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WO2018048142A1 - Particule synthétique d'hydromagnésite et son procédé de production - Google Patents

Particule synthétique d'hydromagnésite et son procédé de production Download PDF

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Publication number
WO2018048142A1
WO2018048142A1 PCT/KR2017/009580 KR2017009580W WO2018048142A1 WO 2018048142 A1 WO2018048142 A1 WO 2018048142A1 KR 2017009580 W KR2017009580 W KR 2017009580W WO 2018048142 A1 WO2018048142 A1 WO 2018048142A1
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Prior art keywords
hydromagnesite
synthetic
magnesium
synthetic hydromagnesite
particle
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Ceased
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PCT/KR2017/009580
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English (en)
Korean (ko)
Inventor
임병길
박충효
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Dansuk Industrial Co Ltd
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Dansuk Industrial Co Ltd
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Priority to CN201780055908.4A priority Critical patent/CN109790043A/zh
Publication of WO2018048142A1 publication Critical patent/WO2018048142A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • 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
    • C01F5/00—Compounds of magnesium
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
    • 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

Definitions

  • the present invention relates to a synthetic hydromagnesite and a method for preparing the same. More specifically, to control the pH and reaction temperature of the reaction material, to control the excess ions generated during the synthesis by the addition of sodium hydroxide, to prevent the aggregation between the particles, high monodispersed synthetic hydromagnesite particles and its preparation method It is about.
  • Hydromagnesite is a hydrous carbonate mineral of magnesium, and its properties are low heat aqueous minerals that form veins among serpentine and altered igneous rocks rich in magnesium, and are confirmed to be mined and produced in Austria, California, and the like.
  • calcite, argonite, or weathering reactions are known, and the chemical formula is Mg 5 (OH) 2 (CO 3 ) 4 nH 2 O (n is 5 or less), and the crystallographic characteristic is known to be a monoclinic system.
  • the hydromagnesite is widely used as a flame retardant, a fire retardant additive for polymers, and an additive for spandex by mixing with huntite, and its amount of use is also gradually increasing.
  • Patent Document 1 discloses a crude raw material in a small amount of water and stirred to form a slurry, and the slurry is heated to almost a boiling point, and while stirring, the thermal slurry is mixed with cold water to produce a mixture having 75 ° F. or less, and in the suspension
  • this method is economical because the reaction temperature is too high and the reaction time is long. Since the hydromagnesite obtained is pulverized and sieved, a desired particle size can be obtained, and an organic solvent must be used for purification. Therefore, such a method is not used at present.
  • Patent Document 2 In the method for producing hydromagnesite obtained by precipitating hydromagnesite by a water-soluble salt containing magnesium and alkali metal carbonate by a double decomposition reaction, the precipitate is represented by the general formula M n + 2 P n O 3 n +1 (wherein M is an alkali metal, n is an integer of 1 or more), and a process for producing an improved hydromagnesium is characterized in that the reaction is carried out in the presence of 0.1 g to 10 g of the reaction medium of the crystallization improving agent selected. have.
  • the hydromagnesite obtained by this method has a great improvement due to its good fluidity, homogeneity, and apparent density, but its average particle size is 80-170 ⁇ m, its use is limited and its reaction time is too long. have.
  • Example 1 was suspended in high-purity magnesium hydroxide in an aqueous potassium hydroxide solution, into the suspension in the high pressure reactor, by introducing into the reactor the CO 2 gas at a high pressure to obtain a solution, the resulting solution was microwave oven To prepare hydromagnesite particles by heating at high current for 10 minutes.
  • This method has a long reaction time because carbon dioxide gas is used as a carbonate source, and magnesium hydroxide is mixed in the resulting hydromagnesite, which may be used for tobacco paper, but it may be used in fields requiring only hydromagnesite. It is difficult.
  • Patent Document 4 discloses slake at least one magnesium oxide feedstock selected from the group consisting of magnesium oxide, magnesiumsite, magnesium carbonate, magnesium hydroxide, brucite and mixtures thereof to convert magnesium oxide to magnesium hydroxide at least in part. Hydrogelesite by reacting gaseous CO 2 and / or carbonate-containing anions to at least partly convert to precipitated nesquchonite, and the obtained precipitated nesquhonite and precipitated calcium carbonate by heat aging. Disclosed is a method of preparing the same.
