CN100467381C - Flake light calcium carbonate and its preparing method and application - Google Patents

Flake light calcium carbonate and its preparing method and application Download PDF

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CN100467381C
CN100467381C CNB2006101478976A CN200610147897A CN100467381C CN 100467381 C CN100467381 C CN 100467381C CN B2006101478976 A CNB2006101478976 A CN B2006101478976A CN 200610147897 A CN200610147897 A CN 200610147897A CN 100467381 C CN100467381 C CN 100467381C
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light calcium
sheet
calcium carbonate
carbonization
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CN1986413A (en
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施晓旦
王彦华
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Shanghai Dongsheng New Material Co Ltd
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Abstract

The present invention discloses flake light calcium carbonate and its preparation process and application. Flake light calcium carbonate is produced through adding flake Zr(HPO4)2 into 2-20 wt% concentration Ca(OH)2 slurry with the Zr(HPO4)2 adding amount being 0.5-5 wt% of Ca(OH)2; and introducing gas containing CO2 to carbonize at the temperature of 10-90 deg.c and CO2 gas concentration of 10-100 vol% to pH 6.5-7.5 to obtain flake light calcium carbonate. Thus produced flake light calcium carbonate is suitable for use as the paint to make paper with excellent brightness, smoothness, opacity and printing adapatability.

