CN103693667B - A kind of Rodlike light calcium carbonate and preparation method thereof - Google Patents
A kind of Rodlike light calcium carbonate and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of Rodlike light calcium carbonate and preparation method thereof, the average minor axis of its primary particle of this Rodlike light calcium carbonate is 0.1-0.2 μm, the average major diameter of primary particle is 0.3-2.0 μm, long-width ratio is 3-20 and shape is mainly bar-shaped and/or cylindric or needle-like.Its preparation method is: in using, calcined lime and hot water digest in the ratio of 1:4-10, then cross 60-120 order vibratory screening apparatus and remove impurity by wet cyclone, add compound crystal control agent after obtained refining to stir, in adjusting life to starch, calcium hydroxide content is at 6-12%, passing into kiln gas carbonization to pH is that 6.5-7 stops carbonization, and reaction solution is obtained light calcium carbonate after dehydration, drying, pulverizing, screening.Rodlike light calcium carbonate of the present invention, as a kind of filler, has the features such as intensity is high, modulus is high, heat-resisting heat-proof quality is good, and its preparation technology is simple, and energy consumption is low, reduces production cost, has good economic benefit and social benefit.
Description
Technical field
The present invention relates to calcium carbonate technical field, especially relate to a kind of Rodlike light calcium carbonate and preparation method thereof.
Background technology
Calcium carbonate is important inorganic chemical product, and conventional calcium carbonate size distribution, between tens nanometers are to tens microns, is commonly used for filler.Be widely used in the operations such as rubber, coating, papermaking and ink, ordinary calcium carbonate is raw material usually with Wingdale, obtains unslaked lime through calcination, and then unslaked lime adds water digestion absorbing carbon dioxide carries out carbonization, finally dewater, dry, pulverize and obtain product.Calcium carbonate production development has developed fine calcium carbonate and the modified products thereof such as cubes, spindle body, spherical, chain shape, chain, whisker or threadiness, sheet, needle-like to today.Rodlike light calcium carbonate and needle-like, whisker or fibrous calcium carbonate have certain similarity, but also have the difference of essence.Spindle body light calcium carbonate is the larger spindle body in centre pointed at both ends, and the shape of Rodlike light calcium carbonate is more longer a little than spindle body light calcium carbonate, for two and centre of a size bar-shaped.
The single crystal filamentary material that calcium carbonate crystal whisker and wire/fiber ring calcium carbonate are diameters is zero point several microns to several microns, length is tens microns.The preparation method of calcium carbonate whisker has a variety of, has a lot of expert and scholar to be prepared by diverse ways in recent years.Application number 200710129524.0 can be retrieved on the net in State Intellectual Property Office of the People's Republic of China to introduce " a kind of method preparing calcium carbonate crystal whisker ", application number 200410022834.9 is introduced " a kind of preparation method of Aragonite Style Calcium Carbonate Whiskers ", application number 201110098679.9 is introduced " a kind of method preparing calcium carbonate crystal whisker ", application number 031342878.6 is introduced " preparation technology of calcium carbonate crystal whisker ", application number 200910059936.0 is introduced " preparation method of the calcium carbonate crystal whisker of morphology controllable ", application number 200810228368.8 " a kind of epoxy propane saponified wastewater produces the method for calcium carbonate crystal whisker ", application number 201010280862.6 is introduced " preparation method of high length-diameter ratio calcium carbonate crystal whisker ", application number 201210490750.2 is introduced " giving calcium carbonate crystal whisker synthesis and the modification integral method of sol-gel method ", application number 201310284604.9 " a kind of production method of calcium carbonate crystal whisker ".Needle-like or aciculiform calcium carbonate are the one of nanometer grade calcium carbonate, also have many experts studying relevant preparation method with scholar in recent years.
Application number is 200710139563.9 introductions " a kind of preparation methods of styliform nano calcium carbonate ".The method without refrigerator under the condition of comparatively high temps and higher lime milk concentration, after a certain amount of unslaked lime and hot water are mixed in proportion, remove the gred after filtration, before carbonization, its solution is jumped to desired concn and temperature, add crystal-directing-agent, move into after stirring in carbonization reactor and carry out carburizing reagent, finally reaction solution is obtained styliform nano calcium carbonate after the operations such as dehydration, washing, drying, surface treatment, pulverizing, screening.The aciculiform calcium carbonate that the method obtains is nanometer grade calcium carbonate.
