KR20230134167A - Manufacturing methods of solid powdery water soluble sulfuric compounds - Google Patents
Manufacturing methods of solid powdery water soluble sulfuric compounds Download PDFInfo
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- KR20230134167A KR20230134167A KR1020220031123A KR20220031123A KR20230134167A KR 20230134167 A KR20230134167 A KR 20230134167A KR 1020220031123 A KR1020220031123 A KR 1020220031123A KR 20220031123 A KR20220031123 A KR 20220031123A KR 20230134167 A KR20230134167 A KR 20230134167A
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- sulfur
- alkali metal
- water
- metal hydroxide
- soluble
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 239000007787 solid Substances 0.000 title claims abstract description 32
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 21
- 150000001875 compounds Chemical class 0.000 title claims description 4
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 82
- 239000011593 sulfur Substances 0.000 claims abstract description 82
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 63
- 150000003464 sulfur compounds Chemical class 0.000 claims abstract description 36
- 239000007864 aqueous solution Substances 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
- 239000000243 solution Substances 0.000 claims abstract description 10
- 229910052500 inorganic mineral Inorganic materials 0.000 claims abstract description 9
- 239000011707 mineral Substances 0.000 claims abstract description 9
- 239000000843 powder Substances 0.000 claims abstract description 8
- 239000002537 cosmetic Substances 0.000 claims abstract description 7
- 239000002778 food additive Substances 0.000 claims abstract description 5
- 235000013373 food additive Nutrition 0.000 claims abstract description 5
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 claims description 33
- -1 alkali metal thiosulfate Chemical class 0.000 claims description 24
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 21
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 21
- 229910052783 alkali metal Inorganic materials 0.000 claims description 19
- 239000003960 organic solvent Substances 0.000 claims description 19
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 claims description 14
- 150000008044 alkali metal hydroxides Chemical class 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 12
- 150000001340 alkali metals Chemical class 0.000 claims description 11
- 229940074993 carbon disulfide Drugs 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 9
- 229910052785 arsenic Inorganic materials 0.000 claims description 8
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 8
- 229910001385 heavy metal Inorganic materials 0.000 claims description 8
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 7
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 7
- 239000012535 impurity Substances 0.000 claims description 7
- 239000008096 xylene Substances 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 6
- 239000005077 polysulfide Substances 0.000 claims description 6
- 229920001021 polysulfide Polymers 0.000 claims description 6
- 150000008117 polysulfides Polymers 0.000 claims description 6
- 239000007921 spray Substances 0.000 claims description 6
- 239000013078 crystal Substances 0.000 claims description 4
- 229910001413 alkali metal ion Inorganic materials 0.000 claims description 3
- 238000001704 evaporation Methods 0.000 claims description 3
- 210000004276 hyalin Anatomy 0.000 claims description 3
- 239000008194 pharmaceutical composition Substances 0.000 claims description 3
- 238000010521 absorption reaction Methods 0.000 abstract description 6
- 238000000034 method Methods 0.000 abstract description 6
- 241001465754 Metazoa Species 0.000 abstract description 5
- 239000003814 drug Substances 0.000 abstract description 5
- 229940079593 drug Drugs 0.000 abstract description 2
- 239000007924 injection Substances 0.000 abstract description 2
- 238000002347 injection Methods 0.000 abstract description 2
- 239000002674 ointment Substances 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract 2
- 150000002500 ions Chemical class 0.000 abstract 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 7
- 239000011734 sodium Substances 0.000 description 7
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 3
- 239000003513 alkali Substances 0.000 description 3
- 238000009835 boiling Methods 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 229910052700 potassium Inorganic materials 0.000 description 3
- 239000011591 potassium Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
- 229910000000 metal hydroxide Inorganic materials 0.000 description 2
- 150000004692 metal hydroxides Chemical class 0.000 description 2
- 229940016409 methylsulfonylmethane Drugs 0.000 description 2
- 229940016373 potassium polysulfide Drugs 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- HHVIBTZHLRERCL-UHFFFAOYSA-N sulfonyldimethane Chemical compound CS(C)(=O)=O HHVIBTZHLRERCL-UHFFFAOYSA-N 0.000 description 2
- DHCDFWKWKRSZHF-UHFFFAOYSA-L thiosulfate(2-) Chemical compound [O-]S([S-])(=O)=O DHCDFWKWKRSZHF-UHFFFAOYSA-L 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 229910052792 caesium Inorganic materials 0.000 description 1
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 description 1
