KR20190086145A - Preparation method of the high activated calcium by sonochemistry - Google Patents
Preparation method of the high activated calcium by sonochemistry Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title description 5
- 150000001669 calcium Chemical class 0.000 title 1
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 63
- FNAQSUUGMSOBHW-UHFFFAOYSA-H calcium citrate Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O.[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O FNAQSUUGMSOBHW-UHFFFAOYSA-H 0.000 claims abstract description 43
- 239000001354 calcium citrate Substances 0.000 claims abstract description 36
- 235000013337 tricalcium citrate Nutrition 0.000 claims abstract description 36
- MKJXYGKVIBWPFZ-UHFFFAOYSA-L calcium lactate Chemical compound [Ca+2].CC(O)C([O-])=O.CC(O)C([O-])=O MKJXYGKVIBWPFZ-UHFFFAOYSA-L 0.000 claims abstract description 35
- 239000001527 calcium lactate Substances 0.000 claims abstract description 32
- 229960002401 calcium lactate Drugs 0.000 claims abstract description 32
- 235000011086 calcium lactate Nutrition 0.000 claims abstract description 32
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 31
- 238000004519 manufacturing process Methods 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 22
- -1 organic acid calcium salt Chemical class 0.000 claims abstract description 20
- 230000001678 irradiating effect Effects 0.000 claims abstract description 16
- 238000002156 mixing Methods 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000000203 mixture Substances 0.000 claims abstract description 12
- 150000007524 organic acids Chemical class 0.000 claims abstract description 11
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000000292 calcium oxide Substances 0.000 claims abstract description 6
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000002904 solvent Substances 0.000 claims abstract description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 34
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 22
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 16
- 238000001035 drying Methods 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 9
- 239000004310 lactic acid Substances 0.000 claims description 8
- 235000014655 lactic acid Nutrition 0.000 claims description 8
- 239000006228 supernatant Substances 0.000 claims description 6
- 229940043430 calcium compound Drugs 0.000 claims description 3
- 150000001674 calcium compounds Chemical class 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 3
- JVTAAEKCZFNVCJ-REOHCLBHSA-N L-lactic acid Chemical compound C[C@H](O)C(O)=O JVTAAEKCZFNVCJ-REOHCLBHSA-N 0.000 claims 2
- WQNHWIYLCRZRLR-UHFFFAOYSA-N 2-(3-hydroxy-2,5-dioxooxolan-3-yl)acetic acid Chemical compound OC(=O)CC1(O)CC(=O)OC1=O WQNHWIYLCRZRLR-UHFFFAOYSA-N 0.000 claims 1
- 229930182843 D-Lactic acid Natural products 0.000 claims 1
- JVTAAEKCZFNVCJ-UWTATZPHSA-N D-lactic acid Chemical compound C[C@@H](O)C(O)=O JVTAAEKCZFNVCJ-UWTATZPHSA-N 0.000 claims 1
- 229940022769 d- lactic acid Drugs 0.000 claims 1
- 235000005985 organic acids Nutrition 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 5
- 159000000007 calcium salts Chemical class 0.000 abstract 1
- 150000001875 compounds Chemical class 0.000 abstract 1
- 239000011259 mixed solution Substances 0.000 description 12
- 239000000243 solution Substances 0.000 description 11
- 239000011575 calcium Substances 0.000 description 10
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 8
- 229960004543 anhydrous citric acid Drugs 0.000 description 8
- 229960005069 calcium Drugs 0.000 description 8
- 229910052791 calcium Inorganic materials 0.000 description 8
- 238000002604 ultrasonography Methods 0.000 description 8
- 239000002245 particle Substances 0.000 description 7
- 239000007858 starting material Substances 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 230000009257 reactivity Effects 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 229960004106 citric acid Drugs 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000012153 distilled water Substances 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 241001465754 Metazoa Species 0.000 description 2
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 238000003795 desorption Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 238000002203 pretreatment Methods 0.000 description 2
- 238000000197 pyrolysis Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- WHQOKFZWSDOTQP-UHFFFAOYSA-N 2,3-dihydroxypropyl 4-aminobenzoate Chemical compound NC1=CC=C(C(=O)OCC(O)CO)C=C1 WHQOKFZWSDOTQP-UHFFFAOYSA-N 0.000 description 1
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 1
- 241000242678 Schistosoma Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 210000004556 brain Anatomy 0.000 description 1
- 235000010216 calcium carbonate Nutrition 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000004227 calcium gluconate Substances 0.000 description 1
- 229960004494 calcium gluconate Drugs 0.000 description 1
- 235000013927 calcium gluconate Nutrition 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 235000011116 calcium hydroxide Nutrition 0.000 description 1
- 229910001424 calcium ion Inorganic materials 0.000 description 1
- 239000001506 calcium phosphate Substances 0.000 description 1
- 229910000389 calcium phosphate Inorganic materials 0.000 description 1