Summary of the invention
The invention provides a kind of favorable dispersity, major diameter and minor axis controlled, suitability for industrialized production, technique is simple, energy consumption is low Rodlike light calcium carbonate and preparation method thereof can be realized under high-temperature high concentration.
To achieve these goals, present invention employs following technical scheme:
A kind of Rodlike light calcium carbonate, the average minor axis of its primary particle is 0.1-0.2 μm, the average major diameter of primary particle is 0.3-2.0 μm, long-width ratio is 3-20 and shape is mainly bar-shaped and/or cylindric or needle-like.
A preparation method for Rodlike light calcium carbonate, it comprises the following steps:
(1) digest: the ratio being 1:4-10 by mass percentage by middle calcined lime and hot water is poured into rotate in digestion machine and carried out digestion reaction, obtained calcium hydroxide emulsion carries out filter cleaner through 60-120 object vibratory screening apparatus, remove the gred further through wet cyclone again, be placed in storage tank for subsequent use after obtaining calcium hydroxide emulsion;
(2) mix: be transferred to 6-12% thickening in groove the weight concentration added water calcium hydroxide emulsion, add compound crystal control agent, the weight of the compound crystal control agent wherein added is the 0.1-2.0% of calcium hydroxide weight, stirs 25-35 minute, makes it fully mix;
(3) carbonization: calcium hydroxide emulsion obtained in step (2) is squeezed into carbonization reactor with pump, opens kiln gas valve, passes into containing CO
2volumetric concentration is that the kiln gas of 15-100% carries out carburizing reagent, the feeding temperature of calcium hydroxide emulsion is 25-70 DEG C, in carbonation reaction, reaction self-heat generation, kiln gas can take away partial heat by emulsion, carbonation reaction temperature is between 30-70 DEG C, and carbonization closes kiln gas valve to during reaction solution pH=6.5-7, stopped reaction;
(3) dehydrate: reaction solution is obtained being mainly Rodlike light calcium carbonate after the normal process steps of dehydration, drying, pulverizing, screening.
Above-described compound crystal control agent is made up of three kinds of components, and the first component is solubility magnesium salts, and the second component is polyvinyl alcohol, and the third component is phosphoric acid or its esters, and wherein three kinds of component weight ratios are: 1.0: 0.8-2.5: 0.2-2.0.
The weight concentration that above-described carburizing reagent controls calcium hydroxide emulsion is 12%, and kiln gas is containing CO
2volumetric concentration is 30%.
Above-described carbonization reactor is with whipping appts or the intermittent type bubbling carbonizing tower without whipping appts.
Compared to prior art, the present invention has following advantage and positively effect:
1, Rodlike light calcium carbonate of the present invention is micron order calcium carbonate, bar-shaped calcium carbonate is diameter zero point several microns to several microns, the calcium carbonate of length to be several microns of shapes be bar-shaped, cylindrical or similar aciculiform, bar-shaped calcium carbonate has the shape of aciculiform calcium carbonate, but thicker than needle-like nano calcium carbonate, there is the much the same minor axis major diameter of calcium carbonate crystal whisker to be but far shorter than calcium carbonate crystal whisker.
2, Rodlike light calcium carbonate of the present invention is as a kind of filler, has the features such as intensity is high, modulus is high, heat-resisting heat-proof quality is good, is applicable to the fields such as plastics, papermaking, the manufacture of electric component, the manufacture of best bright finish structure unit.
3, the major diameter of Rodlike light calcium carbonate of the present invention and minor axis controlled, can realize suitability for industrialized production under high-temperature high concentration, technique is simple, and energy consumption is low, reduces production cost, has good economic benefit and social benefit.
Accompanying drawing explanation
Fig. 1 is that Rodlike light calcium carbonate product prepared by embodiment 1 detects analysis chart through scanning electron microscope.
Fig. 2 is that Rodlike light calcium carbonate product prepared by embodiment 2 detects analysis chart through scanning electron microscope.
