KR100517448B1 - Dispersible water-soluble or water-swellable polymers and process for making toothpastes containing them - Google Patents
Dispersible water-soluble or water-swellable polymers and process for making toothpastes containing them Download PDFInfo
- Publication number
- KR100517448B1 KR100517448B1 KR1019970063848A KR19970063848A KR100517448B1 KR 100517448 B1 KR100517448 B1 KR 100517448B1 KR 1019970063848 A KR1019970063848 A KR 1019970063848A KR 19970063848 A KR19970063848 A KR 19970063848A KR 100517448 B1 KR100517448 B1 KR 100517448B1
- Authority
- KR
- South Korea
- Prior art keywords
- guar
- cellulose
- hydrophobically modified
- water
- water soluble
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 244000303965 Cyamopsis psoralioides Species 0.000 claims description 80
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 50
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 48
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- 239000004137 magnesium phosphate Substances 0.000 description 1
- 229910000157 magnesium phosphate Inorganic materials 0.000 description 1
- 229960002261 magnesium phosphate Drugs 0.000 description 1
- 235000010994 magnesium phosphates Nutrition 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000001525 mentha piperita l. herb oil Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 235000019198 oils Nutrition 0.000 description 1
- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical compound [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 description 1
- 235000019477 peppermint oil Nutrition 0.000 description 1
- 235000021317 phosphate Nutrition 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 229920002401 polyacrylamide Polymers 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 239000001205 polyphosphate Substances 0.000 description 1
- 235000011176 polyphosphates Nutrition 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 235000019422 polyvinyl alcohol Nutrition 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000004208 shellac Substances 0.000 description 1
- ZLGIYFNHBLSMPS-ATJNOEHPSA-N shellac Chemical compound OCCCCCC(O)C(O)CCCCCCCC(O)=O.C1C23[C@H](C(O)=O)CCC2[C@](C)(CO)[C@@H]1C(C(O)=O)=C[C@@H]3O ZLGIYFNHBLSMPS-ATJNOEHPSA-N 0.000 description 1
- 235000013874 shellac Nutrition 0.000 description 1
- 229940113147 shellac Drugs 0.000 description 1
- AQMNWCRSESPIJM-UHFFFAOYSA-M sodium metaphosphate Chemical compound [Na+].[O-]P(=O)=O AQMNWCRSESPIJM-UHFFFAOYSA-M 0.000 description 1
- 235000019731 tricalcium phosphate Nutrition 0.000 description 1
- 239000003232 water-soluble binding agent Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/12—Powdering or granulating
- C08J3/124—Treatment for improving the free-flowing characteristics
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q11/00—Preparations for care of the teeth, of the oral cavity or of dentures; Dentifrices, e.g. toothpastes; Mouth rinses
- A61Q11/02—Preparations for deodorising, bleaching or disinfecting dentures
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/08—Cellulose derivatives
- C08J2301/10—Esters of organic acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2305/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2301/00 or C08J2303/00
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L1/00—Compositions of cellulose, modified cellulose or cellulose derivatives
- C08L1/08—Cellulose derivatives
- C08L1/10—Esters of organic acids, i.e. acylates
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L5/00—Compositions of polysaccharides or of their derivatives not provided for in groups C08L1/00 or C08L3/00
Landscapes
- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Oral & Maxillofacial Surgery (AREA)
- Life Sciences & Earth Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Cosmetics (AREA)
Abstract
본 발명은, 조성물의 총 중량을 기준으로 약 10중량%를 초과하는 농도로 존재하는 하나 이상의 폴리올로 처리함으로써 적어도 부분적으로 응집된 입상 수용성 또는 수팽윤성 중합체를 포함하는 조성물을 제공한다. 폴리올로 처리함으로써 적어도 부분적으로 응집된 입상 수용성 또는 수팽윤성 중합체는 물을 함유한 용매중에서 중합체 덩어리를 형성하지 않으면서 미처리된 수용성 또는 수팽윤성 중합체에 비해 실질적으로 신속하게 수화된다. 본 발명은 하나 이상의 무수 수용성 또는 수팽윤성 중합체를 포함하는 치약 조성물을 제조하기 위한 개선된 방법을 추가로 제공하며, 여기서 상기 개선된 방법은 폴리올로 처리함으로써 적어도 부분적으로 응집된 입상 수용성 또는 수팽윤성 중합체로 무수 수용성 또는 수팽윤성 중합체를 대체함을 포함한다. The present invention provides compositions comprising at least partially aggregated particulate water soluble or water swellable polymers by treatment with one or more polyols present at a concentration of greater than about 10 weight percent based on the total weight of the composition. By treatment with polyols, the particulate water soluble or water swellable polymers at least partially aggregated hydrate substantially faster than the untreated water soluble or water swellable polymers without forming a polymer mass in a solvent containing water. The present invention further provides an improved method for preparing a dentifrice composition comprising at least one anhydrous water soluble or water swellable polymer, wherein the improved method is at least partially aggregated particulate water soluble or water swellable polymer by treatment with a polyol. Replacing anhydrous water soluble or water swellable polymers.
Description
본 발명은 폴리올로 처리함으로써 응집된 수용성 또는 수팽윤성 중합체를 포함하는 조성물, 및 치약 제조시 상기 조성물의 용도에 관한 것이다. The present invention relates to compositions comprising water soluble or water swellable polymers agglomerated by treatment with polyols, and to the use of such compositions in the manufacture of toothpastes.