Description

Flake light calcium carbonate and its production and application
Technical field
The present invention relates to a kind of flake light calcium carbonate and preparation method thereof, specifically, is a kind ofly can be used for flake light calcium carbonate of papermaking paint and preparation method thereof.
Background technology
Lime carbonate is important inorganic chemical product, often makes filler, is widely used in operations such as rubber, plastics, coating, papermaking and printing ink.Flaky calcium carbonate is mainly used in the paper coating, can increase the smooth finish and the planeness of paper, is the kaolinic ideal substitute of paper grade (stock).
Ordinary calcium carbonate is raw material usually with the Wingdale, makes unslaked lime through calcining, and unslaked lime adds water digestion and absorbing carbon dioxide carries out carbonization then, and dehydration, drying obtain product at last.
The preparation method of flaky calcium carbonate mainly is divided into two-step approach and single stage method.Two-step approach is meant under liquid-phase condition, at first with carbonic acid gas the milk of lime carbonization is arrived to a certain degree, and control condition obtains flaky intermediate product, separate, do not changing under the prerequisite that forms crystalline form, continue carbonization, finish the carburizing reagent of second half section, finally obtain flaky calcium carbonate.
The weak point of two-step approach is: the one, and reaction process is carried out in two steps, and is more loaded down with trivial details, and the second step carbonization technique energy consumption is more; The 2nd, in carbonization process, obtain the sheet intermediate and crystalline form be destroyed in the subordinate phase carbonization, condition is difficult to control, the unstable product quality that obtains.
Single stage method is meant that as the common precipitated chalk of preparation, carbonization technique one step finishes, and adds crystal control agent between being characterized in carbonization process in due course to obtain flaky calcium carbonate.Japanese patent laid-open 5-116936 disclose in carbonization process add organic phosphoric compound as crystal control agent in, add water miscible alkaline earth salt and play synergy, the flaky calcium carbonate that this method obtains is used for papermaking, make paper performance that bigger improvement be arranged, but because the organic phosphoric compound toxicity of adding is bigger, and cost an arm and a leg, so this method is restricted aspect industrialization.
Yuan Wei, gold stupidly reported among the No.2 in " fine chemistry industry " in 1998, and the boride that adopts inexpensive, low toxicity also can obtain flaky calcium carbonate as crystal control agent.But yield is lower, poor stability, and radius-thickness ratio is little.
Summary of the invention
The technical issues that need to address of the present invention are to disclose a kind of flake light calcium carbonate and its production and application, to overcome the above-mentioned defective that prior art exists.
The preparation method of flake light calcium carbonate of the present invention comprises the steps:
With sheet Zr (HPO 4) 2Be crystal seed, with sheet Zr (HPO 4) 2Joining weight concentration is 2～20%Ca (OH) 2In the slurry, sheet Zr (HPO 4) 2Add-on be Ca (OH) 20.5～5% (over dry/over dry) of weight feeds and contains CO 2The gas carbonization, carbonization temperature is 10～90 ℃, CO 2The volumetric concentration of gas be 10～100%, carbonization carbonization when the pH of slurry is 6.5-7.5 finishes, and obtains flake light calcium carbonate;
Said sheet Zr (HPO 4) 2For diameter be 0.3-1.0 μ m, radius-thickness ratio is 6:1---10:1.
Said sheet Zr (HPO 4) 2, the preparation method, comprise the steps: the aqueous solution of solubility zirconates and the reactant aqueous solution of soluble phosphoric acid dihydric salt are prepared Zr (HPO 4) 2The gel slurry is with Zr (HPO 4) 2The gel slurry is heated to boiling, and boiling reflux 520 hours filters, washs, and obtains sheet Zr (HPO 4) 2
The concentration of the aqueous solution of described solubility zirconates is 0.2-2.0mol/l, and the concentration of the aqueous solution of soluble phosphoric acid dihydric salt is 0.2-2.0mol/l.
Described solubility zirconates is selected from ZrOCl 28H 2O, Zr (SO 4) 24H 2Among the O one or more.
Described soluble phosphoric acid dihydric salt is selected from one or more in SODIUM PHOSPHATE, MONOBASIC, potassium primary phosphate, the primary ammonium phosphate.
The mol ratio of described solubility zirconates and soluble phosphoric acid dihydric salt is 1:1-1:1.3.
The diameter of described flake light calcium is 0.5-10 μ m, and radius-thickness ratio is 20:1---80:1.
The flake light calcium carbonate of present technique preparation is suitable for doing paper coating, and the coating made from the flake light calcium paper is used for the paper coating, and the page of making has good glossiness, smoothness, opaqueness and printing adaptability.
The advantage of present technique is: adopt sheet crystal seed technology, and the flake light calcium even particle size distribution of preparation, technology is simple, and technology stability is good; Crystal control agent is inexpensive, nontoxic.
Description of drawings
Fig. 1 is the electromicroscopic photograph of product.
Specific implementation method
Embodiment 1
With 1m 31.2mol/L ZrOCl 28H 2The O aqueous solution and 1m 31.2mol/L the SODIUM PHOSPHATE, MONOBASIC reactant aqueous solution prepare Zr (HPO 4) 2The gel slurry is with Zr (HPO 4) 2The gel slurry is put into the 3m that has reflux exchanger 3In the reactor, be heated to boiling then, boiling reflux 5 hours filters, washs, and obtains sheet Zr (HPO 4) 2, obtain solid content and be 30% filter cake 1020kg.With sem observation sheet Zr (HPO 4) 2Diameter is 0.5 μ m, and radius-thickness ratio is 8:1.
With sheet Zr (HPO 4) 2Be crystal seed, with 30kg sheet Zr (HPO 4) 2Filter cake joins 5 tons of 10%Ca (OH) 2In the slurry, feed that to contain volumetric concentration be 10% CO 2The gas carbonization, the temperature during carbonization is 50 ℃, carbonization is that carbonization in 7.0 o'clock finishes to pH, and the flake light calcium slurries filtration is obtained solid content 60.0% flake light calcium filter cake 790kg.With sem observation flake light calcium diameter is 2 μ m, and radius-thickness ratio is 25:1.