  • Patent Document 5 differs in that the magnesium oxide feedstock is expanded in Patent Document 4, and in the process of converting to Nesquchonite, the precipitated Nesquehonite further includes precipitated calcium carbonate, and other processes Almost similar. Therefore, the part pointed out as a problem with patent document 4 is judged to remain still.
  • Patent document 6 discloses "a method for producing magnesite and hydromagnesite, which comprises contacting a brucite with a CO 2 source at 15 to 40 ° C. for 2 to 25 hours at 15 to 40 ° C., especially at 16 to 20 ° C., in a medium of pH 13 or higher. It is starting. It is believed that the present invention employs that the use of a strong base material as a catalyst increases the reaction rate. However, the use of gaseous carbon dioxide has many restrictions on the reactor and reaction time, which is not preferable, and the reaction time is inevitably longer than the liquid phase reaction.
  • Patent Document 7 relates to a method for producing high purity hydromagnesite and magnesium oxide from brine containing magnesium chloride and calcium chloride, the claims of which a) provide a feedstock of magnesium chloride saline solution from the magnesium chloride source, Wherein the feedstock brine solution also comprises calcium chloride, b) mixing the sulfate with the feedstock brine solution to convert the calcium chloride to a calcium sulfate precipitate, c) removing the calcium sulfate precipitate from the brine solution, d) the temperature
  • the process for preparing hydromagnesite from a magnesium chloride source consisting of mixing the brine solution prepared in step c) with sodium carbonate to form a hydromagnesite precipitate while maintaining the temperature at about 20 to 120 ° C.
  • This patent invention is a method of producing hydromagnesite by reacting brine (sea water) with a sulfate ion feedstock compound to precipitate calcium sulfate and removing the resulting magnesium chloride with sodium carbonate to produce hydromagnesite. For many it seems to be undesirable. Moreover, since the final product is obtained in bulk, it is not advantageous because it involves a process that must be purified.
  • Patent document 8 discloses "a) providing a feedstock of a magnesium chloride brine solution from said magnesium chloride source, wherein the feedstock brine solution also comprises calcium chloride; b) mixing the sulfate with said feedstock brine solution to Converting the calcium chloride to a calcium sulfate precipitate; c) removing the calcium sulfate precipitate from the brine solution; d) ammonia the brine solution produced in step c) in a temperature range of about 20 ° C. to about 60 ° C. Converting magnesium chloride into at least partially magnesium hydroxide and forming ammonium chloride, and e) carbonating the magnesium hydroxide to form hydromagnesite precipitate while maintaining the reaction temperature at about 20-120 ° C.
  • This method has the advantage of using inexpensive brine, but it uses a number of processes from obtaining brine to magnesium hydroxide, which leads to higher manufacturing costs, and also dilutes magnesium chloride brine and The process of adding the diluted saline solution and then contacting the carbon dioxide gas under stirring is difficult to be economical due to the long reaction time.
  • Patent Document 9 discloses a composition for producing a chlorine-containing polyurethane urea elastic fiber containing 0.1 to 10% by weight of basic magnesium carbonate and an elastic fiber thereof.
  • basic magnesium carbonate synthetic hydromagnesite
  • Magnesium sulfate hydrate is mixed with anhydrous sodium carbonate aqueous solution, and it stirred for 1 hour at about 85 degreeC, and it reacts to obtain a basic carbonate compound, and it grind
  • Particles are aggregated to form an amorphous particle having an average particle diameter of 0.5 to 15 mu m.
  • the method for synthesizing hydromagnesite is not specifically described. Except for the foregoing, specific synthetic methods and chemical formulas of the hydromagnesite used are not described.
  • Patent documents 10 and 11 describe that there is excellent chlorine resistance when hydrotalcite is mixed with elastic polyurethane fibers. However, when the hydrotalcite component is mixed, the chlorine resistance is improved, but yellowing or the like occurs in the final urethane fiber, and it is proposed to use synthetic hydromagnesite as an alternative material.
  • Patent Literature 12 discloses a fiber in which chlorite resistance is improved by adding a huntite-synthetic hydromagnesite to a spandex fiber.
  • this document does not describe the synthesis of synthetic hydromagnesite or a method for preparing the same, which may be described by using synthetic hydromagnesite or huntite-synthetic hydromagnesite.