치약 제형은 일반적으로 치과용으로 허용가능한 연마제, 보습제, 물, 및 상기 성분들에 대한 농조화제 및 결합제로서 작용하는 수용성 중합체를 함유한다. 풍미제, 감미제, 방부제 및 불화물과 같은 기타 다양한 성분들도 또한 저농도로 사용되고 있다. 글리세롤 및 소르비톨은 (일반적으로 수용액으로서) 치약에 가장 통상적으로 사용되는 보습제로, 생성물에 요구되는 특징에 따라 달라지며, 폴리에틸렌 글리콜 또는 프로필렌 글리콜이 혼입될 수도 있다. 1) 크림 또는 불투명 겔, 및 2) 투명 또는 반투명 겔의 두가지 유형의 치약이 광범위하게 생산되고 있다. Toothpaste formulations generally contain dentally acceptable abrasives, moisturizers, water, and water-soluble polymers that act as thickening agents and binders for the above ingredients. Various other ingredients such as flavors, sweeteners, preservatives and fluorides are also used at low concentrations. Glycerol and sorbitol are the most commonly used moisturizers for toothpaste (generally as aqueous solutions), depending on the characteristics required for the product, and polyethylene glycol or propylene glycol may be incorporated. Two types of toothpaste are widely produced: 1) cream or opaque gel, and 2) clear or translucent gel.
치약에 가장 통상적으로 사용되는 농조화제 또는 결합제로는 카복시메틸 셀룰로즈(CMC), 하이드록시에틸 셀룰로즈(HEC), 실리카 및 마그네슘 알루미늄 규산염이 있다. 카라기난, 잔탄 및 폴리아크릴레이트가 사용될 수도 있지만, 그리 광범위하지는 않다. The most commonly used thickeners or binders for toothpastes are carboxymethyl cellulose (CMC), hydroxyethyl cellulose (HEC), silica and magnesium aluminum silicate. Carrageenan, xanthan and polyacrylates may be used but are not very extensive.
치약의 제조 공정에서, 무수 수용성 결합제 중합체를 조성물내로 혼입하는 것이 종종 어려운데, 이는 무수 중합체를 수성 시스템에 첨가하여 분산시킬 경우 덩어리가 형성되기 쉬운 경향을 갖기 때문이다. 이는 결합제 중합체를 균일하게 수화시키거나 분산시키는데 필요한 시간을 증가시킨다. 결과적으로, 덩어리가 없는 생성물, 신속한 점성 개선 및 감소된 배치 제조 시간이 유도되고 결합제의 편리한 취급이 허용되는 수용성 결합제 중합체를 혼입하는 방법이 산업분야에 요구된다.In the manufacturing process of toothpaste, it is often difficult to incorporate the anhydrous water-soluble binder polymer into the composition, since it tends to form agglomerates when the anhydrous polymer is added and dispersed in the aqueous system. This increases the time required to uniformly hydrate or disperse the binder polymer. As a result, there is a need in the industry for a method of incorporating a water-free binder polymer that results in agglomerate-free products, rapid viscosity improvement and reduced batch production time and allows convenient handling of the binder.
일본 특허 출원 제 73036167 B호는 (1) (a) 글리세롤 또는 알콜에 의해 피복되거나, 또는 (b) 전분 페이스트, 쉘락, 젤라틴 및 아가에 의해 피복된 후 (a) 처리되거나, 또는 (c) (a)에서의 기재와 (b)에서의 기재의 혼합물로 피복된, 카복시메틸 셀룰로즈, 알긴산, 폴리아크릴산 또는 이의 염; (2) (a), (b) 및 (c)의 방법으로 선택적으로 처리된 알칼리 탄산염, 중탄산염, 인산염, 다중인산염 또는 EDTA의 알칼리 염; 및 선택적으로 (3) 글루코즈, 당, 프럭토즈, 말토즈, 만니톨 및 통상의 염을 포함한 조성물을 개시하고 있다. 물을 조성물에 첨가할 경우, 이는 신속하게 습윤되고 분산되며, 알긴산, 폴리아크릴산 또는 카복시메틸 셀룰로즈 용액을 신속하게 수득할 수 있다. Japanese Patent Application No. 73036167 B is (1) (a) coated with glycerol or alcohol, or (b) coated with starch paste, shellac, gelatin and agar followed by (a) treatment, or (c) ( carboxymethyl cellulose, alginic acid, polyacrylic acid or salts thereof, coated with a mixture of the substrate in a) and the substrate in (b); (2) alkali carbonates, bicarbonates, phosphates, polyphosphates or alkali salts of EDTA optionally treated with the methods of (a), (b) and (c); And optionally (3) a composition comprising glucose, sugar, fructose, maltose, mannitol and common salts. When water is added to the composition, it is rapidly wetted and dispersed, and it is possible to obtain alginic acid, polyacrylic acid or carboxymethyl cellulose solution quickly.
일본 특허 출원 제 72044335 B호는 용융된 다가 알콜, 당 또는 유화 보조제로 수용성 중합체를 피복함으로써 상기 수용성 중합체의 용해성을 개선시킴을 교지하고 있다. 수용성 중합체로는 메틸 셀룰로즈, CMC, 폴리비닐 알콜, 알긴산 염, 폴리아크릴산 또는 이의 염 및 폴리아크릴아마이드가 있다. 다가 알콜로는 소르비톨, 만니톨, 이노시톨이 있고, 당으로는 글루코즈, 수크로즈 및 락토즈가 있다. 피복 기재는 중합체에 대해 0.5 내지 10중량%, 바람직하게는 3 내지 5중량%의 양으로 사용된다. Japanese Patent Application No. 72044335 B teaches to improve the solubility of the water-soluble polymer by coating the water-soluble polymer with molten polyhydric alcohol, sugar or emulsifying aid. Water soluble polymers include methyl cellulose, CMC, polyvinyl alcohol, alginic acid salts, polyacrylic acid or salts thereof, and polyacrylamides. Polyhydric alcohols include sorbitol, mannitol and inositol, and sugars include glucose, sucrose and lactose. The coating substrate is used in an amount of 0.5 to 10% by weight, preferably 3 to 5% by weight relative to the polymer.
