CA2437066A1 - Method and apparatus for production of precipitated calcium carbonate and silicate compounds in common process equipment - Google Patents

Method and apparatus for production of precipitated calcium carbonate and silicate compounds in common process equipment Download PDF

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Publication number
CA2437066A1
CA2437066A1 CA002437066A CA2437066A CA2437066A1 CA 2437066 A1 CA2437066 A1 CA 2437066A1 CA 002437066 A CA002437066 A CA 002437066A CA 2437066 A CA2437066 A CA 2437066A CA 2437066 A1 CA2437066 A1 CA 2437066A1
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set forth
slurry
reactor
calcium silicate
lime
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CA002437066A
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CA2437066C (en
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Vijay K. Mathur
Varun K. Mathur
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    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/63—Inorganic compounds
    • D21H17/67—Water-insoluble compounds, e.g. fillers, pigments
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/20—Silicates
    • C01B33/24—Alkaline-earth metal silicates
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F11/00—Compounds of calcium, strontium, or barium
    • C01F11/18—Carbonates
    • C01F11/181—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by control of the carbonation conditions
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/30—Particle morphology extending in three dimensions
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/54—Particles characterised by their aspect ratio, i.e. the ratio of sizes in the longest to the shortest dimension
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/12—Surface area
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/10—Process efficiency
    • Y02P20/129—Energy recovery, e.g. by cogeneration, H2recovery or pressure recovery turbines

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
  • Paper (AREA)
  • Silicates, Zeolites, And Molecular Sieves (AREA)

Abstract

A method and apparatus for the production of calcium carbonate and calcium silicate in common superatmospheric reactors. Multiple reactors (T-31, T-32) can be provided for switching production between reactors, and advantageously utilizing process waste heat. On site production of both PCC and Calcium Silicate Hydrates is thus achieved in a paper mill.

Claims (76)

1. A method for the hydrothermal production of calcium silicate hydrate and calcium carbonate in common process equipment, said method comprising:
(a) providing a first aqueous lime slurry at a predetermined temperature, said aqueous lime slurry comprising Ca(OH)2 solids and dissolved Ca(OH)2 in the form of Ca++
ions;

(b) screening grit from said slurry;

(c) conditioning said slurry to predetermined temperature;

(d) feeding said slurry into a first reactor;

(e) agitating the contents of said first reactor at super-atmospheric pressure;

(f) introducing a stream of CO2 in to said reactor;

(g) reacting said CO2 and said Ca++ to produce insoluble calcium carbonate;

(h) removing said insoluble calcium carbonate and associated aqueous medium from said first reactor;

(i) charging a second reactor with a second aqueous slurry comprising silica at a concentration of from about 1 to about 1.5 pounds of silica per gallon of slurry, while heating said second aqueous slurry in a heat exchange apparatus with said first aqueous medium being discharged from said first reactor;

(j) charging said second reactor with a second aqueous lime slurry;