- 229910052729 chemical element Inorganic materials 0.000 description 1
- 239000008406 cosmetic ingredient Substances 0.000 description 1
- 239000010779 crude oil Substances 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 235000005911 diet Nutrition 0.000 description 1
- 230000000378 dietary effect Effects 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- FGRVOLIFQGXPCT-UHFFFAOYSA-L dipotassium;dioxido-oxo-sulfanylidene-$l^{6}-sulfane Chemical compound [K+].[K+].[O-]S([O-])(=O)=S FGRVOLIFQGXPCT-UHFFFAOYSA-L 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 235000021321 essential mineral Nutrition 0.000 description 1
- 229910052730 francium Inorganic materials 0.000 description 1
- KLMCZVJOEAUDNE-UHFFFAOYSA-N francium atom Chemical compound [Fr] KLMCZVJOEAUDNE-UHFFFAOYSA-N 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229940127554 medical product Drugs 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 239000000825 pharmaceutical preparation Substances 0.000 description 1
- 229940127557 pharmaceutical product Drugs 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 229910052701 rubidium Inorganic materials 0.000 description 1
- IGLNJRXAVVLDKE-UHFFFAOYSA-N rubidium atom Chemical compound [Rb] IGLNJRXAVVLDKE-UHFFFAOYSA-N 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- HYHCSLBZRBJJCH-UHFFFAOYSA-N sodium polysulfide Chemical compound [Na+].S HYHCSLBZRBJJCH-UHFFFAOYSA-N 0.000 description 1
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 description 1
- 235000019345 sodium thiosulphate Nutrition 0.000 description 1
- 235000014347 soups Nutrition 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/02—Preparation of sulfur; Purification
- C01B17/0243—Other after-treatment of sulfur
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
- A23L29/03—Organic compounds
- A23L29/055—Organic compounds containing sulfur as heteroatom
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
- A23L3/40—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by drying or kilning; Subsequent reconstitution
- A23L3/46—Spray-drying
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K33/00—Medicinal preparations containing inorganic active ingredients
- A61K33/04—Sulfur, selenium or tellurium; Compounds thereof
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
- A61K8/23—Sulfur; Selenium; Tellurium; Compounds thereof
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/02—Preparation of sulfur; Purification
- C01B17/0237—Converting into particles, e.g. by granulation, milling
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/22—Alkali metal sulfides or polysulfides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/64—Thiosulfates; Dithionites; Polythionates
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- Veterinary Medicine (AREA)
- Public Health (AREA)
- General Health & Medical Sciences (AREA)
- Nutrition Science (AREA)
- Epidemiology (AREA)
- Polymers & Plastics (AREA)
- Food Science & Technology (AREA)
- Engineering & Computer Science (AREA)
- Pharmacology & Pharmacy (AREA)
- Medicinal Chemistry (AREA)
- Birds (AREA)
- Dermatology (AREA)
- Cosmetics (AREA)
Abstract
본 발명은 물에 녹지 않는 광물 유황을 물에 녹을 수 있도록 분말로 제조하는 방법에 관한 것으로, 보다 상세하게는 유황의 성분의 소화가 가능하며, 흡수 효율을 높이기 위해 수용성으로 활용할 수 있도록 분말상 고형 수용성 유황화합물을 제조하는 방법에 관한 것이다.
본 발명에 의하면 분말상으로 유황화합물을 제조함으로써, 의약이나 화장품 등을 제조하는 경우 유황수용액 보다 유황성분의 함량 조절이 용이하고 취급이 용이하며, 유황 수용액보다 반응이 간접적으로 일어나게 됨으로써, 직접적인 화학반응 속도를 늦추어 동식물의 체내에서 유황성분의 충분한 흡수가 가능해질 수 있다.
또한, 본 발명의 고형 수용성 유황화합물은 필요시에 물에 녹여 유황이 이온으로 수용액 내에 존재함으로써 주사제, 내복약, 연고 등 의료 및 제약 재료, 화장품 재료, 식품첨가물 등으로 광범위하게 사용할 수 있다.The present invention relates to a method of manufacturing mineral sulfur, which is insoluble in water, into a powder so that it can dissolve in water. More specifically, the sulfur component can be digested and can be used in water-soluble form to increase absorption efficiency. It relates to a method of producing sulfur compounds.
According to the present invention, by manufacturing a sulfur compound in powder form, it is easier to control the content of sulfur components and handle it than an aqueous sulfur solution when manufacturing medicines or cosmetics, and the reaction occurs indirectly compared to an aqueous sulfur solution, thereby increasing the speed of the direct chemical reaction. By slowing down the process, sufficient absorption of sulfur components can be achieved in the bodies of animals and plants.
In addition, the solid water-soluble sulfur compound of the present invention can be dissolved in water when necessary and the sulfur exists as ions in the aqueous solution, so it can be widely used as medical and pharmaceutical materials such as injections, oral medicine, and ointments, cosmetic materials, and food additives.
Description
본 발명은 물에 녹지 않는 광물 유황을 물에 녹을 수 있도록 분말로 제조하 The present invention is to manufacture water-insoluble mineral sulfur into powder so that it can dissolve in water.
는 방법에 관한 것으로, 보다 상세하게는 유황의 성분의 소화가 가능하며, 흡수 It relates to the method, and more specifically, the digestion and absorption of sulfur components.
효율을 높이기 위해 수용성으로 활용할 수 있도록 분말상 고형 수용성 유황화합Powdered solid water-soluble sulfur compound that can be used in water-soluble form to increase efficiency.
물을 제조하는 방법에 관한 것이다.It's about how to manufacture water.
