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MXPA97003753A - Method for the purification of calbonate carbonate - Google Patents

Method for the purification of calbonate carbonate

Info

Publication number
MXPA97003753A
MXPA97003753A MXPA/A/1997/003753A MX9703753A MXPA97003753A MX PA97003753 A MXPA97003753 A MX PA97003753A MX 9703753 A MX9703753 A MX 9703753A MX PA97003753 A MXPA97003753 A MX PA97003753A
Authority
MX
Mexico
Prior art keywords
calcium carbonate
suspension
weight
process according
chelating agent
Prior art date
Application number
MXPA/A/1997/003753A
Other languages
Spanish (es)
Other versions
MX9703753A (en
Inventor
Kendall Drummond Donald
Original Assignee
Minerals Technologies Inc
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from US08/343,002 external-priority patent/US5690897A/en
Application filed by Minerals Technologies Inc filed Critical Minerals Technologies Inc
Publication of MX9703753A publication Critical patent/MX9703753A/en
Publication of MXPA97003753A publication Critical patent/MXPA97003753A/en

Links

Abstract

The present invention relates to a method for reducing the iron content of calcium carbonate containing iron, characterized in that it comprises treating an aqueous suspension of said calcium carbonate with a chelating agent, heating said calcium carbonate aqueous suspension containing agent chelating and treating said aqueous calcium carbonate suspension containing chelating agent with carbon dioxide gas, wherein said treatment with said chelating agent is carried out while heating and stirring said suspension and said carbon dioxide gas is introduced to maintain a pH of said suspension on the scale of about 5.5 to no more than 7