Embodiment 2
With 1m 32.0mol/L Zr (SO 4) 24H 2The O aqueous solution and 1m 32.0mol/L the potassium dihydrogen phosphate aqueous solution prepared in reaction obtain Zr (HPO 4) 2The gel slurry is with Zr (HPO 4) 2The gel slurry is put into the 3m that has reflux exchanger 3In the reactor, be heated to boiling then, boiling reflux obtained sheet Zr (HPO in 10 hours 4) 2, filter, wash sheet Zr (HPO 4) 2, obtain solid content and be 40% filter cake 1320kg.With sem observation sheet Zr (HPO 4) 2Diameter is 0.8 μ m, and radius-thickness ratio is 10:1.
With sheet Zr (HPO 4) 2Be crystal seed, with 125kg sheet Zr (HPO 4) 2Filter cake joins 5 tons of 20%Ca (OH) 2In the slurry, feed and contain volumetric concentration 22%CO 2The gas carbonization, the temperature during carbonization is 70 ℃, carbonization is that carbonization in 7.1 o'clock finishes to pH, and the flake light calcium slurries filtration is obtained solid content 58.0% flake light calcium filter cake 1650kg.With sem observation flake light calcium diameter is 10 μ m, and radius-thickness ratio is 80:1.
Embodiment 3
With 1m 31.0mol/L ZrOCl 28H 2The O aqueous solution and 1m 31.0mol/L the ammonium dihydrogen phosphate aqueous solution prepared in reaction obtain Zr (HPO 4) 2The gel slurry is with Zr (HPO 4) 2The gel slurry is put into the 3m that has reflux exchanger 3In the reactor, be heated to boiling then, boiling reflux obtained sheet Zr (HPO in 20 hours 4) 2, filter, wash sheet Zr (HPO 4) 2, obtain solid content and be 38% filter cake 710kg.With sem observation sheet Zr (HPO 4) 2Diameter is 0.4 μ m, and radius-thickness ratio is 7:1.
With sheet Zr (HPO 4) 2Be crystal seed, with 21kg sheet Zr (HPO 4) 2Filter cake joins 10 tons of 2%Ca (OH) 2In the slurry, feed and contain 100%CO 2The gas carbonization, the temperature during carbonization is 90 ℃, carbonization is that carbonization in 6.9 o'clock finishes to pH, and the flake light calcium slurries filtration is obtained solid content 61.0% flake light calcium filter cake 430kg.With sem observation flake light calcium diameter is 5 μ m, and radius-thickness ratio is 40:1.
Embodiment 4
With 1m 30.2mol/L Zr (SO 4) 24H 2The O aqueous solution and 1m 30.2mol/L the SODIUM PHOSPHATE, MONOBASIC reactant aqueous solution prepare Zr (HPO 4) 2The gel slurry is with Zr (HPO 4) 2The gel slurry is put into the 3m that has reflux exchanger 3In the reactor, be heated to boiling then, boiling reflux obtained sheet Zr (HPO in 12 hours 4) 2, filter, wash sheet Zr (HPO 4) 2, obtain solid content and be 41% filter cake 130kg.With sem observation sheet Zr (HPO 4) 2Diameter is 1.0 μ m, and radius-thickness ratio is 6:1.
With sheet Zr (HPO 4) 2Be crystal seed, with 30kg sheet Zr (HPO 4) 2Filter cake joins 5 tons of 8%Ca (OH) 2In the slurry, feed and contain 20%CO 2The gas carbonization, the temperature during carbonization is 10 ℃, carbonization is that carbonization in 7.2 o'clock finishes to pH, and the flake light calcium slurries filtration is obtained solid content 56.0% flake light calcium filter cake 680kg.With sem observation flake light calcium diameter is 2 μ m, and radius-thickness ratio is 31:1.
Embodiment 5
With 1m 31.5mol/L ZrOCl 28H 2The O aqueous solution and 1m 31.5mol/L the ammonium dihydrogen phosphate aqueous solution prepared in reaction obtain Zr (HPO 4) 2The gel slurry is with Zr (HPO 4) 2The gel slurry is put into the 5m that has reflux exchanger 3In the reactor, be heated to boiling then, boiling reflux obtained sheet Zr (HPO in 14 hours 4) 2, filter, wash sheet Zr (HPO 4) 2, obtain solid content and be 37% filter cake 1070kg.With sem observation sheet Zr (HPO 4) 2Diameter is 0.6 μ m, and radius-thickness ratio is 9:1.
With sheet Zr (HPO 4) 2Be crystal seed, with 21kg sheet Zr (HPO 4) 2Filter cake joins 5 tons of 13%Ca (OH) 2In the slurry, feed and contain 16%CO 2The gas carbonization, the temperature during carbonization is 60 ℃, carbonization is that carbonization in 6.9 o'clock finishes to pH, and the flake light calcium slurries filtration is obtained solid content 59.0% flake light calcium filter cake 1030kg.With sem observation flake light calcium diameter is 3 μ m, and radius-thickness ratio is 35:1.
Embodiment 6
With 1m 31.4mol/L Zr (SO 4) 24H 2The O aqueous solution and 1m 31.4mol/L the potassium dihydrogen phosphate aqueous solution prepared in reaction obtain Zr (HPO 4) 2The gel slurry is with Zr (HPO 4) 2The gel slurry is put into the 5m that has reflux exchanger 3In the reactor, be heated to boiling then, boiling reflux obtained sheet Zr (HPO in 8 hours 4) 2, filter, wash sheet Zr (HPO 4) 2, obtain solid content and be 35% filter cake 1070kg.With sem observation sheet Zr (HPO 4) 2Diameter is 0.3 μ m, and radius-thickness ratio is 6:1.
With sheet Zr (HPO 4) 2Be crystal seed, with 31kg sheet Zr (HPO 4) 2Filter cake joins 5 tons of 11%Ca (OH) 2In the slurry, feed and contain 10%CO 2The gas carbonization, the temperature during carbonization is 30 ℃, carbonization is that carbonization in 6.8 o'clock finishes to pH, and the flake light calcium slurries filtration is obtained solid content 58.0% flake light calcium filter cake 910kg.With sem observation flake light calcium diameter is 6 μ m, and radius-thickness ratio is 45:1.
Embodiment 7
Be coated with in the prescription at white card face, use the import china clay and the calcined kaolin of the foregoing description flake light calcium sample instead of part, performance variation situations such as the physical index of investigation coating pattern and printability.Face is coated with the ivory board that the band precoating is adopted in experiment, uses linear spreading rod to carry out face and is coated with glue spread 10g/m 2Compare with the coating pattern of original formulation.Coating rolling condition: get above-mentioned coating pattern respectively with twice of the hard press polish of small-sized rolling press (0.3Mpa, 90 ℃).
Table 1 face is coated with face and is coated with prescription
Figure C200610147897D00081
Table 2 coating pattern detects data
Figure C200610147897D00082
Figure C200610147897D00091
From the result, similarity condition is compared with original formulation down, the foregoing description flake light calcium part substituting import one china clay and calcined kaolin, pattern level and smooth, to be coated with glossiness, surface strength, ink absorption and other difference little.