구켄버거(Guckenberger) 등의 미국 특허 제 3,850,838호는, 쉽게 분산될 수 있고 용해될 수 있는 응집체의 형태인 알콜 불용성 하이드로콜로이드 이온을 제조하는 방법으로, 물과 알콜 및 탄수화물용 수성 알콜 용매 모두에 가용성인 탄수화물 결합제와 하이드로콜로이드를 잘 배합하고, 생성된 혼합물을 과립화한 후, 응집된 과립을 건조시킴을 포함하는 방법을 개시하고 있다. U.S. Patent No. 3,850,838 to Guckenberger et al. Describes a process for preparing alcohol-insoluble hydrocolloid ions in the form of aggregates that can be easily dispersed and dissolved, soluble in both water and aqueous alcohol solvents for alcohols and carbohydrates. A method is disclosed that includes combining a phosphorus carbohydrate binder and a hydrocolloid well, granulating the resulting mixture, and then drying the aggregated granules.
상기 특허들중 어느 것도 치약 조성물중 폴리올-응집된 수용성 또는 수팽윤성 중합체의 용도를 교지하지는 않는다. None of the above patents teach the use of polyol-aggregated water soluble or water swellable polymers in toothpaste compositions.
따라서, 폴리올로 처리함으로써 중합체 덩어리를 형성하지 않으면서 용매에 신속하게 분산될 수 있는 중합체 조성물 및 이를 제조하는 방법을 제공하고자 한다. It is therefore an object of the present invention to provide a polymer composition which can be rapidly dispersed in a solvent without forming a polymer mass by treating with a polyol, and a method of preparing the same.
본 발명은, 조성물의 총 중량을 기준으로 약 10중량%를 초과하는 농도로 존재하는 하나 이상의 폴리올로 처리함으로써 적어도 부분적으로 응집된 입상 수용성 또는 수팽윤성 중합체를 포함하는 조성물에 관한 것이다. 조성물은 용매중에서 중합체 덩어리를 형성하지 않으면서, 상응하는 미처리된 수용성 또는 수팽윤성 중합체에 비해 실질적으로 신속하게 분산될 수 있다. The present invention relates to a composition comprising a particulate water soluble or water swellable polymer that is at least partially aggregated by treatment with one or more polyols present at a concentration of greater than about 10% by weight based on the total weight of the composition. The composition can disperse substantially faster than the corresponding untreated water soluble or water swellable polymer without forming a polymer mass in a solvent.
또다른 태양에서, 본 발명은 또한 하나 이상의 무수 수용성 또는 수팽윤성 중합체를 포함하는 치약 조성물을 제조하기 위한 개선된 방법에 관한 것으로, 여기서 상기 개선된 방법은 무수 수용성 또는 수팽윤성 중합체를 폴리올로 처리함으로써 적어도 부분적으로 응집된 입상 수용성 또는 수팽윤성 중합체로 대체함을 포함하는 것을 포함한다. 폴리올로 처리함으로써 적어도 부분적으로 응집된 입상 수용성 또는 수팽윤성 중합체는 물 또는 물을 함유한 용매중에서 중합체 덩어리를 형성하지 않으면서, 상응하는 미처리된 수용성 또는 수팽윤성 중합체보다 실질적으로 신속하게 수화된다. In another aspect, the present invention also relates to an improved method for preparing a dentifrice composition comprising at least one anhydrous water soluble or water swellable polymer, wherein the improved method is achieved by treating the anhydrous water soluble or water swellable polymer with a polyol. Replacing with at least partially aggregated particulate water soluble or water swellable polymers. By treatment with a polyol, the particulate water soluble or water swellable polymer at least partially aggregated hydrates substantially faster than the corresponding untreated water soluble or water swellable polymer without forming a polymer mass in water or a solvent containing water.
본 발명의 조성물은 조성물의 총 중량을 기준으로 약 10중량%를 초과하는 농도로 존재하는 하나 이상의 폴리올로 처리함으로써 적어도 부분적으로 응집된 입상 수용성 또는 수팽윤성 중합체를 포함한다. 본원에서 응집이라 함은 개별적인 입자가 응집함으로써 입상 물질의 입자 크기가 증가하는 것으로 정의된다. Compositions of the present invention comprise at least partially aggregated particulate water soluble or water swellable polymers by treatment with one or more polyols present at a concentration of greater than about 10% by weight based on the total weight of the composition. Coagulation herein is defined as the increase in particle size of the granular material by aggregation of individual particles.
임의의 천연 또는 합성의 수용성 또는 수팽윤성 중합체는 본 발명의 조성물을 제조하기 위해 사용될 수 있다. 바람직한 수용성 또는 수팽윤성 중합체는 다당류이다. 유용한 다당류로는 셀룰로즈 에테르, 구아, 구아 유도체, 로커스트 콩 고무, 사일륨, 아라비아 고무, 가티 고무, 카라야 고무, 트라가칸트 고무, 카라기난, 한천, 알긴, 잔탄, 스클레로글루칸, 덱스트란, 펙틴, 전분, 키틴 및 키토산이 있지만, 이에 제한되는 것은 아니다. Any natural or synthetic water soluble or water swellable polymer can be used to prepare the compositions of the present invention. Preferred water soluble or water swellable polymers are polysaccharides. Useful polysaccharides include cellulose ethers, guar, guar derivatives, locust bean rubber, silium, gum arabic, gatti rubber, karaya rubber, tragacanth rubber, carrageenan, agar, algin, xanthan, scleroglucan, dextran, Pectin, starch, chitin and chitosan, but are not limited thereto.
바람직한 다당류로는 셀룰로즈 에테르, 카라기난, 구아, 구아 유도체 및 펙틴이 있다. Preferred polysaccharides are cellulose ethers, carrageenan, guar, guar derivatives and pectin.