동식물의 체내에서 주요 대사에 작용하는 유황은 필수 미네랄 성분이Sulfur, which plays a major role in metabolism in the bodies of animals and plants, is an essential mineral.
지만 물에 녹지 않는 성질로 인해 유황 자체로는 식물이나 일부 동물을 제외However, due to its insoluble nature in water, sulfur itself excludes plants and some animals.
하고는 소화할 수 없다. And you can't digest it.
식이유황으로 알려진 MSM(Methylsulfonylmethane)은 흡수율이나 효능 등이 MSM (Methylsulfonylmethane), known as dietary sulfur, has low absorption rate and efficacy.
과학적으로 입증되지 않은 상태이다. It has not been scientifically proven.
일반적으로 사용되는 액상 유황은 다른 화합물과 직접적으로 반응하게 되어 유황의 다른 물질과 반응하여 화학적 성질이 변하거나 효능이 감소할 수 있으나, 분말상 유황의 경우에는 유황의 성분을 조절하여 조제하는 것이 용이하고 다른 화합물과의 직접적인 화학결합을 방지하는 효과가 있으므로, 분 Liquid sulfur, which is commonly used, reacts directly with other compounds and may change its chemical properties or reduce its efficacy by reacting with other substances of sulfur. However, in the case of powdered sulfur, it is easy to prepare by adjusting the components of sulfur. Because it has the effect of preventing direct chemical bonding with other compounds,
말상 유황화합물을 이용하여 필요시에 유황이 물에 녹을 수 있도록 하여 이온상태로 동식물의 체내에 원활히 흡수되도록 하는 기술 개발이 요구되고 있다.There is a need to develop technology that uses powdered sulfur compounds to dissolve sulfur in water when necessary so that it can be smoothly absorbed into the bodies of animals and plants in an ionic state.
상기의 문제점을 해결하기 위해 본 발명은 기존의 유황 정제법과 유황 용 In order to solve the above problems, the present invention combines the existing sulfur purification method and sulfur
해법을 보완하여 유황성분의 투입 용량 조절 및 취급이 용이한 분말상 고형 수Powdered solid water that complements the solution and is easy to control and handle the input amount of sulfur components.
용성 유황화합물을 제조하는 방법을 제공하고자 한다.The object is to provide a method for producing a soluble sulfur compound.
상기 목적을 달성하기 위한 본 발명의 분말상 고형 수용성 유황화합물은 유The powdery solid water-soluble sulfur compound of the present invention for achieving the above purpose is
황과 알칼리금속을 포함하는 분말상 고형 수용성 유황화합물로서, 전체 100 중량It is a powdery solid water-soluble sulfur compound containing sulfur and alkali metal, totaling 100 weight.
부에 대하여 유황 25 내지 30 중량부, 알칼리금속수산화물 30 내지 35 중량부, 25 to 30 parts by weight of sulfur, 30 to 35 parts by weight of alkali metal hydroxide,
알칼리금속다황화물 20 내지 25 중량부 및 티오황산알칼리금속 화합물 10 내지 20 to 25 parts by weight of alkali metal polysulfide and 10 to 10 parts by weight of alkali metal thiosulfate compound
20 중량부를 포함하며, 아래의 반응식으로 제조되는 것을 특징으로 한다. It contains 20 parts by weight and is characterized by being prepared according to the reaction formula below.
[반응식][Reaction formula]
(m+6)[AM]OH + (2n+2)S → 2[AM](m+6)[AM]OH + (2n+2)S → 2[AM] 22 SS nn + m[AM] +m[AM] ++ + nS +nS -2-2 + [AM]2S + [AM]2S 22 OO 33 + 3H +3H 22 O O
[AM]OH 은 알칼리금속수산화물, [AM] 2 S n 은 알칼리금속다황화물, m[AM] + 은 m개 [AM]OH is alkali metal hydroxide, [AM] 2 S n is alkali metal polysulfide, m[AM] + m pieces of silver
의 알칼리금속 이온을, nS -2 은 n개의 유황 이온 및 [AM]2S 2 O 3 티오황산알칼리of alkali metal ions, nS -2 is n sulfur ions and [AM]2S 2 O 3 Alkali thiosulfate
금속 화합물을 뜻함. Refers to a metal compound.
또한, 본 발명의 분말상 고형 수용성 유황화합물 제조방법은 In addition, the method for producing a powdery solid water-soluble sulfur compound of the present invention is
a) 유기용매 싸이클로핵산(Cyclohexane), 크실렌(Xylene), 톨루엔(Toluene), a) Organic solvents Cyclohexane, Xylene, Toluene,
벤젠(Benzene), 클로로벤젠(Chlorobenzene), 카본디설파이Benzene, Chlorobenzene, Carbon Disulfide
드(Carbondisulfide) 중 어느 하나의 유기용매에 광물 유황을 섭씨 110~120Add mineral sulfur to any one of carbondisulfide organic solvents at 110 to 120 degrees Celsius.
도로 가열하여 녹이고, 상기 유기용매에 녹지 않는 비소, 중금속 등 불순물It is dissolved by heating, and impurities such as arsenic and heavy metals that are insoluble in the organic solvent.