- 235000011010 calcium phosphates Nutrition 0.000 description 1
- 235000011132 calcium sulphate Nutrition 0.000 description 1
- NEEHYRZPVYRGPP-UHFFFAOYSA-L calcium;2,3,4,5,6-pentahydroxyhexanoate Chemical compound [Ca+2].OCC(O)C(O)C(O)C(O)C([O-])=O.OCC(O)C(O)C(O)C(O)C([O-])=O NEEHYRZPVYRGPP-UHFFFAOYSA-L 0.000 description 1
- QXDHJHQRJCJRAU-UHFFFAOYSA-N calcium;2-hydroxypropane-1,2,3-tricarboxylic acid Chemical group [Ca].OC(=O)CC(O)(C(O)=O)CC(O)=O QXDHJHQRJCJRAU-UHFFFAOYSA-N 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 235000013373 food additive Nutrition 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- 235000013376 functional food Nutrition 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000003921 particle size analysis Methods 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000021749 root development Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 238000002411 thermogravimetry Methods 0.000 description 1
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/41—Preparation of salts of carboxylic acids
- C07C51/412—Preparation of salts of carboxylic acids by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01K—ANIMAL HUSBANDRY; AVICULTURE; APICULTURE; PISCICULTURE; FISHING; REARING OR BREEDING ANIMALS, NOT OTHERWISE PROVIDED FOR; NEW BREEDS OF ANIMALS
- A01K1/00—Housing animals; Equipment therefor
- A01K1/02—Pigsties; Dog-kennels; Rabbit-hutches or the like
- A01K1/03—Housing for domestic or laboratory animals
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01K—ANIMAL HUSBANDRY; AVICULTURE; APICULTURE; PISCICULTURE; FISHING; REARING OR BREEDING ANIMALS, NOT OTHERWISE PROVIDED FOR; NEW BREEDS OF ANIMALS
- A01K29/00—Other apparatus for animal husbandry
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/10—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing sonic or ultrasonic vibrations
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C59/00—Compounds having carboxyl groups bound to acyclic carbon atoms and containing any of the groups OH, O—metal, —CHO, keto, ether, groups, groups, or groups
- C07C59/01—Saturated compounds having only one carboxyl group and containing hydroxy or O-metal groups
- C07C59/08—Lactic acid
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C59/00—Compounds having carboxyl groups bound to acyclic carbon atoms and containing any of the groups OH, O—metal, —CHO, keto, ether, groups, groups, or groups
- C07C59/235—Saturated compounds containing more than one carboxyl group
- C07C59/245—Saturated compounds containing more than one carboxyl group containing hydroxy or O-metal groups
- C07C59/265—Citric acid
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- Animal Husbandry (AREA)
- Biodiversity & Conservation Biology (AREA)
- General Health & Medical Sciences (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Clinical Laboratory Science (AREA)
- Animal Behavior & Ethology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
Description
본 발명은 높은 이온화도를 갖는 유기산 칼슘염의 제조방법에 관한 것으로, 보다 상세하게는 출발물질인 탄산칼슘의 입자크기를 나노 크기로 줄여줌으로써 반응성을 향상시키기 위한 전처리 단계를 거쳐 칼슘의 이온화 농도를 증가시키고 물에 용해가 잘되어 칼슘의 흡수를 더 잘되게 하고, 제조 비용과 시간을 현저히 단축시킬 수 있는 높은 이온화도를 갖는 유기산 칼슘염의 제조에 관한 것이다.The present invention relates to a method for producing an organic acid calcium salt having a high ionization degree, and more particularly, to a method for producing an organic acid calcium salt having a high ionization degree by increasing the ionization concentration of calcium through a pretreatment step for reducing reactivity by reducing the particle size of calcium carbonate, The present invention relates to the production of an organic acid calcium salt having high ionization degree which can dissolve in water so that calcium is absorbed more easily, and production cost and time are remarkably shortened.
칼슘은 각종 생명체의 구성과 활동에 필수적인 미네랄 성분 중 하나이다. 동물의 경우 뼈와 혈액의 조성 및 생성에 필요한 성분일 뿐만 아니라 심장이나 뇌의 정보전달의 기능을 담당한다. 식물에 있어서 칼슘은 분열 조직의 생장 및 뿌리 발육에 중요한 요소이다. 칼슘은 동식물의 생명체 활성 유지에 중요한 역할을 하는 요소로서, 건강기능 식품이나 식품첨가물 등 다양한 용도로 사용되고 있다. 특히 현재 칼슘이온을 이용한 다양한 기능성 화장품으로서의 응용과 연구가 활발하게 이루어지고 있다. Calcium is one of the minerals essential for the composition and activity of various organisms. Animal is not only a necessary component for the formation and production of bones and blood, but also the function of information transmission in the heart and brain. In plants, calcium is an important factor in the growth and root development of schistosomes. Calcium plays an important role in the maintenance of living organism activity of animals and plants, and is used in diverse uses such as health functional foods and food additives. Particularly, application and research as various functional cosmetics using calcium ion are being actively carried out.
다양한 용도에 적합하게 사용되기 위해서는 칼슘의 용해 속도가 빠르고 그 이온화도가 높아야 한다. 현재 다양한 형태의 칼슘화합물이 사용되고 있는데, 탄산칼슘, 구연산칼슘, 글루콘산칼슘, 젖산칼슘, 인산칼슘, 수산화칼슘, 황산칼슘 등이 사용되고 있다. 그 중에 구연산칼슘과 젖산칼슘이 고이온화도를 갖는 특징이 있어 그 제조방법에 많은 관심을 가지고 있다. In order to be suitable for various applications, the dissolution rate of calcium should be fast and its ionization degree should be high. Currently, various forms of calcium compounds are used, including calcium carbonate, calcium citrate, calcium gluconate, calcium lactate, calcium phosphate, calcium hydroxide, and calcium sulfate. Among them, calcium citrate and calcium lactate have a high ionization degree, and thus there is a great deal of interest in the production method thereof.
