperature is controlled between 950～1050 ℃, calcination time 18～30 hours.
Lime after the calcining sieves, and chooses fat lime and carries out entering the digestion machine after the fragmentation and carry out lime slaking.The temperature of digestion lime water is controlled at 65 ℃, and consumption is 7 times of lime quality.Lime white contains the thick slag of part, and calcium hydroxide concentration is 13%, adopts spinning liquid to separate and the method for vibration screening is removed other impurity such as indigested living calcined lime and silicon-dioxide, magnesium oxide, obtains refining.
The refining that makes, the waste heat when utilizing digestion lime are incubated places the ageing processing.Through ageing in 24 hours, add the water adjusting and make the concentration of calcium hydroxide slurry drop to 6%, add crystal control agent beet sugar, be incorporated as 0.8% of weight of calcium carbonate, by recirculated cooling water slurry temperature is reduced to 20 ℃ simultaneously.Transfer intermittence that living stock pump after the dense temperature adjustment goes into to have agitator in the bubbling carbonizing reactor, the volume of reactor is 15m
3, CO
2The concentration of gas is 32%, and the air compressor gaseous tension is 1.5 normal atmosphere, and carbonization is 8 o'clock to pH, stops carbonization, and aeration time 45 minutes obtains the ripe slurry of nano-calcium carbonate.
The ripe stock pump of carbonization is gone into the ageing pond, and after ageing in 20 hours, PH rises to 10.8 again, feeds CO
2Gas, carbonization is to pH=6.8, stop carbonization, squeeze into special-purpose stirred pot with stock pump, be heated to 50 ℃ after, add the dissolved sodium polyacrylate, its total amount be in the ripe slurry lime carbonate solid content 1.2%, stirred 20 minutes, and added lime carbonate solid content 3% octadecyl trimethyl ammonium chloride again and carry out secondary surface preparation, stir and stop after 35 minutes.
Through the pressure filter press filtration, the drying process by two blade dryers and pan dryer two-stage series connection carries out drying again through the ripe slurry after the secondary modification, and dried lime carbonate promptly gets the Nano calcium carbonate dedicated product of water color ink after pulverizing, classification, packing.
This product median size is 10-20nm, sees accompanying drawing 1, and specific surface area is greater than 60m
2/ g, and do not have agglomeration.With 4
#Stand linseed oil is made into test specimens, good luster, and the transparency height, degree of mobilization 24mm, product performance of the present invention are very excellent, and adhesiveproperties is good, is applicable to high-grade aqueous transparent printing ink.
Implementation column 2
The preparation of lime refining is identical with example 1, the refining that makes was through ageing in 48 hours, add water convert the slurry make calcium hydroxide concentration drop to 7%, add crystal control agent sodium sulfate and trisodium citrate, add-on is respectively 1% and 0.6% of weight of calcium carbonate, by recirculated cooling water slurry temperature is reduced to 18 ℃ simultaneously.Transfer intermittence that living stock pump after the dense temperature adjustment goes into to have agitator in the bubbling carbonizing reactor, the volume of reactor is 10m
3, CO
2The concentration of gas is 28%, and the air compressor gaseous tension is 1.5 normal atmosphere, and carbonization is 8～9 o'clock to pH, stops carbonization, aeration time 30 minutes.
Carbonization after-ripening stock pump is gone into the ageing pond, ageing 40 hours, and pH is elevated to 11.3, feeds CO
2Gas, carbonization pump into special-purpose stirred pot to pH=6.8, be heated to 40 ℃ after, add the dissolved Sodium hexametaphosphate 99, its total amount be in the ripe slurry lime carbonate solid content 1.0%.Stir after 15 minutes, add lime carbonate solid content 3.5% water-soluble rosin modified resin again and carry out secondary surface preparation, stir and stop after 45 minutes.
Through the pressure filter press filtration, the drying process by two blade dryers and pan dryer two-stage series connection carries out drying again through the ripe slurry after the secondary modification, and dried lime carbonate promptly gets the Nano calcium carbonate dedicated product of water color ink after pulverizing, classification, packing.
This product median size is 10-30nm, and specific surface area is greater than 50m
2/ g, and do not have agglomeration.With 4
#Stand linseed oil is made into test specimens, good luster, and the transparency height, degree of mobilization 26mm, adhesiveproperties is good, is applicable to high-grade aqueous transparent printing ink.
Implementation column 3
The preparation of lime refining is identical with example 1, the refining that makes was through ageing in 36 hours, add water convert the slurry make calcium hydroxide concentration drop to 8%, add crystal control agent tertiary sodium phosphate sodium and citric acid, add-on is respectively 0.5% and 1.0% of weight of calcium carbonate, by recirculated cooling water slurry temperature is reduced to 19 ℃ simultaneously.Transfer intermittence that living stock pump after the dense temperature adjustment goes into to have agitator in the bubbling carbonizing reactor, the volume of reactor is 20m
3, CO
2The concentration of gas is 30%, and the air compressor gaseous tension is 1.5 normal atmosphere, and carbonization is 9 o'clock to pH, stops carbonization, and aeration time is 55 minutes.
Carbonization after-ripening stock pump is gone into the ageing pond, ageing 30 hours, and pH is elevated to 11.2, feeds CO
2Gas, carbonization pump into special-purpose stirred pot to pH=6.8, be heated to 40 ℃ after, add dissolved tartrate, its total amount be in the ripe slurry lime carbonate solid content 1.2%.Stir after 15 minutes, add lime carbonate solid content 2.5% water-soluble rosin modified resin again and 1.0% hydramine alkoxyl group titanate coupling agent carries out secondary surface preparation, after 45 minutes, stop to stir.