을 필터로 걸러내고 냉각하여 순수 유황을 제조하는 단계;filtering and cooling to produce pure sulfur;
b) 상기 순수 유황을 알칼리금속수산화물과 질량비 1:1로 혼합하고 혼합물과 b) Mix the pure sulfur with alkali metal hydroxide in a mass ratio of 1:1 and mix with the mixture.
동일 질량의 물에 넣고 섭씨 100도 이상으로 가열하여 유황알칼리금속수산화Add the same mass of water and heat to over 100 degrees Celsius to oxidize sulfur alkali metal.
물 수용액을 제조하는 단계;및preparing an aqueous water solution; and
c) 상기 유황알칼리금속수산화물 수용액을 진공 오븐 내에서 섭씨 60~80도로 c) The sulfur alkali metal hydroxide aqueous solution is heated to 60 to 80 degrees Celsius in a vacuum oven.
가열하여 물을 완전히 증발시키고, 겔(gel) 상태의 유황알칼리 금속수산화물The water is completely evaporated by heating, and the sulfur alkali metal hydroxide is in a gel state.
을 영하의 냉각기에서 냉각하여 결정화하는 단계;Crystallizing by cooling in a sub-zero cooler;
를 포함하는 것을 특징으로 한다.It is characterized by including.
또한, 본 발명의 다른 실시예에 따른 분말상 고형 수용성 유황화합물 제조방In addition, a method for producing a powdery solid water-soluble sulfur compound according to another embodiment of the present invention
법은 The law
a) 유기용매 싸이클로핵산(Cyclohexane), 크실렌(Xylene), 톨루엔(Toluene), a) Organic solvents Cyclohexane, Xylene, Toluene,
벤젠(Benzene), 클로로벤젠(Chlorobenzene), 카본디설파이Benzene, Chlorobenzene, Carbon Disulfide
드(Carbondisulfide) 중 어느 하나의 유기용매에 광물 유황을 섭씨 110~120Add mineral sulfur to any one of carbondisulfide organic solvents at 110 to 120 degrees Celsius.
도로 가열하여 녹이고, 상기 유기용매에 녹지 않는 비소, 중금속 등 불순물It is dissolved by heating, and impurities such as arsenic and heavy metals that are insoluble in the organic solvent.
을 필터로 걸러내고 냉각하여 순수 유황을 제조하는 단계;filtering and cooling to produce pure sulfur;
b) 상기 순수 유황을 알칼리금속수산화물과 질량비 1:1로 혼합하고 혼합물과 b) Mix the pure sulfur with alkali metal hydroxide in a mass ratio of 1:1 and mix with the mixture.
동일 질량의 물에 넣고 섭씨 100도 이상으로 가열하여 유황알칼리금속수산화Add the same mass of water and heat to over 100 degrees Celsius to oxidize sulfur alkali metal.
물 수용액을 제조하는 단계;및preparing an aqueous water solution; and
c) 상기 유황알칼리금속수산화물 수용액을 섭씨 60~80도 저온 저압 스프레이 c) Spray the sulfur alkali metal hydroxide aqueous solution at a low temperature and pressure of 60 to 80 degrees Celsius.
드라이어(spray dryer)로 물을 증발시키고 유황알칼리금속수산화물 결정 분Evaporate the water using a spray dryer and separate the sulfur alkali metal hydroxide crystals.
말을 제조하는 단계;manufacturing horses;
를 포함하는 것을 특징으로 한다. It is characterized by including.
또한, 본 발명은 상기 제조방법 중 어느 하나로 제조되는 분말상 고형 수용In addition, the present invention accommodates powdered solids prepared by any of the above production methods.
성 유황화합물을 제공한다. Provides sulfur compounds.
또한, 본 발명은 상기 분말상 고형 수용성 유황화합물을 포함하는 식품첨가In addition, the present invention is a food additive containing the powdery solid water-soluble sulfur compound.
물, 화장품 및 의약조성물을 제공한다. Provides water, cosmetics and pharmaceutical compositions.
본 발명에 의하면 분말상으로 유황화합물을 제조함으로써, 의약이나 According to the present invention, by producing a sulfur compound in powder form, it can be used as medicine or
화장품 등을 제조하는 경우 유황수용액 보다 유황성분의 함량 조절이 용이하When manufacturing cosmetics, etc., it is easier to control the content of sulfur components than with sulfur aqueous solution.
고 취급이 용이하며, 유황 수용액보다 반응이 간접적으로 일어나게 됨으로It is easy to handle and the reaction occurs more indirectly than in sulfur aqueous solution.
써, 직접적인 화학반응 속도를 늦추어 동식물의 체내에서 유황성분의 충분한 By slowing down the speed of direct chemical reactions, sufficient sulfur components are released into the bodies of animals and plants.
흡수가 가능해질 수 있다. Absorption may become possible.