예를 들어, 대한민국 등록특허 제10-1683150호에는 구연산칼슘의 제조방법이 개시되어 있으며, 구체적으로는 물에 구연산과 탄산칼슘을 녹여서 혼합물을 만들고 에탄올을 첨가하여 48 시간 동안 숙성시켜서 구연산칼슘을 제조하는 방법을 개시하고 있다. 그러나 장시간 숙성해야 하는 문제점을 가지고 있다.For example, Korean Patent No. 10-1683150 discloses a method for producing calcium citrate. More specifically, citric acid and calcium carbonate are dissolved in water to prepare a mixture. Then, ethanol is added thereto and aged for 48 hours to prepare calcium citrate A method is disclosed. However, it has a problem of aging for a long time.
이에 따라 높은 이온화도를 보이고 간단한 공정과 짧은 시간에 제조하는 기술이 요구되고 있다As a result, there is a demand for a simple process and a technique for manufacturing in a short time with a high ionization degree
이에 본 발명자들은 기존의 유기산 칼슘염을 제조하는 방법이 갖는 문제점을 극복하기 위한 연구를 진행하던 중, 초음파를 이용하여 유기산 칼슘염을 제조할 경우 초음파 전처리를 통해 출발 물질의 크기를 줄여 비표면적을 넓힘에 따라 반응성이 매우 높아지면서 기존의 제조방법보다 합성시간이 10분 내외로 매우 빠르며, 이로부터 제조된 유기산 칼슘염은 이온화도가 기존의 제조방법보다 매우 높은 값을 보이고 있음을 발견하였다. Accordingly, the inventors of the present invention have conducted research to overcome the problems of the conventional method of preparing an organic acid calcium salt. When preparing an organic acid calcium salt by using ultrasonic waves, the inventors have reduced the size of the starting material by ultrasonic pretreatment, It was found that the synthesis time of the organic acid calcium salt was very fast as compared with that of the conventional preparation method and the ionization degree of the prepared organic acid calcium salt was much higher than that of the conventional preparation method.
본 발명의 일 목적은 높은 이온화도를 갖는 유기산 칼슘염의 제조방법을 제공하는데 있다.It is an object of the present invention to provide a method for producing an organic acid calcium salt having a high ionization degree.
상기의 목적을 달성하기 위하여,In order to achieve the above object,
본 발명의 일 측면은 탄산칼슘 및 산화칼슘으로 이루어지는 군으로부터 선택되는 1종 이상을 용매에 혼합하고 초음파를 조사하여 전처리를 하는 단계; 상기 단계에서 형성된 용액에 유기산을 혼합하여 혼합물을 형성하는 단계; 및 상기 유기산을 혼합하여 형성된 혼합물에 초음파를 조사하는 단계; 를 포함하는 것을 특징으로 하는 유기산 칼슘염 제조방법을 제공한다.According to an aspect of the present invention, there is provided a method of manufacturing a semiconductor device, comprising: mixing at least one member selected from the group consisting of calcium carbonate and calcium oxide in a solvent and conducting pretreatment by irradiating ultrasonic waves; Mixing the solution formed in the step with an organic acid to form a mixture; And irradiating ultrasound to the mixture formed by mixing the organic acid; And a salt of an organic acid.
본 발명의 일 측면에 따르면, 기존의 제조법에 의해 제조된 유기산 칼슘염에 비해 이온화도가 높고 매우 쉽게 물에 용해되는 유기산 칼슘염을 제공할 수 있고, 이 때 제조 시간은 10분 내외로 매우 빠른 시간에 합성할 수 있는 효과가 있다. According to one aspect of the present invention, there is provided an organic acid calcium salt which has a higher ionization degree and is very easily dissolved in water, as compared with the organic acid calcium salt prepared by the conventional production method. In this case, Can be synthesized.
도 1은 초음파 합성법에 의하여 제조되는 유기산 칼슘염의 제조공정에 대한 모식도이고,
도 2는 초음파 전처리 전후의 탄산 칼슘의 입자사이즈의 분포도 결과값이고,
도 3은 본 발명의 실시예에 의하여 제조된 구연산칼슘과 젖산칼슘의 X-선 회절분석 그래프이고,
도 4는 본 발명의 실시예에 의하여 제조된 구연산칼슘과 젖산칼슘의 열중량분석을 나타낸 것이다.1 is a schematic view of a process for producing an organic acid calcium salt prepared by an ultrasonic synthesis method,
FIG. 2 is a result of the distribution of particle size of calcium carbonate before and after pretreatment with ultrasonic waves,
3 is an X-ray diffraction analysis graph of calcium citrate and calcium lactate produced according to an embodiment of the present invention,
FIG. 4 shows the thermogravimetric analysis of calcium citrate and calcium lactate produced according to an embodiment of the present invention.
높은 이온화도를 갖는 유기산 칼슘염의 제조방법에 관한 것이다. 이하에서 본 발명을 구체적으로 설명한다.And a method for producing an organic acid calcium salt having a high ionization degree. Hereinafter, the present invention will be described in detail.
본 발명의 일 측면은 높은 이온화도를 갖는 유기산 칼슘염을 제조하는데 있어, 구연산칼슘 또는 젖산칼슘을 초음파를 이용하여 빠른 시간에 제조하는 제조방법을 제공한다.One aspect of the present invention provides a method for producing calcium citrate or calcium lactate using ultrasonic waves in a short time in manufacturing an organic acid calcium salt having a high ionization degree.