  • Patent Document 13 discloses a fiber in which chlorine resistance is improved by adding synthetic hydromagnesite to spandex fiber.
  • this document only describes surface treatment of synthetic hydromagnesite, i.e., coating with stearic acid and the like, and using a mixture thereof, and does not describe any preparation of synthetic hydromagnesite particles.
  • Patent Document 14 describes a spandex fiber containing an inorganic chlorine-resistant agent such as hydrotalcite, huntite and synthetic hydromagnesite, zinc oxide, magnesium oxide, and the like. However, this document does not specifically describe the synthesis of synthetic hydromagnesite and the like, but simply describes the purchase and use from the outside.
  • an inorganic chlorine-resistant agent such as hydrotalcite, huntite and synthetic hydromagnesite, zinc oxide, magnesium oxide, and the like.
  • Patent Document 15 describes a carbonic acid group-containing magnesium hydroxide particle and a method for producing the same, and merely a method for controlling the specific surface area of the synthetic hydromagnesite is merely presented, and a specific production method for controlling the particle shape and size is mentioned. Not.
  • Patent Document 1 US Patent No. 1,543,620
  • Patent Document 2 US Patent No.3.723,596
  • Patent Document 3 US Patent No.5.979,461
  • Patent Document 4 European Patent 2 322 581 B1
  • Patent Document 5 European Patent 2,496,648 B1
  • Patent Document 6 European Patent 2,692,691A1
  • Patent Document 7 WO 2015/154194 A1
  • Patent Document 8 WO 2015/154196 A1
  • Patent Document 9 Patent 10-0780602
  • Patent Document 10 US Patent No. 5,447,969
  • Patent Document 11 US Patent No. 6,353,049 B1
  • Patent Document 12 Patent 10-0870533
  • Patent Document 13 Published Patent 10-2009-0005802
  • Patent Document 14 WO 2011/040755
  • Patent Document 15 Patent No. 10-1354837
  • Conventional synthetic hydromagnesite has a particle size of 500 to 15,000 nm (0.5 to 15 ⁇ m), which is too large, and when it is pulverized and atomized, the particle shape is not uniform, resulting in uniform mixing with a raw resin such as spandex.
  • the specific surface area was small and chlorine resistance in the resin was not satisfactory.
  • the present inventors are repeatedly manufactured by modifying the conditions of the method by various modifications using sodium carbonate, potassium carbonate, or sodium bicarbonate and magnesium ion compounds according to the conventional method of hydrotalcite synthesis. saw.
  • the size of the hydromagnesite particle obtained was too large, the particle shape was obtained in plate shape, block shape, etc., and only the average specific surface area was about 5-10 m ⁇ 2> / g.
  • the required particle size can of course be obtained by grinding according to a conventional method, but it was not possible to have an increased specific surface area, and the grain size of the obtained particles was also obtained in an irregular shape due to grinding.
  • hydromagnesite having a small specific surface area and irregularly shaped granules adversely affects the physical properties of the final product obtained by mixing with other resins, and thus has a uniform and specific surface area that can be used in the art without crushing.
  • This large synthetic hydromagnesite has been desired.
  • the synthetic hydromagnesite according to the present invention has an average particle diameter in the range of 0.5 to 2.0 ⁇ m, a specific surface area of 20 to 55 m 2 / g, and does not require any additional grinding step, and the shape of the particles is also in the form of cogs and crackers. It is a plate-like shape, has good flowability, excellent miscibility with a polymer resin and a solvent, and excellent chlorine resistance.
  • FIG. 1 shows low and high magnification electron micrographs (SEM) of synthetic hydromagnesite synthesized in Comparative Example 1.
  • FIG. 3 is a spectrum showing the particle size distribution of the synthetic hydromagnesite particles synthesized in Comparative Example 1.
  • Figure 4 shows a low and high magnification electron micrograph (SEM) of the synthetic hydromagnesite synthesized in Comparative Example 2.
  • FIG. 5 shows low and high magnification electron micrographs (SEM) of the synthetic hydromagnesite synthesized in Example 1.
  • SEM magnification electron micrographs
  • Example 6 is an image pattern showing the X-ray diffraction intensity of the synthetic hydromagnesite synthesized in Example 1.
  • FIG. 7 is a spectrum showing the particle size distribution of the synthetic hydromagnesite particles synthesized in Example 1.
  • a synthetic hydromagnesite was obtained by coprecipitation reaction at a specific reaction temperature and pH.
  • the synthetic hydromagnesite produced by the present invention has the following characteristics.
  • the average particle diameter is 0.5-2.3 micrometers, and particle shape is a form in which the circular plate-shaped object with an uneven edge was laminated