Description

METHOD FOR PURIFICATION OF CALCIUM CARBONATE FIELD OF THE INVENTION The present invention relates to a method for reducing the iron content of calcium carbonate. More particularly, the present invention relates to a method for purifying calcium carbonate. Still more particularly, the present invention relates to a method for decreasing the iron content in calcium carbonate suspensions by treating the calcium carbonate suspension with a chelating agent such as, for example, ethylenediaetetraacetic acid (EDTA). The calcium carbonate produced according to the method of this invention is particularly suitable for use with food or pharmaceutical additives and may also be useful as a filler in paper or co-process processes or an additive in plastic products.
BACKGROUND; OF THE INVENTION The calcium carbonate in most limestone quarries contains a certain level of iron, usually in the form of iron oxide. However, the presence of iron in any form is sometimes considered a contaminant in calcium carbonate. The presence of iron specifically prevents the use of this calcium carbonate in many specialized markets, such as food products and pharmaceutical applications. Moreover, the presence of iron in calcium carbonate decreases the economic value of final products, either in papermaking processes or in the production of plastic. Various physical and chemical procedures have been suggested to remove iron from calcium carbonate. Physical removal first requires the grinding of calcium carbonate to such a fineness that the iron can be subsequently removed by sieving, sorting, magnetic separation or flotation. The chemical leaching or bleaching of calcium carbonate grinded with solvents followed by filtration has also been suggested as a method to remove iron from calcium carbonate. However, these physical and chemical procedures for the removal of iron from calcium carbonate are complex and difficult to administer. Of equal importance are the erratic results, the unpredictable efficiencies of the procedures, the amounts of iron removed, and the expenses associated with many of the chemical and physical processes for removing iron from calcium carbonate. What has been discovered as novel and not anticipated by the prior art is a process for the purification of calcium carbonate containing iron and the subsequent use of such purified calcium carbonate in applications and markets, such as, specialized grade products. , for example, in foods, plastics and pharmaceutical products where a higher purity of calcium carbonate is required. It is therefore an object of the present invention to provide a simple, predictable and inexpensive process for the purification of calcium carbonate containing iron. Another object of the present invention is to provide a purified calcium carbonate product containing less than 500 parts per million of iron. A further object of the present invention is to provide a product that is particularly useful in food grade and pharmaceutical applications where the purity of calcium carbonate is a requirement. These and other objects of the present invention will become apparent from the detailed description that continues.
RELATED PREVIOUS TECHNIQUE The patent of E.U.A. No. 4,824,653 discloses a process for bleaching limestone by first grinding limestone into small sizes by conventional grinding methods, either wet or dry. The milled limestone is then mixed with water to form a suspension having a solids content of about 15 percent to 50 percent. An etching agent, such as ethylenedianinotetraacetic acid (EDTA) and a bleaching agent, such as sodium hydrosulfite, are added to the suspension and mixed at an elevated temperature before filtering and drying. The limestone product produced in accordance with the process of this invention exhibits improved whiteness.
BRIEF DESCRIPTION OF THE INVENTION What was discovered as novel and not anticipated by the prior art is a method for the purification of calcium carbonate containing iron. The iron content of calcium carbonate is substantially decreased by treating an aqueous suspension of calcium carbonate with an iron chelating agent, while heating the suspension and treating the suspension with carbon dioxide. The extracted iron is subsequently separated from the calcium carbonate by filtration. The purified calcium carbonate product produced according to the method of the present invention is particularly useful in food grade products, paper products, coatings and plastic products, where a reduced iron content is required.
DETAILED DESCRIPTION OF THE INVENTION The present invention includes a process for reducing the iron content of calcium carbonate. The iron in the calcium carbonate is extracted by treating an aqueous suspension of calcium carbonate with an iron-containing agent, heating and stirring the suspension at the same time and introducing a gas containing carbon dioxide to control the pH during the process. Mien-o of extraction. The extracted iron is subsequently separated from the calcium carbonate by filtration. The purification process of the present invention can be used to reduce the iron content of any limestone product. This includes U5P and food grade products, fillers and paper and product coating *; of plastic filling. Calcium carbonates that are useful in the present invention include, but are not limited to, any calcium carbonate that con + mineral, eg, limestone, chalk, dolomite, and precipitated calcium carbonate produced synthetically. The calcium carbonate is processed as an aqueous suspension of about 1 weight percent to about 70 weight calcium carbonate, based on the total weight of the suspension. The preferred weight concentration of calcium carbonate is from about 10 percent to about 30 percent by weight of calcium carbonate, based on the total weight of the suspension. Suspension concentrations of less than about 10 weight percent based on the total weight of the suspension tend not to be practical based on economic considerations. More than 30 percent by weight of calcium carbonate based on the total weight of the suspension may require the use of a dispersant, which could interfere with the extraction process, although not necessarily. Routine experimentation would determine what dispersant could be used in the present inventive process. The iron chelating agents useful in the method of the present invention