본 발명에 사용하기 위한 셀룰로즈 에테르로는 하이드록시에틸 셀룰로즈(HEC), 하이드록시프로필 셀룰로즈(HPC), 수용성 에틸하이드록시에틸 셀룰로즈(EHEC), 카복시메틸 셀룰로즈(CMC), 카복시메틸하이드록시에틸 셀룰로즈(CMHEC), 하이드록시프로필하이드록시에틸 셀룰로즈(HPHEC), 메틸 셀룰로즈(MC), 메틸하이드록시프로필 셀룰로즈(MHPC), 메틸하이드록시에틸 셀룰로즈(MHEC), 카복시메틸메틸 셀룰로즈(CMMC), 소수성으로 개질된 카복시메틸 셀룰로즈(HMCMC), 소수성으로 개질된 하이드록시에틸 셀룰로즈(HMHEC), 소수성으로 개질된 하이드록시프로필 셀룰로즈(HMHPC), 소수성으로 개질된 에틸하이드록시에틸 셀룰로즈(HMEHEC), 소수성으로 개질된 카복시메틸하이드록시에틸 셀룰로즈(HMCMHEC), 소수성으로 개질된 하이드록시프로필하이드록시에틸 셀룰로즈(HMHPHEC), 소수성으로 개질된 메틸 셀룰로즈(HMMC), 소수성으로 개질된 메틸하이드록시프로필 셀룰로즈(HMMHPC), 소수성으로 개질된 메틸하이드록시에틸 셀룰로즈(HMMHEC), 소수성으로 개질된 카복시메틸메틸 셀룰로즈(HMCMMC), 양이온성 하이드록시에틸 셀룰로즈(양이온성 HEC) 및 소수성으로 개질된 양이온성 하이드록시에틸 셀룰로즈(양이온성 HMHEC)가 있다. 바람직한 셀룰로즈 에테르는 카복시메틸 셀룰로즈 및 하이드록시에틸 셀룰로즈이다. Cellulose ethers for use in the present invention include hydroxyethyl cellulose (HEC), hydroxypropyl cellulose (HPC), water soluble ethyl hydroxyethyl cellulose (EHEC), carboxymethyl cellulose (CMC), carboxymethyl hydroxyethyl cellulose ( CMHEC), hydroxypropylhydroxyethyl cellulose (HPHEC), methyl cellulose (MC), methylhydroxypropyl cellulose (MHPC), methylhydroxyethyl cellulose (MHEC), carboxymethylmethyl cellulose (CMMC), hydrophobically modified Carboxymethyl cellulose (HMCMC), hydrophobically modified hydroxyethyl cellulose (HMHEC), hydrophobically modified hydroxypropyl cellulose (HMHPC), hydrophobically modified ethylhydroxyethyl cellulose (HMEHEC), hydrophobically modified carboxymethyl Hydroxyethyl cellulose (HMCMHEC), hydrophobically modified hydroxypropyl hydroxyethyl cellulose (HMHPHEC), hydrophobic Hydroly modified methyl cellulose (HMMC), hydrophobically modified methylhydroxypropyl cellulose (HMMHPC), hydrophobically modified methylhydroxyethyl cellulose (HMMHEC), hydrophobically modified carboxymethylmethyl cellulose (HMCMMC), cationic hydride Hydroxyethyl cellulose (cationic HEC) and hydrophobically modified cationic hydroxyethyl cellulose (cationic HMHEC). Preferred cellulose ethers are carboxymethyl cellulose and hydroxyethyl cellulose.
본 발명에 사용하기 위한 구아 유도체로는 카복시메틸 구아(CM 구아), 하이드록시에틸 구아(HE 구아), 하이드록시프로필 구아(HP 구아), 카복시메틸하이드록시프로필 구아(CMHP 구아), 양이온성 구아, 소수성으로 개질된 구아(HM 구아), 소수성으로 개질된 카복시메틸 구아(HMCM 구아), 소수성으로 개질된 하이드록시에틸 구아(HMHE 구아), 소수성으로 개질된 하이드록시프로필 구아(HMHP 구아), 소수성으로 개질된 양이온성 하이드록시프로필 구아(양이온성 HMHP 구아), 소수성으로 개질된 카복시메틸하이드록시프로필 구아(HMCMHP 구아) 및 소수성으로 개질된 양이온성 구아(HM 양이온성 구아)가 있다. Guar derivatives for use in the present invention include carboxymethyl guar (CM guar), hydroxyethyl guar (HE guar), hydroxypropyl guar (HP guar), carboxymethylhydroxypropyl guar (CMHP guar), cationic guar Hydrophobically modified guar (HM guar), hydrophobically modified carboxymethyl guar (HMCM guar), hydrophobically modified hydroxyethyl guar (HMHE guar), hydrophobically modified hydroxypropyl guar (HMHP guar), hydrophobic Cationic hydroxypropyl guar (cationic HMHP guar), hydrophobically modified carboxymethylhydroxypropyl guar (HMCMHP guar) and hydrophobically modified cationic guar (HM cationic guar).
본 발명의 조성물을 제조하는데 사용하기 위한 보다 바람직한 다당류는 카복시메틸 셀룰로즈, 카라기난 및 펙틴, 또는 이들의 혼합물이다. 카복시메틸 셀룰로즈가 가장 바람직하다. More preferred polysaccharides for use in preparing the compositions of the present invention are carboxymethyl cellulose, carrageenan and pectin, or mixtures thereof. Most preferred is carboxymethyl cellulose.
수용성 또는 수팽윤성 중합체를 응집시키기 위해 사용된 폴리올로는 당, 당 알콜, 글리세롤, 폴리에틸렌 글리콜, 프로필렌 글리콜 및 이들의 혼합물이 있지만, 이에 제한되는 것은 아니다. Polyols used to aggregate the water soluble or water swellable polymers include, but are not limited to, sugars, sugar alcohols, glycerol, polyethylene glycols, propylene glycols, and mixtures thereof.
당의 예로는 수크로즈, 글루코즈, 락토즈, 프럭토즈 및 자일로즈, 또는 이들의 혼합물이 있다. 당 알콜의 예로는 소르비톨, 이노시톨, 만니톨, 갈락티돌, 아라비톨, 리비톨, 자일리톨 및 이들의 혼합물이 있다. Examples of sugars are sucrose, glucose, lactose, fructose and xylose, or mixtures thereof. Examples of sugar alcohols are sorbitol, inositol, mannitol, galactidol, arabitol, ribitol, xylitol and mixtures thereof.