(k) heating the contents of said second reactor under hydrothermal conditions to produce a calcium silicate precipitate.
2. The method as set forth in claim 1, wherein said silica comprises fluxed calcined diatomaceous earth (fade).
3. The method as set forth in claim 1, wherein the step of heating said second aqueous slurry is carried out in countercurrent fashion.
4. The method as set forth in claim 3, wherein said step of heating is carried out in a shell and tube heat exchanger.
5. The method as set forth in claim 1, wherein said hydrothermal conditions comprise pressure up to 1000 psig.
6. The method as set forth in claim 1, wherein during the step of reacting silica in said second reactor, agitation is provided in said second reactor.
7. The method as set forth in claim 1,wherein said carbon dioxide is dissolved in an aqueous medium before introduction into said first reactor under pressure.
8. The method as set forth in claim 1, wherein said step of conditioning said slurry to predetermined temperature comprises chilling said slurry in a chiller.
9. The method as set forth in claim 1, wherein the step of conditioning said slurry to a predetermined temperature comprises heating said slurry in a heat exchanger.
10. The method as set forth in claim 1, wherein said first reactor and said second reactor are reversed, so that, in an additional step, calcium carbonate is produced in said second reactor, and calcium silicate is produced in said first reactor.
11. The method as set forth in claim 10, wherein multiple reactor pairs are provided.
12. The method as set forth in claim 11, wherein at least two pair of superatrnospheric reactors is provided.
13. The method as set forth in claim 1, wherein a specially designed pressure bank of carbonators are employed for the carbonation reaction.
14. The method as set forth in claim 13, wherein said carbonation reaction is controlled isothermally.
15. The process as set forth in claim 1, where the time for preparation of said lime slurry preparation time (slaking) is matched with the time for the carbonation reaction in said first reactor, so that the whole manufacturing process can be carried out continuously.
16. The method as set forth in claim 1 wherein said said lime slurry has a concentration between 30 grams per liter and 300 grams per liter of sodium hydroxide
17. The process as set forth in claim 1 wherein the pH of said lime slurry is at least of pH 12.
18. The method as set forth in claim 1 where said lime slurry is temperature adjusted to between 50F and 120F.
19. The method as set forth in claim 1 where said lime slurry temperature is adjusted to approximately 50F by passing it through a heat exchanger, and wherein said insoluble calcium carbonate comprises a rhombohedral crystal habit.
20. The method as set forth in claim 1 where said lime slurry temperature is adjusted to 120F by passing it through a heat exchanger and a chiller, and wherein said insoluble calcium carbonate comprises aragonite crystals.
21. The method as set forth in claim 1 where said lime slurry temperature is adjusted to the range from about 80F to about 100F, and wherien said insoluble calcium carbonate comprises crystals having a sclenohedral crystal habit.
22. The method as set forth in claim 1 wherein the concentration of said lime slurry is in the range from about 30 gpl of calcium hydroxide to about 300 gpl of calcium hydroxide.
23. The method as set forth in claim 1 wherein the concentration of said. lime slurry is in the range from about 200 gpl of calcium hydroxide to about 250 gpl of calcium hydroxide.
24. The method as set forth in claim 1 where in the CO2 concentration is in the range of 5.0% CO2 by volume to 100% CO2 by volume.
25. The method as set forth in claim 1 wherein the CO2 flow rate (at 20% CO2 and 80% other gasses in the lab scale) into the 2-liter pressure reactor, having 1.2 liters of Ca(OH)2 slurry, varies from 0.5 lpm to 5.31pm.
26. The method as set forth in claim 1 wherein the agitation in the pressure reactor during the carbonation reaction is carried out by a mechanical agitator and the speed of agitation ranges from 500. rpm to 1500 rpm, preferably at 1500 rpm
27. The method as set forth in claim 1 where as the end of the carbonation reaction is indicated until the pH is reduced from ~l2 to ~8.
28. The method as set forth in claim 1 where as the end of the carbonation in the lab reactor is measured when the slurry temperature reaches a maximum.
29. The method as set forth in claim 1 wherein process variables are selected from a group consisting of:
(a) Pressure in the reactor vessel or carbonator;
(6) CO2 or flue gas concentration (c) CO2 or flue gas flow rate (d) Lime slurry concentration (e) Lime slurry temperature entering the pressure vessel (starting temperature) (f) Isothermal temperature during the carbonation reaction (g) Rate of agitation by the mechanical agitator
30. The method as set forth in claim 29, wherein said process variables are selected to manufacture sclenohedral PCC.