may be any material capable of iron complexing, more specifically the chelating agent must have a much higher formation constant with iron than with calcium. The chelating agents especially useful in the method of the present invention are selected from the group consisting of nitrilotriacetic acid (H3NTA), ethylenediaminetetraacetic acid (H4EDTA), diethylenetria inopentaacetic acid (H5DPTA) and hydroxyethylenediaminetriacetic acid (H3HEDTA) and salts thereof. The preferred chelating agent is ethylenediaetetraacetic acid (EDTA) and any salt thereof. The calcium carbonate containing iron is treated with from about 0.01 percent to about 10 percent chelating agent. When the chelating agent is EDTA the preferred treatment level is from about 0.1 weight percent to about 1.0 weight percent, based on the weight of the calcium carbonate present, depending on the amount of iron present in the calcium carbonate. The gas containing carbon dioxide useful in the process of the present invention contains between about 1 percent to about 100 percent CO2 on a volume basis. Typical concentrations of CO2 range from approximately 10 percent to approximately 30 percent CO2 on a volume basis. In view of the fact that the gas containing carbon dioxide described above is used to control the pH of the calcium carbonate suspension, the rate of addition of said gas containing CO2 is adjusted to maintain the pH of the suspension in the range of about 5.5 to about 7.0, preferably about 6.0 to about 6.5. The calcium carbonate suspension and the chelating agent are heated to a high temperature scale of from about 20 degrees to about 100 degrees centigrade. The preferred temperature scale is from about 40 degrees to about 60 degrees centigrade. The suspension is stirred, filtered, washed and dried. It is believed that by employing an iron chelating agent, controlling both the temperature and the pH, it promotes the dissolution of the iron in calcium carbonate. The dissolved iron is conpleted by the chelating agent. When the iron is dissolved by lowering the pH and raising the temperature, the iron is complexed by the chelating agent and diverts the equilibrium to solubilize more iron. Additionally, the lower pH provides a higher formation constant between the iron and the chelating agent, thus improving the overall equilibrium towards the solubilization of the iron. The calcium carbonate and the iron are subsequently separated by filtration, containing the filtrate to the complexed iron. However, what is being suggested here is a theory about why the method of the present invention decreases iron calcium carbonate. This should be accepted only as a theory as to why the invention works and should not be used under any conditions or whatever to limit the scope of the present invention, which is illustrated in more detail by means of the examples below and it is defined more specifically by means of the claims.
EXAMPLES 1 TO 6 In Examples 1 to 6, calcium carbonate (untreated) with an iron content of 715 ppm of Fß2? 3 was treated as a suspension with 0.33 weight percent of EDTA during variable treatment times, at different treatment temperatures and at different suspension pH values. The resulting treated calcium carbonate suspensions were filtered, the treated products thus obtained were washed, dried and analyzed to verify the F 2? 3 content. The experiments were carried out as follows: EXAMPLE 1 To 81 rnl of deionized water, 9 ml of a 0.01 molar solution of Na2H2 EDTA.2H2O was added. To the above stirred solution were added 10 grams of precipitated calcium carbonate. The suspension was then heated to 60 ° C and stirred at 60 ° C for 24 hours. The pH of the suspension was 8.0 and remained 8.0 since no pH control (no CO2) was used in this treatment. The suspension was filtered, the collected solids were washed with deionized water and subsequently dried.
EXAMPLE 2 In the same manner described in example 1, to 90 ml of deionized water containing 9 ml of 0.02 molar Na2H2 EDTA.2H2O solution, 10 grams of precipitated calcium carbonate was added. While stirring, CO2 was introduced into the suspension to adjust the pH of the suspension to 6.0 and the suspension was heated to 60 ° C. The suspension was stirred for 24 hours at 60 ° C, maintaining the pH at 6.0 introducing CO2 as necessary, the resulting treated calcium carbonate slurry was further processed as in Example 1. 5 EXAMPLE 3 In the same manner as in example 2, the calcium carbonate product was treated with 0.33 weight percent of O EDTA as a suspension at a temperature of 60 ° C and a pH of 6.0, using CO2 to con + roll the pH, only for 2 hours. The resulting suspension was processed as in Example 1.
EXAMPLE 4 In the same manner as in example 2, the calcium carbonate product was treated with 0.33 weight percent EDTñ in the form of a suspension at a temperature of 60 ° C and a pH 0 of 6.0, using CO2 to con + roll the pH only for 1 hour. The resulting suspension was processed as in Example 1.
EXAMPLE 5 F In the same manner as described in Example 2, the lime carbonate product was treated with 0.33 weight percent EDTA as a suspension, the pH of the suspension was adjusted to 6.0 and maintained at 6.0 using CO2. The suspension was heated to 40 ° C with stirring and kept at 40 ° C, pH 6.0 for 3 hours. The resulting treated product was processed dictionally as in Example 1.
EXAMPLE 6 In the same manner as that described in Example 5, the calcium carbonate product was treated with 0.33 weight percent EÜTO as a suspension at a temperature of 40 ° C and a pH of 6.0 only for 1 hour. The resulting product was further processed after filtering, washing and drying as in Example 1. rü CJ! s L? PICTURE Product Resulting time Example Atmosphere Treatment PH Temp.QC. agitation ppm F? 2? 3 Carbonate of 715 precipitated calcium without treatment 0.J3% by weight Air 8.0 60 24 701 of EDTA 0.33% by weight C0- 6.0 60 24 286 of EDTA 1- ' 0. 33% by weight CO 6.0 60 272 of EDTA 0.33% by weight CO. 6.0 60 315 of EDTA 0.33% by weight C0-- 6.0 40 372 of EDTA 0.33% by weight C0-- 6.0 40 415 of EDTA The treated calcium carbonate products were analyzed to verify the iron content and compared with the calcium carbonate not treated in the table. The data in the table show the pH adjustment value, the value of elevated temperatures and the effect of the present inventive procedure for the removal of iron.