본 발명에 사용하기에 바람직한 폴리올은 소르비톨 및 폴리에틸렌 글리콜, 또는 이들의 혼합물이다. 본 발명에 사용하기 위한 폴리에틸렌 글리콜의 분자량은 제한되지 않는다. 바람직하게, 폴리에틸렌 글리콜은 약 200 내지 약 5,000,000, 보다 바람직하게는 약 600 내지 약 25,000, 가장 바람직하게는 약 1,000 내지 약 10,000의 분자량을 갖는다. Preferred polyols for use in the present invention are sorbitol and polyethylene glycol, or mixtures thereof. The molecular weight of polyethylene glycol for use in the present invention is not limited. Preferably, the polyethylene glycol has a molecular weight of about 200 to about 5,000,000, more preferably about 600 to about 25,000, most preferably about 1,000 to about 10,000.
본 발명의 조성물에서, 응집을 위해 사용되는 폴리올은 조성물의 총 중량을 기준으로 약 10중량%를 초과하는 농도로 존재한다. 폴리올의 최대 농도는 바람직하게 약 90중량%, 보다 바람직하게는 약 50중량%, 가장 바람직하게는 약 30중량%이다. In the compositions of the present invention, the polyols used for aggregation are present at concentrations greater than about 10% by weight based on the total weight of the composition. The maximum concentration of the polyol is preferably about 90% by weight, more preferably about 50% by weight and most preferably about 30% by weight.
응집된 조성물은 액체 형태의 폴리올을 입상 중합체에 분무함으로써 제조될 수 있다. 폴리올은 용융 상태이거나 용액일 수 있고, 수용액이 바람직하다. 바람직한 방법에서, 용융된 폴리올 또는 폴리올 용액을 유동층(fluidized bed)중 수용성 또는 수팽윤성의 입자상에 분무하고, 폴리올이 용액일 경우, 동시에 상기 입자를 건조시킨다. 상업적으로 입수가능한 유동층 분무 유닛이 상기 조작에 사용될 수 있다. Aggregated compositions can be prepared by spraying a polyol in liquid form onto the particulate polymer. The polyols may be molten or in solution, with aqueous solutions being preferred. In a preferred method, the molten polyol or polyol solution is sprayed onto water soluble or water swellable particles in a fluidized bed, and when the polyol is a solution, the particles are dried at the same time. Commercially available fluidized bed spray units can be used for this operation.
본 발명의 응집된 조성물은 물 또는 물을 함유한 용매중에서 중합체 덩어리를 형성하지 않으면서 상응하는 미처리된 수용성 또는 수팽윤성 중합체에 비해 실질적으로 신속하게 수화되거나 용해된다. 이러한 수화 또는 용해 속도는 하크 비스코 시험기(Haake Visco Tester) 501을 사용하여 측정되며, 이는 중합체가 수화되고 농조화될 경우 설정 속도(400rpm)에서 용액중 센서의 회전을 유지하는데 요구되는 토크(힘)의 양을 측정한다. 수화 시간은 최종 점성의 95%를 달성하는데 걸리는 시간(분)으로 고려되고, 이때 최종 점성은 2시간의 시험 동안 마지막 20분간의 점성의 평균치이다. The agglomerated compositions of the present invention hydrate or dissolve substantially rapidly compared to the corresponding untreated water soluble or water swellable polymers without forming a polymer mass in water or a solvent containing water. This rate of hydration or dissolution is measured using a Haake Visco Tester 501, which is the torque (force) required to maintain the rotation of the sensor in solution at a set rate (400 rpm) when the polymer is hydrated and thickened. Measure the amount of. Hydration time is considered the number of minutes it takes to achieve 95% of the final viscosity, where final viscosity is the average of the last 20 minutes of viscosity over a two hour test.
상기 작업시, 물에서의 수화는 55℃에서 측정되었다. 예를 들면, 상기 조건하에서, 미처리된 카복시메틸 셀룰로즈는 즉시 덩어리지고, 이후 95% 점성에 도달하기 위해 약 15분이 요구되었다. 반면, 20중량%의 소르비톨 또는 20중량%의 폴리에틸렌 글리콜로 처리함으로써 응집된 카복시메틸 셀룰로즈는 어느 정도는 즉시 덩어리졌지만, 이는 1분 이내에 재빨리 분산되고 용해되었다. In this operation, hydration in water was measured at 55 ° C. For example, under the above conditions, the untreated carboxymethyl cellulose massed immediately and then required about 15 minutes to reach 95% viscosity. On the other hand, the carboxymethyl cellulose aggregated by treatment with 20% by weight of sorbitol or 20% by weight of polyethylene glycol immediately massed to some extent, but quickly dispersed and dissolved within 1 minute.
상기 조성물의 추가의 이점은, 응집 현상이 미처리된 중합체를 취급할 경우 발생하는 더스트의 양을 감소시키는 작용을 한다는 것이다. A further advantage of the composition is that the agglomeration phenomenon acts to reduce the amount of dust that occurs when handling untreated polymers.
본 발명의 치약은 연마제, 보습제 및 수용성 중합체를 함유한다. 보습제는 치약에서 특히 치약이 공기와 지속적으로 접촉될 수 있는 튜브의 노즐 말단부에서 수분을 보존하기 위해 사용된다. 수용성 중합체는 성분들에 대한 농조화제 및 결합제로서 작용한다. 풍미제, 감미제, 방부제, 세제, 치석 억제제(tartar control agent), 플라크 억제제 및 불화물 등의 다양한 다른 성분들이 또한 저농도로 사용될 수 있다. The toothpaste of the present invention contains an abrasive, a humectant and a water soluble polymer. Moisturizers are used in toothpaste, particularly to preserve moisture at the nozzle end of the tube where the toothpaste can be in constant contact with air. The water soluble polymer acts as a thickening agent and binder for the components. Various other ingredients may also be used at low concentrations, such as flavors, sweeteners, preservatives, detergents, tartar control agents, plaque inhibitors and fluorides.