Embodiment
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention are not limited thereto.
Embodiment 1:
A kind of light calcium carbonate, the average minor axis of its primary particle is 0.1-0.2 μm, the average major diameter of primary particle is 0.4-1.0 μm, long-width ratio is 4-10 and shape is bar-shaped.It comprises the following steps and is prepared from:
(1) digest: calcium carbonate content is greater than calcined lime in the limestone calcination one-tenth of 97.0%, the middle calcined lime burnt till and hot water be by mass percentage 1: 5 ratio pour into rotate in digestion machine and carry out digestion reaction, obtained calcium hydroxide emulsion carries out filter cleaner through 80 object vibratory screening apparatuss, remove the gred further through wet cyclone again, be placed in storage tank for subsequent use after obtaining calcium hydroxide emulsion;
(2) mix: according to magnesium chloride: polyvinyl alcohol: the weight ratio of phosphoric acid is 1.0: 2.0: 0.8 configuration crystal control agents; Be transferred to 12 thickening in groove the weight concentration added water calcium hydroxide emulsion obtained in step (1), add the compound crystal control agent prepared, the weight of the compound crystal control agent wherein added is 1.5% of calcium hydroxide weight, stir 30 minutes, make it fully mix;
(3) carbonization: with pump, calcium hydroxide emulsion obtained in step (2) is squeezed into carbonization reactor, described carbonization reactor is with whipping appts; Open kiln gas valve, pass into containing CO
2volumetric concentration is 30%, through purifying and being cooled to the kiln gas of less than 35 DEG C to carry out carburizing reagent, the feeding temperature of calcium hydroxide emulsion is 40 DEG C, in carbonation reaction, reaction self-heat generation, kiln gas can take away partial heat by emulsion, carbonation reaction temperature is between 35-70 DEG C, and carbonization closes kiln gas valve to during reaction solution pH=6.5-7, stopped reaction;
(4) dehydrate: by ripe for reaction solution suction slurry storage tank, after depositing slurry amount and meeting continuous seepage, take out slurry obtain filter cake by centrifugal filter dewatering and filtering, Belt Conveying filter cake carries out drying to rotary furnace drying stove, the oven dry material obtained sends into pulverizer by rotary conveyor, after pulverizing selection by winnowing sieve classification, obtain Rodlike light calcium carbonate finished product, product detects through scanning electron microscope and analyzes as shown in Figure 1.
Embodiment 2:
A kind of light calcium carbonate, the average minor axis of its primary particle is 0.1-0.2 μm, the average major diameter of primary particle is 0.8-1.5 μm, long-width ratio is 8-15 and shape is bar-shaped.It comprises the following steps and is prepared from:
(1) digest: calcium carbonate content is greater than calcined lime in the limestone calcination one-tenth of 97.0%, the middle calcined lime burnt till and hot water be by mass percentage 1: 6 ratio pour into rotate in digestion machine and carry out digestion reaction, obtained calcium hydroxide emulsion carries out filter cleaner through 100 object vibratory screening apparatuss, remove the gred further through wet cyclone again, be placed in storage tank for subsequent use after obtaining calcium hydroxide emulsion;
(2) mix: according to magnesium sulfate: polyvinyl alcohol: phosphoric acid=1: 1.8: 1.0 configuration crystal control agents; Be transferred to 8% thickening in groove the weight concentration added water calcium hydroxide emulsion obtained in step (1), add the compound crystal control agent prepared, the weight of the compound crystal control agent wherein added is 1.0% of calcium hydroxide weight, stir 30 minutes, make it fully mix;
(3) carbonization: with pump, calcium hydroxide emulsion obtained in step (2) is squeezed into carbonization reactor, described carbonization reactor is the intermittent type bubbling carbonizing tower without whipping appts; Open kiln gas valve, pass into containing CO
2volumetric concentration is 40% through purifying and being cooled to the kiln gas of less than 35 DEG C to carry out carburizing reagent, the feeding temperature of calcium hydroxide emulsion is 60 DEG C, in carbonation reaction, reaction self-heat generation, kiln gas can take away partial heat by emulsion, carbonation reaction temperature is between 50-70 DEG C, and carbonization closes kiln gas valve to during reaction solution pH=6.5-7, stopped reaction;
(4) dehydrate: by ripe for reaction solution suction slurry storage tank, after depositing slurry amount and meeting continuous seepage, take out slurry obtain filter cake by centrifugal filter dewatering and filtering, Belt Conveying filter cake carries out drying to rotary furnace drying stove, the oven dry material obtained sends into pulverizer by rotary conveyor, after pulverizing selection by winnowing sieve classification, obtain Rodlike light calcium carbonate finished product, product detects through scanning electron microscope and analyzes as shown in Figure 2.