Claims (9)

1. the preparation method of a flake light calcium carbonate is characterized in that, comprises the steps:
With sheet Zr (HPO 4) 2Joining weight concentration is 2～20%Ca (OH) 2In the slurry, sheet Zr (HPO 4) 2Add-on be Ca (OH) 20.5～5% of weight feeds and contains CO 2The gas carbonization, carbonization temperature is 10～90 ℃, CO 2The volumetric concentration of gas be 10～100%, carbonization carbonization when the pH of slurry is 6.5-7.5 finishes, and obtains flake light calcium carbonate;
Said sheet Zr (HPO 4) 2Diameter be 0.3-1.0 μ m, radius-thickness ratio is 6:1--10:1.
2. method according to claim 1 is characterized in that, said sheet Zr (HPO 4) 2The preparation method, comprise the steps: the aqueous solution of solubility zirconates and the reactant aqueous solution of soluble phosphoric acid dihydric salt are prepared Zr (HPO 4) 2The gel slurry is with Zr (HPO 4) 2The gel slurry is heated to boiling, and boiling reflux 5-20 hours filters, washs, and obtains sheet Zr (HPO 4) 2
3. method according to claim 2 is characterized in that, the concentration of the aqueous solution of described solubility zirconates is 0.2-2.0mol/l, and the concentration of the aqueous solution of soluble phosphoric acid dihydric salt is 0.2-2.0mol/l.
4. method according to claim 2 is characterized in that, described solubility zirconates is selected from ZrOCl 28H 2O, Zr (SO 4) 24H 2Among the O one or more.
5. method according to claim 2 is characterized in that, described soluble phosphoric acid dihydric salt is selected from one or more in SODIUM PHOSPHATE, MONOBASIC, potassium primary phosphate, the primary ammonium phosphate.
6. method according to claim 2 is characterized in that, the mol ratio of described solubility zirconates and soluble phosphoric acid dihydric salt is 1:1-1:1.3.
7. according to the flake light calcium carbonate of each described method preparation of claim 1～6.
8. flake light calcium carbonate according to claim 7, diameter are 0.5-10 μ m, and radius-thickness ratio is 20:1---80:1.
9. according to the application of claim 7 or 8 described flake light calcium carbonates, be used to do paper coating.
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Publication number Priority date Publication date Assignee Title
CN101302026B (en) * 2008-06-30 2010-08-25 上海东升新材料有限公司 Honeycomb calcium carbonate, and preparation and application method thereof
CN101514533B (en) * 2008-12-30 2011-06-15 上海东升新材料有限公司 Flaky calcium carbonate, preparation method and application thereof
CN105484099A (en) * 2014-10-13 2016-04-13 东升新材料（山东）有限公司 Aragonite-type light calcium composition used in paper coating, and application method thereof
CN105152198B (en) * 2015-10-15 2017-03-29 广西民族大学 A kind of preparation method of lamellar aragonitic calcium carbonate superfine powder granule
CN118064099A (en) * 2024-04-17 2024-05-24 上海惊叹化学有限公司 Sprayable high-temperature-resistant polyurethane adhesive and preparation method thereof

Citations (1)

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CN1080909A (en) * 1993-07-15 1994-01-19 北京化工学院 The preparation method of lamellar crystal light calcium carbonate

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1080909A (en) * 1993-07-15 1994-01-19 北京化工学院 The preparation method of lamellar crystal light calcium carbonate

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