본 발명의 치약에 사용하기 위한 치과용 연마제로는 전형적으로 실리카 및 불용성 무기염이 있다. 바람직한 무기염으로는 탄산칼슘, 이염기성 인산칼슘, 삼염기성 인산칼슘, 황산칼슘, 불용성 메타인산 나트륨, 수화된 산화알루미늄, 및 탄산마그네슘 및 인산마그네슘이 있다. 실리카 및 실리카 제로겔이 특히 반투명 또는 투명 치약에 유용하다. Dental abrasives for use in the toothpaste of the present invention typically include silica and insoluble inorganic salts. Preferred inorganic salts are calcium carbonate, dibasic calcium phosphate, tribasic calcium phosphate, calcium sulfate, insoluble sodium metaphosphate, hydrated aluminum oxide, and magnesium carbonate and magnesium phosphate. Silica and silica zero gels are particularly useful for translucent or transparent toothpastes.
본 발명의 치약에 사용하기 위한 전형적인 보습제로는 글리세롤, 소르비톨, 프로필렌 글리콜, 또는 이들의 혼합물이 있고, 이들은 물 등의 적합한 보습제 비히클과 혼합된다. Typical moisturizers for use in the toothpaste of the present invention are glycerol, sorbitol, propylene glycol, or mixtures thereof, which are mixed with a suitable moisturizer vehicle such as water.
본 발명의 치약에서, 응집된 수용성 또는 수팽윤성 중합체는 응집된 수용성 또는 수팽윤성 중합체의 총 중량을 기준으로 약 0.5 내지 약 90중량% 농도의 폴리올을 함유할 수 있다. 바람직한 농도는 약 2 내지 약 50중량%이고, 보다 바람직하게는 약 10 내지 약 30중량%이다. In the toothpaste of the invention, the aggregated water soluble or water swellable polymer may contain a polyol at a concentration of about 0.5 to about 90 weight percent based on the total weight of the aggregated water soluble or water swellable polymer. Preferred concentrations are about 2 to about 50 weight percent, more preferably about 10 to about 30 weight percent.
본 발명의 치약을 제조할 경우 완전한 치약 제형을 수득하기 위해, 폴리올로 처리함으로써 응집된 수용성 또는 수팽윤성 중합체를 a) 보습제 또는 보습제 혼합물, b) 보습제 비히클, 가장 전형적으로는 물; c) 염, 풍미제, 착색제, 계면활성제, 및 d) 연마제와 함께 교반한다. 바람직한 제조 방법에서, 응집된 수용성 중합체를 직접 보습제와 보습제 비히클의 혼합물에 첨가하고, 중합체 입자가 완전히 용해되고 팽윤될 때까지 교반한다. 그런 다음, 임의의 염을 첨가한 후, 연마제를 첨가한다. 연마제는 염이 완전히 용해된 후 첨가한다. 혼합물은 연마제의 입자가 습윤될 때까지 교반하고, 그런 다음, 풍미제를 첨가한 후 계면활성제를 첨가한다. In the preparation of the toothpaste of the invention, in order to obtain a complete toothpaste formulation, the aggregated water-soluble or water-swellable polymers are treated with a polyol to a) a moisturizer or moisturizer mixture, b) a moisturizer vehicle, most typically water; c) with salts, flavors, colorants, surfactants, and d) abrasives. In a preferred manufacturing method, the aggregated water soluble polymer is added directly to the mixture of the humectant and humectant vehicle and stirred until the polymer particles are completely dissolved and swelled. Then, after adding any salt, the abrasive is added. The abrasive is added after the salt is completely dissolved. The mixture is stirred until the particles of abrasive are wet, and then the flavoring agent is added followed by the surfactant.
본 발명은 하기 실시예에 의해 설명되고 있지만, 이는 단지 예시하기 위한 것으로 제한하려는 것은 아니다. 모든 백분율, 부 등은 별도의 지시가 없는 한 중량을 기준으로 한다. The invention is illustrated by the following examples, which are intended to be illustrative only and not intended to be limiting. All percentages, parts, etc., are by weight unless otherwise indicated.
실시예 1 내지 14는 폴리에틸렌 글리콜 또는 소르비톨로 처리함으로써 응집된 카복시메틸 셀룰로즈 및 카라기난의 제조 및 시험을 나타낸다. 카라기난으로는 등록상표 GENU 카라기난(델라웨어주 윌밍턴 소재의 헤르큘레스 인코포레이티드(Hercules Incorporated) 제품)을 사용하였다. 카복시메틸 셀룰로즈로는 CMC 7MF 또는 CMC 7MXF(델라웨어주 윌밍턴 소재의 헤르큘레스 인코포레이티드 제품)를 사용하였다. Examples 1-14 show the preparation and testing of aggregated carboxymethyl cellulose and carrageenan by treatment with polyethylene glycol or sorbitol. Carrageenan was used under the trademark GENU Carrageenan (Hercules Incorporated, Wilmington, Delaware). As carboxymethyl cellulose, CMC 7MF or CMC 7MXF (Hercules Incorporated, Wilmington, Delaware) was used.
중합체를 글래트 유체층 처리장치(Glatt Fluid Bed Processor)(모델 GPCG-5) 상부 분무 유닛에서 폴리에틸렌 글리콜, PEG 4600 및 1450(유니온 카바이드(Union Carbide), 등록상표 Carbowax 4600 및 1450)의 수용액(25, 33 및 50%)으로 처리하여 약 20중량%의 최종 폴리올 농도가 되도록 하였다. 또한, 소르비톨의 70% 수용액을 가함으로써 이들을 10% 및 20% 농도의 소르비톨로 처리하였다. Polymers were treated with an aqueous solution of polyethylene glycol, PEG 4600 and 1450 (Union Carbide®, Carbowax 4600 and 1450) in a Glat Fluid Bed Processor (model GPCG-5) top spray unit. , 33 and 50%) to a final polyol concentration of about 20% by weight. Furthermore, they were treated with sorbitol at 10% and 20% concentrations by adding a 70% aqueous solution of sorbitol.