Embodiment 3:
A kind of Rodlike light calcium carbonate, the average minor axis of its primary particle is 0.1-0.2 μm, the average major diameter of primary particle is 0.3-1.0 μm, long-width ratio is 3-10 and shape is mainly bar-shaped and cylindric or needle-like.It comprises the following steps and is prepared from:
(1) digest: calcium carbonate content is greater than calcined lime in the limestone calcination one-tenth of 97.0%, the middle calcined lime burnt till and hot water be by mass percentage 1: 4 ratio pour into rotate in digestion machine and carry out digestion reaction, obtained calcium hydroxide emulsion carries out filter cleaner through 60 object vibratory screening apparatuss, remove the gred further through wet cyclone again, be placed in storage tank for subsequent use after obtaining calcium hydroxide emulsion;
(2) mix: according to magnesium chloride: polyvinyl alcohol: the weight ratio of sodium hydrogen phosphate is 1.0: 0.8: 0.2 configuration crystal control agents; Be transferred to 6% thickening in groove the weight concentration added water calcium hydroxide emulsion obtained in step (1), add the compound crystal control agent prepared, the weight of the compound crystal control agent wherein added is 0.1 of calcium hydroxide weight, stir 25 minutes, make it fully mix;
(3) carbonization: with pump, calcium hydroxide emulsion obtained in step (2) is squeezed into carbonization reactor, described carbonization reactor is with whipping appts; Open kiln gas valve, pass into containing CO
2volumetric concentration is 15%, through purifying and being cooled to the kiln gas of less than 35 DEG C to carry out carburizing reagent, the feeding temperature of calcium hydroxide emulsion is 25 DEG C, in carbonation reaction, reaction self-heat generation, kiln gas can take away partial heat by emulsion, carbonation reaction temperature is between 30-70 DEG C, and carbonization closes kiln gas valve to during reaction solution pH=6.5-7, stopped reaction;
(4) dehydrate: by ripe for reaction solution suction slurry storage tank, after depositing slurry amount and meeting continuous seepage, take out slurry obtain filter cake by centrifugal filter dewatering and filtering, Belt Conveying filter cake carries out drying to rotary furnace drying stove, the oven dry material obtained sends into pulverizer by rotary conveyor, obtains being mainly Rodlike light calcium carbonate finished product after pulverizing selection by winnowing sieve classification.
Embodiment 4:
A kind of light calcium carbonate, the average minor axis of its primary particle is 0.1-0.2 μm, the average major diameter of primary particle is 1.0-2.0 μm, long-width ratio is 10-20 and shape is mainly bar-shaped or cylindric or needle-like.It comprises the following steps and is prepared from:
(1) digest: calcium carbonate content is greater than calcined lime in the limestone calcination one-tenth of 97.0%, the middle calcined lime burnt till and hot water be by mass percentage 1: 10 ratio pour into rotate in digestion machine and carry out digestion reaction, obtained calcium hydroxide emulsion carries out filter cleaner through 120 object vibratory screening apparatuss, remove the gred further through wet cyclone again, be placed in storage tank for subsequent use after obtaining calcium hydroxide emulsion;
(2) mix: according to magnesium chloride: polyvinyl alcohol: the weight ratio of potassium hydrogen phosphate is 1.0: 2.5: 2.0 configuration crystal control agents; Be transferred to 12% thickening in groove the weight concentration added water calcium hydroxide emulsion obtained in step (1), add the compound crystal control agent prepared, the weight of the compound crystal control agent wherein added is 2.0% of calcium hydroxide weight, stir 35 minutes, make it fully mix;
(3) carbonization: with pump, calcium hydroxide emulsion obtained in step (2) is squeezed into carbonization reactor, described carbonization reactor is the intermittent type bubbling carbonizing tower without whipping appts; Open kiln gas valve, pass into containing CO
2volumetric concentration is 100%, through purifying and being cooled to the kiln gas of less than 35 DEG C to carry out carburizing reagent, the feeding temperature of calcium hydroxide emulsion is 70 DEG C, in carbonation reaction, reaction self-heat generation, kiln gas can take away partial heat by emulsion, carbonation reaction temperature is between 50-70 DEG C, and carbonization closes kiln gas valve to during reaction solution pH=6.5-7, stopped reaction;
(4) dehydrate: by ripe for reaction solution suction slurry storage tank, after depositing slurry amount and meeting continuous seepage, take out slurry obtain filter cake by centrifugal filter dewatering and filtering, Belt Conveying filter cake carries out drying to rotary furnace drying stove, the oven dry material obtained sends into pulverizer by rotary conveyor, obtains being mainly bar-shaped calcium carbonate finished product after pulverizing selection by winnowing sieve classification.