또한, 본 발명의 고형 수용성 유황화합물은 필요시에 물에 녹여 유황이 이In addition, the solid water-soluble sulfur compound of the present invention can be dissolved in water when necessary to transform sulfur into
온으로 수용액 내에 존재함으로써 주사제, 내복약, 연고 등 의료 및 제약 Medical and pharmaceutical products such as injections, oral medicines, ointments, etc. are present in an aqueous solution.
재료, 화장품 재료, 식품첨가물 등으로 광범위하게 사용할 수 있다.It can be widely used as ingredients, cosmetic ingredients, food additives, etc.
본 발명에 있어서 분말상 고형 수용성 유황화합물의 제조방법을 실시예를 들 In the present invention, the method for producing a powdery solid water-soluble sulfur compound is given as an example.
어 설명을 하면 다음과 같다. 본 발명은 하기의 실시예에 한정되지 않으며, The explanation is as follows. The present invention is not limited to the following examples,
본 발명이 속한 기술분야의 당업자에 의한 다양한 변형이 가능함을 이해할 It will be understood that various modifications are possible by those skilled in the art to which the present invention pertains.
것이다. will be.
이하, 본 발명에 따른 바람직한 실시예를 들어 상세하게 설명한다.Hereinafter, a preferred embodiment according to the present invention will be described in detail.
본 발명의 분말상 고형 수용성 유황화합물은 유황과 알칼리금속을 포함하는 The powdery solid water-soluble sulfur compound of the present invention contains sulfur and alkali metal.
분말상 고형 수용성 유황화합물로서, 전체 100 중량부에 대하여 유황 25 내It is a powdery solid water-soluble sulfur compound, containing 25 parts by weight of sulfur per 100 parts by weight.
지 30 중량부, 알칼리금속수산화물 30 내지 35 중량부, 알칼리금속다황화물 30 parts by weight, alkali metal hydroxide, 30 to 35 parts by weight, alkali metal polysulfide
20 내지 25 중량부 및 티오황산알칼리금속 화합물 10 내지 20 중량부를 포함Contains 20 to 25 parts by weight and 10 to 20 parts by weight of an alkali metal thiosulfate compound.
하는 것을 특징으로 한다. It is characterized by:
이하, 본 발명의 다른 실시예에 따른 분말상 고형 수용성 유황화합물 제조방Hereinafter, a method for producing a powdery solid water-soluble sulfur compound according to another embodiment of the present invention.
법을 상세히 설명하면 다음과 같다. The law is explained in detail as follows.
광물 유황은 화산이나 원유 정제 부산물에서 얻으며 이때 포함되는 비소와 Mineral sulfur is obtained from volcanoes or crude oil refining by-products, and contains arsenic and
다양한 중금속 성분들로 인해 순수 유황으로 정제해야 하며 이를 위해 유기Due to the various heavy metal components, it must be purified into pure sulfur, and for this purpose, organic
용매인 싸이클로핵산(Cyclohexane), 크실렌(Xylene), 톨루엔(Toluene), 벤Solvents Cyclohexane, Xylene, Toluene, and Beneath
젠(Benzene), 클로로벤젠(Chlorobenzene), 카본디설파이드(Carbondisulfide) Benzene, Chlorobenzene, Carbondisulfide
중 하나의 용매를 섭씨 110도로 가열하여 유황을 녹이고, 상기 유기용매에 Heat one of the solvents to 110 degrees Celsius to dissolve sulfur and add it to the organic solvent.
녹지 않는 비소, 중금속 등 불순물을 필터로 걸러내고, 걸러진 용액을 냉각Impurities such as insoluble arsenic and heavy metals are filtered out and the filtered solution is cooled.
하여 순수 유황 결정을 얻을 수 있다.Thus, pure sulfur crystals can be obtained.
상기 순수 유황을 알칼리금속수산화물과 중량비 1:1로 혼합하고 상기 혼합물The pure sulfur was mixed with alkali metal hydroxide in a weight ratio of 1:1 and the mixture
을 동일 질량의 물에 넣고 섭씨 110도로 가열하여 유황-알칼리금속수화물 수Add the same mass of water and heat it to 110 degrees Celsius to form sulfur-alkali metal hydrate.
용액을 제조한다.Prepare the solution.
상기 수용액에서 수분을 제거하여 분말상 고형 수용성 유황화합물을 제조한A powdery solid water-soluble sulfur compound was prepared by removing moisture from the aqueous solution.
다.all.
상기 제조공정을 반응식으로 설명하면,If the manufacturing process is explained in a reaction equation,
(m+6)[AM]OH + (2n+2)S → 2[AM](m+6)[AM]OH + (2n+2)S → 2[AM] 22 SS nn + m[AM] +m[AM] ++ + nS +nS -2-2 + [AM]2S + [AM]2S 22 OO 33 + 3H +3H 22 O O
상기 반응식에서 [AM] 은 알칼리금속으로 화학원소 주기율표 상 1그룹에 속하In the above reaction formula , [AM] is an alkali metal and belongs to group 1 on the periodic table of chemical elements.
는 리튬(Li), 나트륨(Na), 포타슘(K), 루비듐(Rb), 세슘(Cs), 프란슘(Fr)의 is lithium (Li), sodium (Na), potassium (K), rubidium (Rb), cesium (Cs), and francium (Fr).