조작시, 모든 폴리올 수용액을 50℃로 가열하고, 눈금교정된 펌프 및 저울로 계측하였다. 모든 실험에 있어서, 글래트 유체층 처리장치를 예열하였다. 슐리크(Schlick) 945 노즐을 30분/3초의 여과기 진탕 사이클로 사용하였으며, 입자 크기가 증가한 후 2분/3초로 감소시켰다. 분무 공기압을 2bar로 설정하였다. 모든 생성물을 약 6 내지 8% 습도로 건조시킨 후, 30 내지 34℃로 냉각하였다. 배치 크기는 3kg이었다. In operation, all polyol aqueous solutions were heated to 50 ° C. and measured with a calibrated pump and balance. In all experiments, the glat fluid bed treating apparatus was preheated. The Schlick 945 nozzle was used for a 30 min / 3 sec filter shake cycle and reduced to 2 min / 3 sec after increasing the particle size. The atomizing air pressure was set to 2 bar. All products were dried to about 6-8% humidity and then cooled to 30-34 ° C. The batch size was 3 kg.
FL 10 센서가 구비된 하크 VT 501 점도계를 사용하여, 응집된 시료 및 미처리 대조군을 55℃에서 탈이온수중 이들의 분산성 및 수화/용해 특성에 대해 평가하였다. 기기에서, 중합체가 수화되고 농조화됨에 따라 설정 속도(400rpm)에서 용액중 센서의 회전을 유지시키는데 필요한 토크(힘)의 양을 측정한다. 그런 다음, 이 데이터를 컴퓨터를 이용해 수학적으로 점성(cps)으로 전환시킨다. Agglomerated samples and untreated controls were evaluated for their dispersibility and hydration / dissolution characteristics in deionized water at 55 ° C. using a Hark VT 501 viscometer with FL 10 sensor. In the instrument, the amount of torque (force) required to maintain the rotation of the sensor in solution at a set speed (400 rpm) is measured as the polymer hydrates and thickens. The data is then mathematically converted into viscosities (cps) using a computer.
표 1에 보고된 수화 시간은 두시간의 가동중 마지막 20분 동안의 점성을 100%로 할 경우 95%의 점성에 도달하는데 요구되는 시간(분)이다. 각 시료의 점성은 총 용액 중량을 기준으로 2% 농도에서 수행되었다. 시료중 폴리올 또는 수분의 양에 대해서는 어떠한 보정도 이루어지지 않았다. The hydration time reported in Table 1 is the time (in minutes) required to reach 95% viscosity at 100% viscosity during the last 20 minutes of two hours of operation. The viscosity of each sample was performed at 2% concentration based on the total solution weight. No correction was made to the amount of polyol or moisture in the sample.
실시예 1 내지 8 및 비교예 AExamples 1-8 and Comparative Example A
이 실시예는 소르비톨 및 폴리에틸렌 글리콜로 처리된 카라기난의 응집을 예시한다. 데이터는 표 1에 나타나 있다. 미처리된 카라기난의 수화 시간을 제시하기 위해 비교예 A를 제시한다. This example illustrates the aggregation of carrageenan treated with sorbitol and polyethylene glycol. The data is shown in Table 1. Comparative Example A is shown to show the hydration time of untreated carrageenan.
실시예 9 내지 14와 비교예 B 및 CExamples 9-14 and Comparative Examples B and C
이 실시예는 소르비톨 및 폴리에틸렌 글리콜로 처리된 카복시메틸 셀룰로즈의 응집을 예시한다. 데이터는 표 2에 나타나 있다. 미처리된 카복시메틸 셀룰로즈에 대한 수화 시간을 제시하기 위해 비교예 B와 C를 제공하였다. This example illustrates the aggregation of carboxymethyl cellulose treated with sorbitol and polyethylene glycol. The data is shown in Table 2. Comparative Examples B and C were provided to show the hydration time for untreated carboxymethyl cellulose.
데이터에서는 카복시메틸 셀룰로즈의 수화 시간이 10%이상 농도의 소르비톨 또는 폴리에틸렌 글리콜로 응집시킴으로써 실질적으로 감소함을 나타낸다. The data show that the hydration time of carboxymethyl cellulose is substantially reduced by flocculation with sorbitol or polyethylene glycol at a concentration of at least 10%.
실시예 15 및 16과 비교예 D 및 EExamples 15 and 16 and Comparative Examples D and E
이 실시예는 소르비톨 또는 폴리에틸렌 글리콜로 처리함으로써 응집된 카복시메틸 셀룰로즈를 이용한 치약의 배합을 예시한다. 비교예는 미처리된 카복시메틸 셀룰로즈가 사용된 대조 조성물의 제형을 나타낸다. This example illustrates the formulation of a toothpaste with carboxymethyl cellulose aggregated by treatment with sorbitol or polyethylene glycol. Comparative Examples show the formulation of a control composition in which untreated carboxymethyl cellulose was used.
실시예 15 및 16은 각각 9% 소르비톨 및 16% 폴리에틸렌 글리콜(PEG 1450)로 처리함으로써 응집된 카복시메틸 셀룰로즈 CMC 7MF를 사용하여 실온에서 치약을 제조하는 것을 예시한다. 비교예 D 및 E는 CMC 7MF로 처리되지 않은 유사한 제형을 나타낸다. 각 제형에 대한 성분 및 그의 농도는 표 3에 나열되고 있다. Examples 15 and 16 illustrate the preparation of toothpaste at room temperature using aggregated carboxymethyl cellulose CMC 7MF by treatment with 9% sorbitol and 16% polyethylene glycol (PEG 1450), respectively. Comparative Examples D and E show similar formulations not treated with CMC 7MF. The components and their concentrations for each formulation are listed in Table 3.