Claims (12)

NOVELTY OF THE INVENTION CLAIMS
1. A process to decrease the iron content of calcium carbonate which consists of treating an aqueous suspension of calcium carbonate with a chelating agent, heating the aqueous suspension of calcium carbonate and treating the aqueous suspension of calcium carbonate with 10 carbon dioxide gas.
2. The process according to claim 1, wherein the concentration of calcium carbonate in the aqueous suspension of calcium carbonate is from 1% by weight to 70% by weight, based on the total weight of the suspension 1 r? of calcium carbonate.
3. The process according to claim 1 or 2, wherein the concentration of calcium carbonate in the aqueous calcium carbonate suspension is from JO percent to 30 percent by weight, based on the total weight of ? ü the calcium carbonate suspension.
4. The process of any of the foregoing reactions, in which the chelating agent is selected from the group consisting of nitrile tpacetic acid, ethylenediaminetetraacetic acid, sodium lactate diet, hydroxothylethyldenetriacetic acid and leaves the same.
5. The process according to any of the preceding claims, wherein the amount of chelating agent is 0.01% on weight at 10% by weight, based on the weight of calcium carbonate.
6. The process according to claim 4, wherein the chelating agent is etiiendia inotetraaceti acid and wherein the amount of chelating agent is 0.1% by weight to 1.0% by weight, based on the weight of the carbonate of calcium.
7. The process according to any of the preceding claims, wherein the gas containing carbon dioxide has a concentration of CO2 of 1% to 100% and in which the pH of the carbonate suspension of calcium is from 5.5 to 7.0.
8. The process according to any of the preceding claims, wherein the gas containing carbon dioxide preferred has a concentration of CO2 of 1% at J00% and in which the preferred pH is 6.0 to ñ "5. %:
9. The process according to any of the preceding claims, wherein the temperature scale of the aqueous calcium carbonate suspension is from 20 to 100 degrees centigrade.
10. The process according to claim 9, wherein the preferred temperature scale of the aqueous calcium carbonate suspension is from 40 to 60 degrees centigrade. Ifi
11. - The process according to any of the preceding claims, which further comprises treating an aqueous suspension of calcium carbonate with a chelating agent, heating the aqueous suspension of calcium carbonate, stirring the aqueous suspension of calcium carbonate introducing the same time on said aqueous calcium carbonate suspension a gas containing carbon dioxide.
12. A food product, a pharmaceutical drug, a plastic product or a paper product containing calcium carbonate produced in accordance with the process of any of the preceding claims.
MXPA/A/1997/003753A 1994-11-21 1995-11-16 Method for the purification of calbonate carbonate MXPA97003753A (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
US08/343,002 US5690897A (en) 1994-11-21 1994-11-21 Method for purification of calcium carbonate
US08343002 1994-11-21
PCT/US1995/014994 WO1996015985A1 (en) 1994-11-21 1995-11-16 Method for purification of calcium carbonate

Publications (2)

Publication Number Publication Date
MX9703753A MX9703753A (en) 1997-09-30
MXPA97003753A true MXPA97003753A (en) 1998-07-03

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