본 발명의 일 실시예에 따른 구연산칼슘의 제조방법은 출발물질인 탄산칼슘에 초음파 전처리를 거쳐 입자사이즈를 줄이고 무수구연산을 혼합하여 혼합물을 만들고 초음파를 조사하여 제조한다.The method of preparing calcium citrate according to one embodiment of the present invention is prepared by ultrasonically pretreating calcium carbonate, which is a starting material, by reducing particle size and mixing anhydrous citric acid to prepare a mixture and irradiating ultrasonic waves.
도 1은 본 발명의 일 실시예에 따른 구연산칼슘의 제조방법의 모식도이다.1 is a schematic view of a method for producing calcium citrate according to an embodiment of the present invention.
탄산칼슘 및 산화칼슘으로 이루어지는 군으로부터 선택되는 1종 이상을 용매에 혼합하고 초음파를 조사하여 전처리를 하는 단계;Mixing at least one member selected from the group consisting of calcium carbonate and calcium oxide in a solvent and irradiating ultrasonic waves to perform pre-treatment;
상기 단계에서 형성된 용액에 무수구연산을 용해시켜 혼합용액을 제조하는 단계; 및Dissolving anhydrous citric acid in the solution formed in the above step to prepare a mixed solution; And
상기 무수구연산을 용해시켜 제조된 혼합용액에 초음파를 조사하는 단계;를 포함하는 방법으로 구연산칼슘을 제조할 수 있다. And a step of irradiating ultrasound to the mixed solution prepared by dissolving the anhydrous citric acid to prepare calcium citrate.
상기 전처리 단계에서의 용매는 물 및 에탄올을 사용하는 것이 바람직하며, 에탄올을 사용하지 않고 물만을 사용하는 경우에는, 반응물이 용해된 상태로서 유기산 칼슘염이 석출될 수 없고, 물 및 에탄올을 혼합하여야 반응과 동시에 유기산 칼슘이 석출되는 효과를 나타낸다.In the pretreatment step, water and ethanol are preferably used. When only water is used without using ethanol, the organic acid calcium salt can not be precipitated as the reactant is dissolved, and water and ethanol are mixed And exhibits an effect of precipitating calcium carbonate at the same time as the reaction.
또한, 상기 전처리 단계의 초음파는 1 내지 100kHz 강도로 조사되는 것이 바람직하다.It is preferable that the ultrasonic wave in the pre-treatment step is irradiated at an intensity of 1 to 100 kHz.
상기 전처리 단계 의 초음파 강도는 1 내지 100kHz 강도로 1분-60분의 시간범위 내에서 조사할 수 있고, 구체적으로는 20kHz의 강도로 1분-10분의 시간범위 내에서 조사할 수 있으며, 더욱 구체적으로는 20kHz의 강도로 3분-5분의 시간범위 내에서 조사될 수 있다.The ultrasonic intensity in the pretreatment step can be irradiated within a time range of 1 to 60 minutes at an intensity of 1 to 100 kHz, specifically, within a time range of 1 to 10 minutes at an intensity of 20 kHz, Specifically, it can be irradiated at an intensity of 20 kHz within a time range of 3 minutes to 5 minutes.
만약, 초음파가 1kHz미만의 강도로 조사될 경우, 초음파 조사가 충분히 이루어지지 않아 원하는 크기의 탄산칼슘이 제조되지 않는 문제점이 있고, 100kHz 초과의 강도로 조사될 경우, 초음파조사에 의한 열 때문에 탄산칼슘이 순간적으로 용해될 뿐 상온에서 다시 원래 크기의 탄산칼슘을 형성하는 문제점이 있다.If the ultrasonic wave is irradiated at a strength of less than 1 kHz, ultrasonic irradiation is not sufficiently carried out and calcium carbonate of a desired size can not be produced. If irradiated with a strength of more than 100 kHz, calcium carbonate There is a problem that calcium carbonate is originally formed again at room temperature.
또한, 상기 무수구연산을 용해시켜 제조된 혼합용액에 초음파를 조사하는 단계의 초음파는 2 내지 200kHz 강도로 조사되는 것이 바람직하다.In addition, it is preferable that the ultrasonic wave irradiated to the mixed solution prepared by dissolving the anhydrous citric acid is irradiated at an intensity of 2 to 200 kHz.
상기 무수구연산을 용해시켜 제조된 혼합용액에 초음파를 조사하는 단계의 초음파 강도는 2 내지 200kHz 강도로 5분-12시간의 시간범위 내에서 조사할 수 있고, 구체적으로는 20kHz의 강도로 5분-1시간의 시간범위 내에서 조사할 수 있으며, 더욱 구체적으로는 20kHz의 강도로 10분-20분의 시간범위 내에서 조사될 수 있다.The ultrasonic intensity of the step of irradiating ultrasonic waves to the mixed solution prepared by dissolving the anhydrous citric acid can be irradiated within a time range of 5 to 12 hours at an intensity of 2 to 200 kHz, 1 hour, and more specifically, within a time range of 10 minutes to 20 minutes at an intensity of 20 kHz.
만약, 초음파가 2kHz미만의 강도로 조사될 경우, 초음파 조사가 충분히 이루어지지 않아 원하는 형태의 구연산칼슘이 제조되지 않는 문제점이 있고, 200kHz 초과의 강도로 조사될 경우, 초음파조사에 의한 열 때문에 구연산칼슘이 응집되어 집합체를 형성하는 문제점이 발생할 수 있다.If the ultrasonic wave is irradiated at a strength of less than 2 kHz, ultrasonic irradiation is not sufficiently performed and calcium citrate in a desired form can not be produced. When irradiated at a strength of more than 200 kHz, calcium citrate May aggregate to form aggregates.