알칼리금속이며, 본 발명에 따른 과제에는 Sodium(Na, 나트륨), It is an alkali metal, and the subject according to the present invention includes Sodium (Na),
Potassium(K, 칼륨)의 수산화물이 바람직하다.Potassium (K) hydroxide is preferred.
또한 상기 반응식에서 m 과 n 은 복수개를 뜻하는 기호이며, In addition, in the above reaction formula, m and n are symbols indicating plurality,
[AM]OH 은 수산화나트륨(Sodium Hydroxide, NaOH), 수산화칼륨(Potassium [AM]OH is Sodium Hydroxide (NaOH), Potassium Hydroxide (Potassium)
Hydroxide, KOH) 등의 알칼리금속수산화물을 뜻하며,Refers to alkali metal hydroxides such as hydroxide, KOH),
[AM] 2 S n 은 나트륨다황화물(Sodium Polysulfide, Na2Sn), 칼륨다황화 [AM] 2 S n is sodium polysulfide (Na 2 S n ), potassium polysulfide
물(Potassium Polysulfide, K2Sn) 등의 알칼리금속다황화물을 뜻하며,It refers to alkali metal polysulfides such as water (Potassium Polysulfide, K 2 S n ),
m[AM] + 은 m개의 Na+, K+ 등의 알칼리금속 이온을 뜻하며, m[AM] + refers to m alkali metal ions such as Na + and K + .
nS -2 은 n개의 유황 이온을 뜻하며, nS -2 means n sulfur ions,
[AM] 2 S 2 O 3 은 티오황산나트륨(Sodium Thiosulfate, Na2S2O3), 티오황산칼 [AM] 2 S 2 O 3 is sodium thiosulfate (Na 2 S 2 O 3 ), cal thiosulfate
륨(Potassium Thiosulfate, K2S2O3) 등의 티오황산알칼리금속 화합물을 뜻한Refers to alkali metal thiosulfate compounds such as Potassium Thiosulfate (K 2 S 2 O 3 ).
다. all.
본 발명에 따른 분말상 고형 수용성 2[AM] 2 S n , m[AM] + , nS -2 , [AM]2S 2 O 3 이 혼Powder-like solid water-soluble 2[AM] 2 S n , m[AM] + , nS -2 , [AM] 2 S 2 O 3 according to the present invention
합된 상태이다. It is in a combined state.
또한 수용액을 결정화하는 일반적인 방법은 수분 증발, 석출 등이 있으나 본 In addition, common methods for crystallizing aqueous solutions include water evaporation and precipitation.
발명의 고형 수용성 유황화합물의 끓는 점은 약 섭씨 110도로 유황의 끓는 The boiling point of the solid water-soluble sulfur compound of the invention is about 110 degrees Celsius, which is the boiling point of sulfur.
점보다 낮고 고온 가열 시 유황이 기화되어 가스가 발생하며 유황의 손실이 When heated to a high temperature below that point, sulfur vaporizes, gas is generated, and sulfur loss occurs.
발생하므로 결정화과정이 필요하다. Therefore, a crystallization process is necessary.
본 발명에 의한 상기 고형 수용성 유황화합물 수용액의 결정화 방법을 설명Describe the crystallization method of the solid water-soluble sulfur compound aqueous solution according to the present invention.
하면,if,
첫번째로 물은 진공상태에 가까워질수록 끓는점이 낮아지므로 고형 수용성 First, the boiling point of water decreases as it approaches a vacuum state, so the solid water-soluble
유황화합물 수용액을 진공 오븐 내에서 섭씨 60~80도로 가열하여 물을 완전The sulfur compound aqueous solution is heated to 60 to 80 degrees Celsius in a vacuum oven to completely dissolve the water.
히 증발시키고, 유리질(hyaline) 상태의 고형 수용성 유황화합물을 영하의 After evaporation, the hyaline solid water-soluble sulfur compound is sub-zero.
냉각기에서 냉각하여 결정화 한 후 분쇄한다.It is cooled in a cooler to crystallize and then pulverized.
두번째로, 상기 고형 수용성 유황화합물 수용액을 저온 저압 스프레이 드라Second, the solid water-soluble sulfur compound aqueous solution is spray dried at low temperature and pressure.
이어(spray dryer)로 물을 증발시키고 유황화합물 결정 분말을 제조한다.Then, water is evaporated using a spray dryer and sulfur compound crystal powder is prepared.
[실시예 1][Example 1]
먼저, 유기용매 싸이클로핵산(Cyclohexane), 크실렌(Xylene), 톨루First, the organic solvents cyclohexane, xylene, and tolu
엔(Toluene), 벤젠(Benzene), 클로로벤젠(Chlorobenzene), 카본디설파이Toluene, Benzene, Chlorobenzene, Carbon Disulfide
드(Carbondisulfide) 중 어느 하나의 유기용매 60 ~ 70 중량부에 광물 유황 60 to 70 parts by weight of mineral sulfur in any one of carbondisulfide organic solvents
30 ~ 40 중량부를 녹이고, 상기 유기용매에 녹지 않는 비소, 중금속 등 불순Dissolve 30 to 40 parts by weight and impurities such as arsenic and heavy metals that are insoluble in the organic solvent.