Claims (4)
1. a preparation method for Rodlike light calcium carbonate, is characterized in that: it comprises the following steps:
(1) digest: the ratio being 1:4-10 by mass percentage by middle calcined lime and hot water is poured into rotate in digestion machine and carried out digestion reaction, obtained calcium hydroxide emulsion carries out filter cleaner through 60-120 object vibratory screening apparatus, remove the gred further through wet cyclone again, be placed in storage tank for subsequent use after obtaining calcium hydroxide emulsion;
(2) mix: be transferred to 6-12% thickening in groove the weight concentration added water calcium hydroxide emulsion, add compound crystal control agent, the weight of the compound crystal control agent wherein added is the 0.1-2.0% of calcium hydroxide weight, stirs 25-35 minute, makes it fully mix;
(3) carbonization: calcium hydroxide emulsion obtained in step (2) is squeezed into carbonization reactor with pump, opens kiln gas valve, passes into containing CO
2volumetric concentration is that the kiln gas of 15-100% carries out carburizing reagent, the feeding temperature of calcium hydroxide emulsion is 25-70 DEG C, in carbonation reaction, reaction self-heat generation, kiln gas can take away partial heat by emulsion, carbonation reaction temperature is between 30-70 DEG C, and carbonization closes kiln gas valve to during reaction solution pH=6.5-7, stopped reaction;
(4) dehydrate: reaction solution is obtained being mainly Rodlike light calcium carbonate after the normal process steps of dehydration, drying, pulverizing, screening;
The average minor axis of its primary particle of described Rodlike light calcium carbonate is 0.1-0.2 μm, the average major diameter of primary particle is 0.3-2.0 μm, long-width ratio is 3-20;
Described compound crystal control agent is made up of three kinds of components, and the first component is solubility magnesium salts, and the second component is polyvinyl alcohol, and the third component is phosphoric acid or its esters, and wherein three kinds of component weight ratios are: 1.0: 0.8-2.5: 0.2-2.0.
2. the preparation method of a kind of Rodlike light calcium carbonate according to claim 1, is characterized in that: the weight concentration that described carburizing reagent controls calcium hydroxide emulsion is 12%, and kiln gas is containing CO
2volumetric concentration is 30%.
3. the preparation method of a kind of Rodlike light calcium carbonate according to claim 1, is characterized in that: described carbonization reactor is with whipping appts or the intermittent type bubbling carbonizing tower without whipping appts.
4. the preparation method of a kind of Rodlike light calcium carbonate according to claim 1, is characterized in that: described Rodlike light calcium carbonate is applicable to plastics, papermaking, the manufacture of electric component, the manufacture of best bright finish structure unit.
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Denomination of invention: A rod-shaped light calcium carbonate and its preparation method Effective date of registration: 20220715 Granted publication date: 20160120 Pledgee: Guangxi Guihui Financing Guarantee Co.,Ltd. Pledgor: Guangxi Warner New Material Co.,Ltd. Registration number: Y2022450000115 |
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