나아가, 상기 무수구연산을 용해시켜 제조된 혼합용액에 초음파를 조사하는 단계를 수행한 후 구연산칼슘을 세척 및 건조하는 단계를 더 수행할 수 있다.Further, the step of irradiating ultrasound to the mixed solution prepared by dissolving the anhydrous citric acid may be further followed by washing and drying the calcium citrate.
이하, 상기 제조방법을 단계별로 상세히 설명한다.Hereinafter, the manufacturing method will be described step by step.
상기 세척 및 건조 단계는 상기 무수구연산을 용해시켜 제조된 혼합용액에 초음파를 조사하는 단계를 수행한 후 반응용액에서 구연산칼슘을 세척 및 건조하는 단계이다.The washing and drying step is a step of irradiating ultrasound to the mixed solution prepared by dissolving the anhydrous citric acid, and washing and drying the calcium citrate in the reaction solution.
구체적으로, 상기 무수구연산을 용해시켜 제조된 혼합용액에 초음파를 조사하는 단계를 수행한 후 반응용액 내에 있는 구연산칼슘을 원심분리에 의하여 분리할 수 있고, 에탄올을 이용하여 세척 및 원심분리를 3회 이상 수행함으로써 분말의 회수가 가능하다.Specifically, the step of irradiating ultrasonic waves to the mixed solution prepared by dissolving the anhydrous citric acid, the calcium citrate in the reaction solution can be separated by centrifugation, and the washing and centrifugation using ethanol are repeated three times It is possible to recover the powder.
상기 세척 및 건조 단계의 건조온도는 특별히 제한된 것은 아니나, 30 내지 150℃의 온도에서 수행할 수 있고, 구체적으로는 50 내지 120℃의 온도에서 수행할 수 있고, 더욱 구체적으로는 50 내지 100℃의 온도에서 수행할 수 있고, 보다 구체적으로는 70℃의 온도에서 수행할 수 있다.The drying temperature of the washing and drying step is not particularly limited but may be carried out at a temperature of 30 to 150 ° C, specifically 50 to 120 ° C, more specifically 50 to 100 ° C Temperature, more specifically at a temperature of 70 < 0 > C.
상기 세척 및 건조 단계의 건조시간은 특별히 제한된 것은 아니나, 1 내지 20시간 동안 수행할 수 있고, 구체적으로는 3 내지 18시간 동안 수행할 수 있고, 더욱 구체적으로는 4 내지 10시간 동안 수행할 수 있고, 보다 구체적으로는 5시간 동안 수행할 수 있다.The drying time of the washing and drying step is not particularly limited, but may be 1 to 20 hours, specifically 3 to 18 hours, more specifically 4 to 10 hours , ≪ / RTI > more specifically 5 hours.
또한, 도 1은 본 발명의 실시예에 따른 젖산칼슘의 제조방법의 모식도이다.1 is a schematic diagram of a method for producing calcium lactate according to an embodiment of the present invention.
탄산칼슘 및 산화칼슘으로 이루어지는 군으로부터 선택되는 1종 이상을 용매에 혼합하여 초음파 전처리를 하는 단계;Mixing at least one member selected from the group consisting of calcium carbonate and calcium oxide in a solvent to perform ultrasonic pretreatment;
상기 전처리 단계의 용액에 젖산을 용해시켜 혼합용액을 제조하는 단계; 및Dissolving lactic acid in the solution of the pretreatment step to prepare a mixed solution; And
상기 젖산을 용해시켜 제조한 혼합용액에 초음파를 조사하는 단계;를 포함하는 방법으로 젖산칼슘을 제조할 수 있다.And irradiating ultrasound to the mixed solution prepared by dissolving the lactic acid, thereby preparing calcium lactate.
자세한 제조방법은 상기 구연산칼슘 제조에 언급되어 있는 내용과 동일하다.The detailed production method is the same as that mentioned in the production of calcium citrate.
이하에서는 실시예 및 실험예를 통하여 본 발명을 더욱 상세하게 설명한다. 그러나, 이하의 실시예 및 실험예는 본 발명의 설명을 위한 예일 뿐, 본 발명의 권리범위가 이하의 실시예 및 실험예에 의하여 한정되는 것은 아니다.Hereinafter, the present invention will be described in more detail with reference to Examples and Experimental Examples. However, the following examples and experimental examples are only illustrative of the present invention, and the scope of the present invention is not limited by the following examples and experimental examples.
<실시예 1> ≪ Example 1 >
구연산칼슘의Of calcium citrate 제조 Produce
탄산칼슘 5 mmol을 5 mL 증류수와 10 mL 에탄올이 들어있는 용기에 넣고 초음파 조사기를 이용하여 5분간 20kHz(50%)강도의 초음파를 조사하여 전처리한 후, 전처리한 용액에 구연산 23.4 mmol를 용해하고 10분간 20kHz(50%)강도의 초음파를 조사하였다. 5 mmol of calcium carbonate was placed in a container containing 5 mL of distilled water and 10 mL of ethanol and pretreated by applying ultrasonic waves of 20 kHz (50%) intensity for 5 minutes using an ultrasonic wave irradiator. Then, 23.4 mmol of citric acid was dissolved in the pretreated solution Ultrasonic waves of 20 kHz (50%) intensity were irradiated for 10 minutes.