물을 필터로 걸러내고 냉각하여 순수 유황을 제조한다. Pure sulfur is produced by filtering the water and cooling it.
다음으로, 상기 순수 유황을 수산화나트륨(Sodium Hydroxide, NaOH) 또는 수Next, the pure sulfur is dissolved in sodium hydroxide (NaOH) or water.
산화칼륨(Potassium Hydroxide, KOH)의 알칼리금속수산화물과 질량비 1:1로 Potassium Hydroxide (KOH) in a mass ratio of 1:1 with alkali metal hydroxide.
혼합하고 혼합물과 동일 질량의 물에 넣고 섭씨 100도 이상으로 가열하여 유Mix and add the same mass of water as the mixture and heat to over 100 degrees Celsius.
황알칼리금속수산화물 수용액을 제조한다. Prepare an aqueous solution of sulfur alkali metal hydroxide.
이후, 상기 유황알칼리금속수산화물 수용액을 진공 오븐 내에서 섭씨 60~80Thereafter, the sulfur alkali metal hydroxide aqueous solution was heated at 60 to 80 degrees Celsius in a vacuum oven.
도로 가열하여 물을 완전히 증발시키고, 유리질(hyaline) 상태의 유황알칼리 By heating again, the water is completely evaporated and the sulfur alkali is in a hyaline state.
금속수산화물을 영하의 냉각기에서 냉각하여 결정화시킨다. The metal hydroxide is cooled in a sub-zero cooler to crystallize.
[실시예 2] [Example 2]
먼저, 유기용매 싸이클로핵산(Cyclohexane), 크실렌(Xylene), 톨루First, the organic solvents cyclohexane, xylene, and tolu
엔(Toluene), 벤젠(Benzene), 클로로벤젠(Chlorobenzene), 카본디설파이Toluene, Benzene, Chlorobenzene, Carbon Disulfide
드(Carbondisulfide) 중 어느 하나의 유기용매 60 ~ 70 중량부에 광물 유황 60 to 70 parts by weight of mineral sulfur in any one of carbondisulfide organic solvents
30 ~ 40 중량부를 녹이고, 상기 유기용매에 녹지 않는 비소, 중금속 등 불순Dissolve 30 to 40 parts by weight and impurities such as arsenic and heavy metals that are insoluble in the organic solvent.
물을 필터로 걸러내고 냉각하여 순수 유황을 제조한다. Pure sulfur is produced by filtering the water and cooling it.
다음으로, 상기 순수 유황을 알칼리금속수산화물과 질량비 1:1로 혼합하고 Next, the pure sulfur was mixed with alkali metal hydroxide in a mass ratio of 1:1.
혼합물과 동일 질량의 물에 넣고 섭씨 100도 이상으로 가열하여 유황알칼리Add the same mass of water as the mixture and heat it to over 100 degrees Celsius to create sulfur alkali.
금속수산화물 수용액을 제조한다. Prepare an aqueous metal hydroxide solution.
이후, 상기 유황알칼리금속수산화물 수용액을 섭씨 60~80도 저온 저압 스프Thereafter, the sulfur alkali metal hydroxide aqueous solution was subjected to low temperature and low pressure soup at 60 to 80 degrees Celsius.
레이 드라이어(spray dryer)로 물을 증발시키고 유황알칼리금속수산화물 결Evaporate the water with a spray dryer and form the sulfur alkali metal hydroxide.
정 분말을 제조한다. Produce tablet powder.
또한, 본 발명은 상기 제조방법 중 어느 하나로 제조되는 분말상 고형 수용In addition, the present invention accommodates powdered solids prepared by any of the above production methods.
성 유황화합물을 제공한다. Provides sulfur compounds.
또한, 본 발명은 상기 분말상 고형 수용성 유황화합물을 포함하는 식품첨가In addition, the present invention is a food additive containing the powdery solid water-soluble sulfur compound.
물, 화장품 및 의약조성물을 제공한다. Provides water, cosmetics and pharmaceutical compositions.
본 발명에 의하면 분말상으로 유황화합물을 제조함으로써, 의약이나 화장품 According to the present invention, by manufacturing a sulfur compound in powder form, it can be used as medicine or cosmetics.
등을 제조하는 경우 유황수용액 보다 유황성분의 함량 조절이 용이하고 취급In the case of manufacturing etc., the content of sulfur components is easier to control and handle than sulfur aqueous solution.
이 용이하며, 유황 수용액보다 반응이 간접적으로 일어나게 됨으로써, 직접This is easier and the reaction occurs more indirectly than in sulfur aqueous solution, so it can be directly
적인 화학반응 속도를 늦추어 유황성분의 충분한 흡수가 가능해진다. By slowing down the speed of chemical reactions, sufficient absorption of sulfur components is possible.