  • the particles have a specific surface area of 20 to 55 m2 / g as measured by the BET method (used by BELSORP-MAX).
  • carbonates of alkali metals such as sodium carbonate, sodium bicarbonate or potassium carbonate can be used, and as magnesium ions, magnesium oxide, magnesium hydroxide, magnesium chloride, magnesium sulfate, magnesium nitrate Can be used.
  • magnesium ion magnesium sulfate is preferable.
  • the reaction is preferably performed at 0.5 to 6 hours, more preferably 0.5 to 3 hours.
  • the sulfate group (SO 4 -2 ) of magnesium sulfate must be combined with sodium ions (Na + ) to produce a stable salt as a by-product. do. Otherwise, SO 4_ 2 will prevent Mg +2 from forming hydromagnesite particles.
  • SO 4 - 2 ion is responsible for the destabilization by surface charge, the generated synthetic hydro magnesite particle surface induced aggregation.
  • the 2 SO 4- ions produced in the reaction by-products can be neutralized by improving the input-stage dispersion of the particles by the Na + ions, where to put the NaOH to form the OH -1 ions synthetic hydro magnesite of NaOH It acts as a hydroxyl supply, which doubles the rate of particle formation and stabilizes the particles.
  • the concentration of the reactants is not particularly limited, but is preferably about 30% by weight or less, more preferably 20% by weight or less in consideration of the solubility of the reactants.
  • the hydromagnesite of the present invention prepared under the above conditions shows a large difference in particle size, particle size distribution, specific surface area, etc., compared to that prepared according to the conventional method.
  • the hydromagnesite synthesized according to the conventional method has a particle diameter of 5 to 15 ⁇ m, an average particle size distribution of about 15 to 40 ⁇ m, a specific surface area of 5 to 10 m 2 / g, and a granularity as shown in FIG. It can be seen that the aggregates and plate-like form.
  • the hydromagnesite produced according to the present invention has a particle size of 0.5 to 3.0 mu m, an average particle size distribution of about 1.8 to 1.9 mu m, and a specific surface area of about 30 to 50 m 2 / g. Therefore, it can be seen that the particles are smaller than those commercially available and are excellent in blendability with resins such as polyurethane and excellent in chlorine resistance.
  • the synthetic hydromagnesite obtained above is surface treated in an amount of 0.5 to 10% by weight relative to the synthetic hydromagnesite by a conventional method in the art, such as alkali metal salts of alkali metal salts such as stearic acid or oleic acid salts and surfactants and the like. Can be used.
  • a 5 mol aqueous solution of magnesium sulfate was prepared in a 5 L raw material tank.
  • a 4 mol aqueous solution of sodium carbonate was separately prepared, and the magnesium sulfate aqueous solution was added over about 15 minutes while stirring.
  • An aqueous sodium hydroxide solution was added dropwise to the reaction to react for 1 hour while maintaining the pH of the reaction solution at 10.89.
  • Synthetic hydromagnesite was obtained by reacting in the same manner as in Example 1 with the reactants described in Table 1, the pH of the reactants, and the raw material input time. The particle size of the obtained synthetic hydromagnesite is described together.
  • Example 2 Example 3 Comparative Example 1 Comparative Example 2 Comparative Example 3 MgSO 4 5 mall 5 mall 5 mall 5 mall 5 mall Na 2 CO 3 4 mall 4 mall 4 mall 4 mall 4 mall 4 mall PH of the reactants 10.54 10.28 9.12 *) 9.61 11.20 Reaction temperature 85 °C 85 °C 85 °C 85 °C Raw material input time 15 minutes 15 minutes 15 minutes 15 minutes 15 minutes 15 minutes Reaction time 1h 1h 1h 1h Particle size ( ⁇ m) 1.87 1.49 13.07 5.72 4.34
  • Comparative Example 1 is a result of synthesis without adjusting the pH of the reactants with an aqueous sodium hydroxide solution.
  • FIGS. 1 to 4 An electron micrograph (SEM) image, an X-ray diffraction (XRD) image pattern, and a particle size distribution diagram of the synthetic hydromagnesite obtained in the comparative example are shown in FIGS. 1 to 4.
  • the synthetic hydromagnesite of the present invention has a smaller particle size, a smaller particle size distribution and uniformity than those of the comparative example, and does not need to be separately ground when used, and it can be confirmed that it is advantageous for raw material blending.
  • the excellent properties of the hydromagnesite of the present invention can be obtained by adjusting the pH using a base such as sodium hydroxide in the carbonate and magnesium ion solution.
  • Hydromagnesite prepared according to the method of the present invention described above has an average particle diameter in the range of 0.5 to 2.0 ⁇ m, a specific surface area of 20 to 55 m 2 / g, and does not require an additional grinding step. Since it is excellent in mixing property with raw material resin, it is excellent in chlorine resistance, its particle