상기 전처리 과정에서 초음파를 조사함에 따라 10 μm이던 탄산칼슘의 입자 사이즈가 100-200 nm의 크기로 줄어드는 것을 관찰할 수 있었는데, 이는 탄산칼슘의 비표면적이 더 커지면서 반응성이 매우 높아진다는 것을 의미한다.As the ultrasound was irradiated in the pretreatment process, it was observed that the particle size of calcium carbonate, which was 10 μm, decreased to 100-200 nm, which means that the specific surface area of calcium carbonate becomes larger and reactivity becomes higher.
또한, 전처리한 탄산칼슘 용액에 젖산을 용해시켜 초음파를 조사함에 따라 초기 투명하던 용액이 시간이 지남에 따라 뿌옇게 바뀌는 것을 관찰할 수 있었는데, 이것은 구연산칼슘이 성공적으로 합성되었다는 것을 의미한다.Also, by dissolving lactic acid in the pretreated calcium carbonate solution and irradiating ultrasonic waves, it was observed that the initially transparent solution changed to a puddle over time, indicating that calcium citrate was successfully synthesized.
상기 구연산칼슘이 제조된 혼합용액에 과량의 에탄올을 첨가하고, 원심분리를 하여 구연산칼슘과 상층액을 분리하여 상층액은 제거하는 세척과정은 최소 3회 이상 반복하였고, 침전물은 70℃에서 5시간 건조하여 구연산칼슘 분말을 얻었다.Excess ethanol was added to the calcium citrate mixed solution, centrifuged to separate the calcium citrate and supernatant, and the supernatant was removed at least three times. The precipitate was centrifuged at 70 ° C for 5 hours And dried to obtain a calcium citrate powder.
<실시예 2>≪ Example 2 >
젖산칼슘의Of calcium lactate 제조 Produce
탄산칼슘 5 mmol을 5 mL 증류수와 10 mL 에탄올이 들어있는 용기에 넣고 초음파 조사기를 이용하여 5분간 20kHz(50%)강도의 초음파를 조사하여 전처리한 후, 전처리한 용액에 젖산 10 mmol를 넣고 교반하면서 혼합용액을 제조한 다음, 초음파 조사기를 이용하여 10분간 20kHz(50%)강도의 초음파를 조사하였다. 5 mmol of calcium carbonate was placed in a vessel containing 5 mL of distilled water and 10 mL of ethanol and pretreated by applying ultrasonic waves of 20 kHz (50%) intensity for 5 minutes using an ultrasonic wave irradiator. 10 mmol of lactic acid was added to the pretreated solution, , And ultrasonic waves of 20 kHz (50%) intensity were irradiated for 10 minutes using an ultrasonic wave irradiator.
상기 전처리 과정에서 초음파를 조사함에 따라 10 μm이던 탄산칼슘의 입자 사이즈가 100-200 nm의 크기로 줄어드는 것을 관찰할 수 있었는데, 이는 탄산칼슘의 비표면적이 더 커지면서 반응성이 매우 높아진다는 것을 의미한다.As the ultrasound was irradiated in the pretreatment process, it was observed that the particle size of calcium carbonate, which was 10 μm, decreased to 100-200 nm, which means that the specific surface area of calcium carbonate becomes larger and reactivity becomes higher.
또한, 전처리한 탄산칼슘 용액에 젖산을 용해시켜 초음파를 조사함에 따라 초기 투명하던 용액이 시간이 지남에 따라 뿌옇게 바뀌는 것을 관찰할 수 있었는데, 이것은 젖산칼슘이 성공적으로 합성되었다는 것을 의미한다.Also, by dissolving lactic acid in the pretreated calcium carbonate solution and irradiating it with ultrasonic waves, it was observed that the initial transparent solution was swollen with time, indicating that calcium lactate was successfully synthesized.
상기 젖산칼슘이 제조된 혼합용액에 과량의 에탄올을 첨가하고, 원심분리를 하여 젖산칼슘과 상층액을 분리하여 상층액은 제거하는 세척과정은 최소 3회 이상 반복하였고, 침전물은 70℃에서 5시간 건조하여 젖산칼슘 분말을 얻었다.Excess ethanol was added to the mixed solution of calcium lactate, centrifuged to separate the calcium lactate and the supernatant, and the supernatant was removed at least three times. The precipitate was centrifuged at 70 ° C for 5 hours And dried to obtain calcium lactate powder.
<비교예 1>≪ Comparative Example 1 &
젖산칼슘의 제조방법에 있어서, 전처리 과정을 생략한 것을 제외하고는, 상기 실시예 2 의 젖산칼슘의 제조 방법과 동일한 방법으로 진행하였으며, 구체적으로는, 탄산칼슘 5 mmol을 5 mL 증류수와 10 mL 에탄올이 들어있는 용기에 넣고, 젖산 10 mmol를 넣고 교반하면서 혼합용액을 제조한 다음, 초음파 조사기를 이용하여 10분간 20kHz(50%)강도의 초음파를 조사하였다.The preparation of calcium lactate was carried out in the same manner as the preparation of calcium lactate in Example 2 except that the pretreatment step was omitted. Specifically, 5 mmol of calcium carbonate was dissolved in 5 mL of distilled water and 10 mL Ethanol, 10 mmol of lactic acid was added, and mixed solution was prepared by stirring. Ultrasonic waves of 20 kHz (50%) intensity were irradiated for 10 minutes using an ultrasonic wave irradiator.