상기에 제시된 실시예는 예시적인 것으로 이 분야에서 통상의 지식을 가지는 The embodiments presented above are illustrative and those of ordinary skill in the art will
자는 본 발명의 기술적 사상을 벗어나지 않는 범위에서 제시된 실시예에 대The person explains the presented embodiments without departing from the technical spirit of the present invention.
한 다양한 변형 및 수정 발명을 만들 수 있을 것이다. 이러한 변형 및 수정 Various variations and modifications can be made. These variations and modifications
발명에 의하여 본 발명의 범위는 제한되지 않는다.The scope of the present invention is not limited by this invention.
Claims (7)
[반응식]
(m+6)[AM]OH + (2n+2)S → 2[AM] 2 S n + m[AM] + + nS -2 + [AM]2S 2 O 3 + 3H 2 O
[AM]OH 은 알칼리금속수산화물, [AM] 2 S n 은 알칼리금속다황화물, m[AM] + 은 m개의 알칼리금속 이온을, nS -2 은 n개의 유황 이온 및 [AM]2S 2 O 3 티오황산알칼리금속 화합물을 뜻함. A powdery solid water-soluble sulfur compound containing sulfur and alkali metal, 25 to 30 parts by weight of sulfur, 30 to 35 parts by weight of alkali metal hydroxide, 20 to 25 parts by weight of alkali metal polysulfide, and alkali metal thiosulfate, based on 100 parts by weight of the total. A powdery solid water-soluble sulfur compound comprising 10 to 20 parts by weight of the compound and prepared according to the reaction formula below.
[Reaction formula]
(m+6)[AM]OH + (2n+2)S → 2[AM] 2 S n + m[AM] + + nS -2 + [AM]2S 2 O 3 + 3H 2 O
[AM]OH is alkali metal hydroxide, [AM] 2 S n is alkali metal polysulfide, m[AM] + is m alkali metal ions, nS -2 is n sulfur ions and [AM]2S 2 O 3 It refers to an alkali metal thiosulfate compound.
b) 상기 순수 유황을 알칼리금속수산화물과 질량비 1:1로 혼합하고 혼합물과 동일 질량의 물에 넣고 섭씨 100도 이상으로 가열하여 유황알칼리금속수산화물 수용액을 제조하는 단계;
c) 상기 유황알칼리금속수산화물 수용액을 진공 오븐 내에서 섭씨 60~80도로 가열하여 물을 완전히 증발시키고, 유리질(hyaline) 상태의 유황알칼리금속수산화물을 영하의 냉각기에서 냉각하여 결정화하는 단계;
를 포함하는 분말상 고형 수용성 유황화합물 제조방법.a) Organic solvent: Dissolve mineral sulfur in any one of the organic solvents Cyclohexane, Xylene, Toluene, Benzene, Chlorobenzene, and Carbondisulfide at 110 to 120 degrees Celsius. Preparing pure sulfur by heating and dissolving, filtering out impurities such as arsenic and heavy metals that are insoluble in the organic solvent through a filter, and cooling;
b) mixing the pure sulfur with alkali metal hydroxide in a mass ratio of 1:1, adding the same mass of water as the mixture, and heating to 100 degrees Celsius or more to prepare an aqueous sulfur alkali metal hydroxide solution;
c) heating the sulfur alkali metal hydroxide aqueous solution to 60 to 80 degrees Celsius in a vacuum oven to completely evaporate the water, and cooling the hyaline sulfur alkali metal hydroxide in a sub-zero cooler to crystallize it;
A method for producing a powdery solid water-soluble sulfur compound comprising a.
b) 상기 순수 유황을 알칼리금속수산화물과 질량비 1:1로 혼합하고 혼합물과 동일 질량의 물에 넣고 섭씨 100도 이상으로 가열하여 유황알칼리금속수산화물 수용액을 제조하는 단계;및
c) 상기 유황알칼리금속수산화물 수용액을 섭씨 60~80도 저온 저압 스프레이 드라이어(spray dryer)로 물을 증발시키고 유황알칼리금속수산화물 결정 분말을 제조하는 단계;
를 포함하는 분말상 고형 수용성 유황화합물 제조방법.a) Organic solvent: Dissolve mineral sulfur in any one of the organic solvents Cyclohexane, Xylene, Toluene, Benzene, Chlorobenzene, and Carbondisulfide at 110 to 120 degrees Celsius. Preparing pure sulfur by heating and dissolving, filtering out impurities such as arsenic and heavy metals that are insoluble in the organic solvent through a filter, and cooling;
b) mixing the pure sulfur with alkali metal hydroxide in a mass ratio of 1:1, adding the same mass of water as the mixture, and heating to 100 degrees Celsius or more to prepare an aqueous sulfur alkali metal hydroxide solution; And
c) evaporating the water from the sulfur alkali metal hydroxide aqueous solution using a low-temperature, low-pressure spray dryer at 60 to 80 degrees Celsius and preparing sulfur alkali metal hydroxide crystal powder;
A method for producing a powdery solid water-soluble sulfur compound comprising a.
A pharmaceutical composition comprising the powdery solid water-soluble sulfur compound of claim 1.
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