Through the program control pressure filter filter-press dehydration of barrier film, water content is that 48% filter cake is the Nano calcium carbonate dedicated product of water color ink to user's use directly after the press filtration through the ripe slurry after the secondary modification.
This product median size is 20-40nm, and specific surface area is greater than 40m
2/ g, and do not have agglomeration.With 4
#Stand linseed oil is made into test specimens, good luster, and the transparency height, degree of mobilization 29mm, adhesiveproperties is good, is applicable to high-grade aqueous transparent printing ink.
Claims (3)
1. a wet method prepares the Nano calcium carbonate dedicated method of water color ink, be that Wingdale is calcined with broken, make calcium oxide, and carry out sizing screening, choose calcium oxide of fine quality through the digestion of revolution digestion machine lime, secondary ageing and secondary carbonization, make lime carbonate, it is characterized in that calcium oxide is through being incubated the digestion of revolution digestion machine, the first time ageing, add crystal control agent, after carrying out the bubbling carbonizing first time, through the ageing second time and carbonization for the second time, add material loosening conditioning agent and surface treatment agent and carry out secondary modification again; Slurries are pressed into filter cake and directly use to the user, or use to the user through secondary drying, pulverizing, packing again through filter-press dehydration;
Be incubated ageing the described first time and be meant thick slurry through removing the refining that obtains behind the impurity, the waste heat when utilizing ashing is incubated ageing, and the aged time is 24～48 hours, then makes by converting water that calcium hydroxide concentration drops to 6～8% in the refining;
Described first time, bubbling carbonizing was meant the aged refining of process, and regulating the carbonization starting temperature is 17-25 ℃, fed CO
2Gas, CO
2The concentration of gas is 25～35%, and carbonization is to stop carbonization at 8～9 o'clock to slurry pH value, and aeration time is 30-60 minute, is through stirring carbonization intermittence, obtaining ripe slurry;
The described ageing second time is meant introduces ageing tank with ripe slurry, carries out 20～80 hours ageing;
The described carbonization second time is meant discharge section water after the ageing second time, and the concentration of regulating the slurry of nano-calcium carbonate is 12-14%, feeds CO
2Gas, CO
2Gas concentration is 25～35%, and pH value≤7 of control nano-calcium carbonate slurry o'clock stop carbonization, aeration time 10-20 minute;
In the described secondary modification, modification for the first time is meant at first squeezes into special-purpose stirred pot with ageing after-ripening slurry by stock pump, after being heated to 50～80 ℃, add and dissolved good material loosening conditioning agent, the amount that adds is respectively 1.0～3.0% of lime carbonate solid content in the ripe slurry, and churning time is 15～30 minutes;
In the described secondary modification, modify for the second time be meant modify for the first time finish after, add surface treatment agent, the amount of adding be in the ripe slurry lime carbonate solid content 2.0～3.5%, churning time is 25～40 minutes;
Described filter cake is meant that slurries are again through the program control pressure filter filter-press dehydration of barrier film, press filtration to the filter cake of water content 40%-50% directly uses to the user, or the ripe slurry after the activation is through the pressure filter filter-press dehydration, drying process by two blade dryers and pan dryer two-stage series connection carries out drying again, and dried powder promptly gets the Nano calcium carbonate dedicated product of water color ink after pulverizing, classification, packing;
Described crystal control agent is: the carbohydrate of one or more mixtures in sucrose, lactose, beet sugar, fructose, the glucose; The sulfuric acid based of sulfuric acid, Tai-Ace S 150 or sodium sulfate; The phosphoric acid class of ammonium phosphate, phosphoric acid, sodium phosphate; The acetate class of acetate or sodium acetate; The lemon acids of citric acid or Trisodium Citrate, add-on are 0.5～3.0% of weight of calcium carbonate;
Described material loosening conditioning agent is meant one or more mixture of sodium polyacrylate, polyol, polyphosphoric acid salt, wherein sodium polyacrylate is meant the acrylic copolymer of molecular weight at 3000-8000, and polyol is meant tartrate or polysaccharide; Polyphosphoric acid salt is meant Sodium hexametaphosphate 99, tripoly phosphate sodium STPP or trisodium phosphate;
Described surface treatment agent agent is meant a kind of or any multiple mixture of cats product, water-base resin, chelating type aqueous titanic acid ester coupling agent;
Described water-base resin is meant one or both mixtures in water-soluble rosin modified resin, the water-borne acrylic resin.
2. wet method according to claim 1 prepares the Nano calcium carbonate dedicated method of water color ink, it is characterized in that cats product is meant Trimethyllaurylammonium bromide, cetyl trimethylammonium bromide, octadecyl trimethylammonium bromide, Dodecyl trimethyl ammonium chloride, palmityl trimethyl ammonium chloride or octadecyl trimethyl ammonium chloride.
3. wet method according to claim 1 prepares the Nano calcium carbonate dedicated method of water color ink, it is characterized in that chelating type aqueous titanic acid ester class coupling agent is meant titanate coupling agent, hydramine alkoxyl group titanate coupling agent, hydramine lipid acid titanate coupling agent.
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2009
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103693668A (en) * | 2013-11-28 | 2014-04-02 | 广西华纳新材料科技有限公司 | Granular fine calcium carbonate and preparation method thereof |
| CN103693668B (en) * | 2013-11-28 | 2015-09-16 | 广西华纳新材料科技有限公司 | A kind of Granular fine calcium carbonate and preparation method thereof |
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| CN101570343A (en) | 2009-11-04 |
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