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)

Abstract

L'invention concerne une particule d'hydromagnésite synthétique et son procédé de production, la particule d'hydromagnésite synthétique étant caractérisée par les caractéristiques (1) à (3) suivantes : (1) formule générale Mg3.8 - 5.2(OH)1.8 - 2.15(CO3)3.7 - 4.2 ·mH2O (où m est 0 à 5); (2) l'hydromagnésite synthétique a une taille de particule moyenne de 0,5 à 2,3 µm, et la particule a une forme dans laquelle des matériaux de type plaque ayant des bords irréguliers sont empilés dans plusieurs directions; et (3) la particule d'hydromagnésite synthétique a une surface spécifique de 20 à 55 ㎡/g telle que mesurée par un procédé BET.
PCT/KR2017/009580 2016-09-12 2017-09-01 Particule synthétique d'hydromagnésite et son procédé de production Ceased WO2018048142A1 (fr)

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KR102112572B1 (ko) * 2019-10-01 2020-05-19 한국지질자원연구원 마그네사이트 광석으로부터 수산화마그네슘 분말의 제조 방법 및 수득된 수산화마그네슘 분말
CN111285407A (zh) * 2020-02-23 2020-06-16 武汉工程大学 以高镁磷尾矿为原料制备钙镁铝铁水滑石的方法

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US20150044469A1 (en) * 2012-03-22 2015-02-12 S.A. Lhoist Recherche Et Developpement Mineral Composition Made From A Mixed Solid Phase of Calcium and Magnesium Carbonates, Method of Preparing Same and Use Thereof
KR20160060760A (ko) * 2013-10-29 2016-05-30 조인트 스탁 컴퍼니 카우스티크 수산화마그네슘 내연성 나노입자 및 이의 생산 방법

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