<실험예 1><Experimental Example 1>
출발물질인 탄산칼슘의 초음파 전처리 전후의 입자 사이즈 분석 Particle size analysis before and after ultrasonic pretreatment of calcium carbonate as a starting material
상기 실시예에서 출발물질인 탄산칼슘에 전처리를 하였을 때, 전처리 전후의 입자사이즈를 분석하기 위해 Horiba 사의 LA-960 모델을 사용하였으며, 그 결과를 도 2에 나타내었다. In the above example, when calcium carbonate as a starting material was pretreated, Horiba's LA-960 model was used to analyze the particle size before and after the pretreatment, and the results are shown in FIG.
도 2에 나타낸 바와 같이, 실시예의 유기산 칼슘염을 제조할 때 초음파 전처리를 실시한 경우가 실시하지 않았을 경우에 비해 매우 작은 크기의 탄산칼슘이 제조된다.As shown in Fig. 2, calcium carbonate having a very small size can be produced in the case of preparing the organic acid calcium salt of the present invention, as compared with the case where the ultrasound pretreatment is not carried out.
이를 통해, 상기 실시예의 초음파 전처리 과정을 수행하여야 유기산 칼슘염의 출발물질인 탄산칼슘의 입자 크기가 매우 작아지게 되어 비표면적이 커짐에 따라 반응성이 증가하고 반응 시간이 줄어드는 것을 확인하였다.As a result, the particle size of the calcium carbonate, which is a starting material of the calcium carbonate salt of the organic acid, must be minimized by performing the pretreatment of the ultrasonic wave of the above-described embodiment. As a result, the reactivity increases and the reaction time decreases as the specific surface area increases.
<실험예 2><Experimental Example 2>
구연산칼슘의Of calcium citrate X-선 회절 분석 X-ray diffraction analysis
상기 실시예에서 제조한 구연산칼슘의 성분을 분석하기 위해 X-선 회절분석을 실시하였다. Rigaku 사의 D/MAX2200V/PC 모델을 사용하였으며, 그 결과를 도 3에 나타내었다. X-ray diffraction analysis was performed to analyze the components of calcium citrate prepared in the above examples. Rigaku's D / MAX2200V / PC model was used, and the results are shown in FIG.
도 3에 나타낸 바와 같이, 실시예의 출발물질인 탄산칼슘과 확연하게 다른 구연산칼슘의 XRD 패턴이 관찰된다. As shown in FIG. 3, an XRD pattern of calcium citrate, which is remarkably different from calcium carbonate, which is the starting material of the examples, is observed.
이를 통해, 상기 실시예에서 제조한 구연산칼슘이 결정성 있게 제조됨을 확인하였다.As a result, it was confirmed that the calcium citrate prepared in the above example was crystallized.
<실험예 3><Experimental Example 3>
구연산칼슘과Calcium citrate 젖산칼슘의Of calcium lactate 열중량Thermal weight 분석 analysis
상기 실시예에서 제조한 구연산칼슘과 젖산칼슘을 분석하기 위해 열중량분석기를 사용해 관찰하였다. TA Instrument 사의 TGA Q5000 모델을 사용하였으며, 그 결과를 도 4에 나타내었다. The calcium citrate and calcium lactate prepared in the above examples were analyzed using a thermogravimetric analyzer. A TGA Q5000 model of TA Instrument was used and the results are shown in FIG.
도 4에 나타낸 바와 같이, 실시예에서 제조한 구연산칼슘의 열분해는 단계적으로 일어나는데, 물리적 흡착수의 탈착단계, 화학적 흡착수의 탈착단계, 구연산칼슘의 분해에 따른 탄산칼슘 형성 단계, 그리고 CO2 생성에 따른 산화칼슘 형성단계를 거친다.Thermal decomposition of the citric acid calcium prepared in Example As shown in Figure 4 is stepwise ileonaneunde, physical desorption step of the adsorbed water and chemical desorption of the adsorbed water, calcium carbonate according to the decomposition of the citric acid calcium-forming step, and CO according to the second generation Calcium oxide formation step.
젖산칼슘의 열분해도 젖산칼슘의 분해 외에 상기에 언급한 열분해 과정과 동일하다.Pyrolysis of calcium lactate is the same as the above-mentioned pyrolysis process in addition to decomposition of calcium lactate.
<실험예 4><Experimental Example 4>
구연산칼슘과Calcium citrate 젖산칼슘의Of calcium lactate 이온농도분석 Ion concentration analysis
상기 실시예에서 제조한 구연산칼슘과 젖산칼슘을 분석하기 위해 이온농도측정기를 이용하여 함량을 측정하였다. Thermo Scientific 사의 iCAP 6500 duo Inductively Coupled Plasma-Emission Spectrometer 모델을 사용하였으며, 그 결과를 하기 표 1에 나타내었다. The contents of calcium citrate and calcium lactate prepared in the above examples were measured using an ion concentration meter. An iCAP 6500 duo Inductively Coupled Plasma-Emission Spectrometer model from Thermo Scientific was used, and the results are shown in Table 1 below.
(실시예 1)Calcium citrate
(Example 1)
(실시예 2)Calcium lactate
(Example 2)
상기 표 1에 나타낸 바와 같이, 실시예에서 제조한 구연산칼슘과 젖산칼슘은 상용 펄 젖산칼슘과 비슷하거나 더 많은 칼슘의 함량을 보이고 있으며, 불순물이 거의 없는 순도가 높음을 확인하였다.As shown in Table 1, the calcium citrate and calcium lactate prepared in the examples showed a calcium content similar to or higher than that of commercial calcium perchlorate and showed high purity with almost no impurities.