31. The method as set forth in claim 29 wherein said process variables are selected in optimization mode to produce rhombohedral PCC.
32. The method as set forth in claim29, wherein the process parameters are selected in optimum mode so as to produce aragonite PCC
33. The method as set forth in claim 29, wherein, said process parameters are selected in optimization mode so as to produce "stacked" rhombohedral PCC
34. The method as set forth in claim 29, wherein said process parameters are selected to produce shapes, sizes, and particle distributions resulting in production of sclenohedral PCC.
35. The method as set forth in claim 29, wherein said process parameters are selected to produce different shapes, sizes, particle size distributions, and aspect ratios of rhombohedral PCC
36. The process as set forth in claim 29, wherein said process parameters are selected to produce different shapes, sizes, and particles size distributions of aragonite PCC
37. The method as set forth in claim 34, wherein said reaction conditions are selected to give sclenohedral PCC suitable for use in paper filling, coating, and size press applications.
38. The process as set forth in claim 35 wherein the reaction conditions are selected to give a variety of rhombohedral PCC suitable in use for paper filling, coating, and size press, applications.
39. The method as set forth in claim 32, wherein said reaction conditions are selected to provide aragonite PCC suitable for application in paper filling, coating, and size press applications.
40. A.n improved process, equipment, and equipment configuration to produce calcium silicate hydrates, said process comprising:
(a) providing an aqueous lime slurry at near boiling temperature (200F);
(b) providing an aqueous slurry of silica source, preferably consisting of fine Fluxed Calcined, Diatomaceous Earth (FCDE), concentration of approximately 1.0 to 1.5 lbs/gallon.
(c) Processing the said slurry through a shell and tube heat recuperator, countercurrent to a hot liquid.
(d) Filling up the pressure reactor capable of operating up to 1000 psig.
(e) The reactants are heated with super heated steam (400 to 600psig) to carry out a hydrothermal reaction between Ca(OH)2 particles and silica from the diatoms, forming a calcium silicate hydrate.
(f) Slowly agitating the entire content of the pressure vessels during the formation of calcium silicate hydrates.
41. The process set forth in claim 40 wherein the lime slurry is formed in the same slaker as for the precipitated calcium carbonates.
42. The process set forth in claim 40 wherein said hydrothermal reaction is carried out in the same reactor as the carbonation process in the manufacture of precipitated calcium carbonate.
43. The process as set forth in claim 40 wherein the hydrothermal reaction between hot lime slurry and FCDE takes place in a bank of pressure reactors, the same ones used in the manufacture of PCC.
44. The process as set forth in claim 40 wherein the rate of hydrothermal reaction is balanced in such a way so as the feeding silica slurry and the discharging of the silicate slurry from the bank of reactors is continuous.
45. The process as set forth in claim 40 wherein the heat recovery is maximized by employing a series of heat exchangers to recuperate heat from the calcium silicate product.
46. The process as set forth in claim 40 wherein the lime slurry concentration is in the range of 0.2 to 0.4 lb/gallon.
47. The process as set forth in claim 40 wherein the FCDE slurry concentration is ~1.22 lb/gal.
48. The process as set forth in claim 40 wherein the lime to silica mole ratio ranges from 0.75 to 3Ø
49. The process as set forth in claim 40 wherein the lime/silica slurry concentration ranges from 0.2 lb/gal to 1.0 lb/gal.
50. The process as set forth in claim 40 wherein the time for the hydrothermal reaction varies between 1 to 4 hours.
51. The process as set forth in claim 50, wherein said time of reaction is approximately 2 hours.
52. The process as set forth in claim 40 wherein the temperature for the hydrothermal reaction varies from 355F to 527F.
53. The process as set forth in claim 40, wherein the pressure is maintained corresponding to the reaction temperature between 130 and 600 psig.
54. The process as set forth in claim 40, wherein the heat to the hydrothermal process is provided by super saturated steam at 450F to 600F.
55. The process as set forth in claim 40, or in the method of claim 1,wherein the sequence of addition of lime and of addition of silica slurry are interchangeable.
56. The process as set forth in claim 40, wherein the filling time of the pressure reactor is between 45 to 60 minutes.
57. The process as set forth in claim 40 wherein the discharge time for the calcium silicate slurry is between 45 to 60 minutes.
58. The process as set forth in claim 40, wherein the cooling time is between 30 and about 45 minutes.