<실험예 5><Experimental Example 5>
구연산칼슘과Calcium citrate 젖산칼슘의Of calcium lactate 용해도분석 Solubility analysis
상기 실시예에서 제조한 구연산칼슘과 젖산칼슘의 용해도를 알아보기 위해 원자흡광분광강도계를 이용하여 특성을 측정하였다. Metrohm 사의 MIC-7 Advanced Ion Chromatograph 모델을 사용하였으며, 그 결과를 하기 표 2에 나타내었다.The solubilities of calcium citrate and calcium lactate prepared in the above examples were measured using an atomic absorption spectrophotometer. The MIC-7 Advanced Ion Chromatograph model of Metrohm was used, and the results are shown in Table 2 below.
(비교예 1)Calcium lactate
(Comparative Example 1)
(실시예 1)Calcium citrate
(Example 1)
(실시예 2)Calcium lactate
(Example 2)
상기 표 2에 나타낸 바와 같이, 본 발명의 실시예에서 제조된 구연산칼슘과 젖산칼슘의 경우 상용 수용성 탄산칼슘, 상용 젖산칼슘 및 전처리를 시행하지 않은 젖산칼슘(비교예 1)에 비해 칼슘의 용해도가 훨씬 높음을 알 수 있다.As shown in Table 2 above, the calcium citrate and calcium lactate prepared in the examples of the present invention had a higher solubility of calcium than that of commercial water-soluble calcium carbonate, commercial calcium lactate, and calcium lactate without the pretreatment (Comparative Example 1) Much higher.
Claims (12)
상기 단계의 용액에 유기산을 혼합하여 혼합물을 형성하는 단계; 및
상기 유기산을 혼합하여 형성된 혼합물에 초음파를 조사하는 단계;
를 포함하는 것을 특징으로 하는 유기산 칼슘염의 제조방법.
Mixing at least one member selected from the group consisting of calcium carbonate and calcium oxide in a solvent and subjecting the mixture to ultrasonic irradiation;
Mixing the solution of the step with an organic acid to form a mixture; And
Irradiating a mixture formed by mixing the organic acid with ultrasonic waves;
≪ / RTI > wherein the organic acid salt is selected from the group consisting of:
상기 유기산은 구연산 또는 젖산인 것을 특징으로 하는 유기산 칼슘염의 제조방법.
The method according to claim 1,
Wherein the organic acid is citric acid or lactic acid.
상기 구연산은 함수 구연산 및 무수 구연산으로 이루어지는 군으로부터 선택되는 1종 이상인 것을 특징으로 하는 유기산 칼슘염의 제조방법.
3. The method of claim 2,
Wherein the citric acid is at least one selected from the group consisting of citric acid and citric acid anhydride.
상기 젖산은 D-젖산 및 L-젖산으로 이루어지는 군으로부터 선택되는 1종 이상인 것을 특징으로 하는 유기산 칼슘염의 제조방법.
3. The method of claim 2,
Wherein the lactic acid is at least one selected from the group consisting of D-lactic acid and L-lactic acid.
상기 전처리 단계의 초음파는 1 내지 100 kHz의 강도로 1분 내지 10분 동안 조사되는 것을 특징으로 하는 유기산 칼슘염의 제조방법.
The method according to claim 1,
Wherein the ultrasonic wave in the pretreatment step is irradiated at an intensity of 1 to 100 kHz for 1 minute to 10 minutes.
상기 유기산을 혼합하여 형성된 혼합물에 조사하는 초음파는 2 내지 200 kHz의 강도로 5분 내지 20분 동안 조사되는 것을 특징으로 하는 유기산 칼슘염의 제조방법.
The method according to claim 1,
Wherein the ultrasonic waves irradiated to the mixture formed by mixing the organic acids are irradiated at an intensity of 2 to 200 kHz for 5 minutes to 20 minutes.
상기 유기산 칼슘염은 구연산칼슘 또는 젖산칼슘인 것을 특징으로 하는 유기산 칼슘염의 제조방법.
The method according to claim 1,
Wherein the organic acid calcium salt is calcium citrate or calcium lactate.
상기 유기산을 혼합하여 형성된 혼합물에 초음파를 조사하는 단계 수행 후, 칼슘화합물을 세척 및 건조하는 단계를 더 수행하는 것을 특징으로 하는 유기산 칼슘염의 제조방법.
The method according to claim 1,
A step of irradiating ultrasonic waves to the mixture formed by mixing the organic acid, and then washing and drying the calcium compound.
상기 세척 단계는 원심분리를 이용하여 칼슘화합물과 상층액을 분리하고, 이후 상층액을 제거하는 것을 특징으로 하는 유기산 칼슘염의 제조방법.
9. The method of claim 8,
Wherein the washing step separates the calcium compound and the supernatant using centrifugation and then removes the supernatant.
The method for producing an organic acid calcium salt according to claim 9, wherein the washing step is carried out three to ten times.
상기 건조 단계는 30 내지 150 ℃ 의 온도에서 1 내지 20 시간 동안 수행하는 것인 유기산 칼슘염의 제조방법.
9. The method of claim 8,
Wherein the drying step is carried out at a temperature of 30 to 150 DEG C for 1 to 20 hours.
상기 용매는 물 및 에탄올인 것을 특징으로 하는 유기산 칼슘염의 제조방법.The method according to claim 1,
Wherein the solvent is water and ethanol.
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