59. The process as set forth in claim 40, wherein the process variables are selected from a group, consisting of:
a) Lime to Silica mole ratio b) Lime/Silica slurry concentration c) Type of lime (shape, size, and brightness) d) Type of FCDE (shape, size, and brightness) e) Sequencing of batch operations (i.e. filling, heating to reaction temp, time at reaction temp, time for discharge or "cooling")
60. The process as set forth in claim 59, wherein the reaction parameters are selected as follows:
(a) The lime to silica mole ratio is in the range of 1.2 to 1.6, preferably 1.33 to 1.41 (b) The lime/Silica slurry concentration is between 0.4 lb/gal to 0.8 lb/gal, preferably 0.6 lb/gal (c) Using 1/2" rotary pebble, high brightness quicklime (d) Using fine Fluxed Calcined Diatomaceous Earth (FCDE) (e) Wherein the heating sequence involves:
Time to Heat ~ 100 min Time at Temperature ~ 120 min Time to Cool ~ 30 min (f) The hydrothermal reaction is performed in the range of 390 F to 518F, and more preferably between about 464F and about 480F and such process conditions produced multiphase calcium silicate hydrates comprised predominately of ultra fine fibrous foshagite crystals with some fine fibrous xenotlite crystals and other minor phases of CSH.
61. The process as set forth in claim 59, wherein said foshagite of the calcium silicate hydrate consists primarily of fibrous crystals ranging in size from 0.1 to 0.3 microns and in length from 3 to 5 microns.
62. The process as set forth in claim 59, wherein said primary fibrous particles are interlocked. into a secondary particle structure, and said secondary particle structure varying from 7 microns to 30 microns, with an average particle sized in the range of 12 to 18 microns.
63. The process as set forth in claim 40, wherein the brightness of the multiphase calcium silicates is in the range of 95 +/- 2.
64. The process as set forth in claim 40, wherein the water absorption of the calcium silicate hydrate is in the range of 400 to 1000%, preferably between 700 and 1000%.
89 63. The process as set forth in claim 40, wherein the air permeability of the calcium silicate hydrate (as measured by Blaine method) is in the range of 60 to 200 seconds.
66. The process as set forth in claim 40 wherein the weight of the calcium silicate hydrate (as measured by Blame method) is in the range of 0.35 to 0.5 grams.
67. The process as set forth in claim 40 wherein the X.R.D. pattern of the powder is:
Foshagite: dMajor = 2.97 .ANG.
dMinor = 5.05 .ANG.
Xenotlite: dMajor = 3.107 .ANG.
DMinor = 3.66 .ANG.
68. The process as set forth in claim, 40 wherein the calcium silicate hydrate improved sheet bulk over standard pulp by 20 - 25%.
69. The process as set forth in claim 40 wherein the calcium silicate hydrate improved sheet opacity over pulp by 20 - 24 points.
70. The process as set forth in claim 40 wherein the calcium silicate hydrate improved sheet scattering power over pulp by 150% - 200%,
71. The process as set forth in claim 40 wherein the calcium silicate hydrate improved filler scattering coefficient over PCC by 20% - 25%.
72. The process as set forth in claim 40 wherein said calcium silicate hydrate has a scattering coefficient in the range of 2800 cm2/g to 3200 cm2/g.
73. The process as set forth in claim 40 wherein the calcium silicate hydrate improved sheet porosity over pulp by 20% to 25%.
74. Paper containing the calcium silicate hydrate produced by the process as set forth in claim 40 has porosity than paper containing market PCC by 100% to 200%.
75. Paper made by the process as set forth in claim 40, wherein paper containing the calcium silicate hydrate gave 30% to 40% higher stiffness than a pulp sheet alone.
76. Paper made by the process as set forth in claim 40, wherein said paper sheet containing the calcium silicate hydrate provides 10% to 15% higher tensile strength.
CA002437066A 2001-01-31 2002-01-31 Method and apparatus for production of precipitated calcium carbonate and silicate compounds in common process equipment Expired - Lifetime CA2437066C (en)

Applications Claiming Priority (5)

Application Number Priority Date Filing Date Title
US26565701P 2001-01-31 2001-01-31
US60/265,657 2001-01-31
US09/797,173 US7048900B2 (en) 2001-01-31 2001-02-28 Method and apparatus for production of precipitated calcium carbonate and silicate compounds in common process equipment
US09/797,173 2001-02-28
PCT/US2002/003142 WO2002060986A2 (en) 2001-01-31 2002-01-31 Method and apparatus for production of precipitated calcium carbonate and silicate compounds in common process equipment

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CA2437066A1 true CA2437066A1 (en) 2002-08-08
CA2437066C CA2437066C (en) 2009-12-22

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AU (1) AU2002247062A1 (en)
CA (1) CA2437066C (en)
WO (1) WO2002060986A2 (en)

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US20060272549A1 (en) 2006-12-07

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