글리세롤이 없는 제형의 경우(실시예 15, 16 및 비교예 E), 하기 절차가 사용되었다: For formulations without glycerol (Examples 15, 16 and Comparative Example E), the following procedure was used:
1. 테트라 소듐 피로포스페이트(0.42부), 소듐 사카린(0.20부), 소듐 모노플루오로포스페이트(0.76부) 및 벤조산 나트륨(0.50부)을 교반하에 6.25부의 물에 첨가하고, 약 60℃에서 가열하여 용해시켰다. Tetrasodium pyrophosphate (0.42 parts), sodium saccharin (0.20 parts), sodium monofluorophosphate (0.76 parts) and sodium benzoate (0.50 parts) are added to 6.25 parts of water under stirring and heated at about 60 DEG C. Dissolved.
2. 카복시메틸 셀룰로즈(1.10부)를 비이커중 소르비톨 용액(35.43부)에 첨가하고, 15분 동안 또는 적절하게 분산될 때까지 교반하였다. 그런 다음, 8.79부의 물을 첨가하고, 생성된 혼합물을 15 내지 30분 동안 교반하여 중합체가 완전히 수화(겔이 없음)되도록 하였다. 그런 다음, 단계 1로부터의 따뜻한 염 용액을 교반하에 첨가하였고, 15분 동안 또는 균질화(덩어리 또는 겔이 없음)될 때까지 교반을 지속하였다. 그런 다음, 혼합물을 로스 이중 유성형 혼합기(Ross double planetary mixer)로 옮겼다. 2. Carboxymethyl cellulose (1.10 parts) was added to a sorbitol solution (35.43 parts) in a beaker and stirred for 15 minutes or until properly dispersed. Then 8.79 parts of water was added and the resulting mixture was stirred for 15-30 minutes to allow the polymer to fully hydrate (no gel). The warm salt solution from step 1 was then added under stirring and stirring continued for 15 minutes or until homogenized (no lumps or gels). The mixture was then transferred to a Ross double planetary mixer.
3. 이수화 인산이칼슘(DCP)(45.00부)을 혼합기에 넣고, DCP를 완전히 습윤시키기 위해 10분 동안 지속적으로 혼합하였다. 그런 다음, 혼합기를 개봉하고 교반기(beater) 및 용기 측면을 긁어내었다. 그런 다음, 혼합기를 닫고, 진공시키고, 20분 동안 또는 혼합물이 유연해 질때까지 고속하에 지속적으로 혼합하였다. 3. Dihydrate dicalcium phosphate (DCP) (45.00 parts) was placed in a mixer and mixed continuously for 10 minutes to fully wet the DCP. The mixer was then opened and the beater and vessel sides scraped off. The mixer was then closed, vacuumed and continuously mixed at high speed for 20 minutes or until the mixture became soft.
4. 그런 다음, 소듐 라우릴 설페이트(1.00부)를 첨가하고, 진공없이 5분 동안 저속에서 지속적으로 혼합하였다. 그런 다음, 풍미제(0.55부)를 첨가한 후, 저속에서 2분 동안 혼합하였다. 그런 다음, 혼합기를 개방하고, 교반기 및 용기 측면을 긁어내었다. 그런 다음, 혼합기를 닫고, 진공시키고, 15분 동안 중간 속도에서 지속적으로 혼합하였다. 혼합기의 작동을 중단시키고, 진공을 없애고, 치약을 충진시켰다. 4. Sodium lauryl sulfate (1.00 parts) was then added and mixing was continued at low speed for 5 minutes without vacuum. Then flavor (0.55 parts) was added and mixed for 2 minutes at low speed. The mixer was then opened and the stirrer and vessel sides scraped off. The mixer was then closed, vacuumed and mixed continuously at medium speed for 15 minutes. The mixer was shut down, the vacuum removed and the toothpaste filled.
글리세롤이 사용된 비교예 D에서, 절차는 단계 2에서 카복시메틸 셀룰로즈를 교반하에 글리세롤에 분산시킴을 제외하고 상기와 본질적으로 동일하였다. 5분 동안 또는 카복시메틸 셀룰로즈가 적절하게 분산될 때까지 지속적으로 교반하였다. 그런 다음, 소르비톨 용액을 첨가하고, 추가로 10분 동안 지속적으로 교반하였다. 물(14.36부)을 첨가하고, 15 내지 30분 동안 지속적으로 교반하여 중합체가 완전히 수화(겔이 없음)되도록 하였다. 따뜻한 염 용액을 첨가하고, 15분 동안 또는 균질화(덩어리 또는 겔이 없음)될 때까지 지속적으로 교반하였다. 그런 다음, 남은 단계를 위해 혼합물을 로스 혼합기로 옮겼다. In Comparative Example D in which glycerol was used, the procedure was essentially the same as above except dispersing the carboxymethyl cellulose in glycerol under agitation in step 2. Stirring is continued for 5 minutes or until the carboxymethyl cellulose is properly dispersed. Then, sorbitol solution was added and stirring continued for an additional 10 minutes. Water (14.36 parts) was added and stirring continued for 15-30 minutes to allow the polymer to fully hydrate (no gel). Warm salt solution was added and stirring continued for 15 minutes or until homogenized (no lumps or gels). Then, the mixture was transferred to a Ross mixer for the remaining steps.
실시예 15 및 16에서, 응집된 카복시메틸 셀룰로즈가 소르비톨 수용액에 매우 쉽게 분산되었음을 관찰하였다. 중합체의 수화는 약 3 내지 4분내에 시작되었고, 물과 염 용액을 첨가할 때까지 천천히 진행되었다. 카복시메틸 셀룰로즈가 덩어리지는 것은 전혀 관찰되지 않았다. In Examples 15 and 16, it was observed that the aggregated carboxymethyl cellulose was very easily dispersed in aqueous sorbitol solution. Hydration of the polymer started within about 3-4 minutes and proceeded slowly until water and salt solution was added. Agglomeration of carboxymethyl cellulose was not observed at all.
비교예 D에서, 미처리된 카복시메틸 셀룰로즈는 무수 글리세롤내에서 덩어리를 형성하지 않으면서 쉽게 분산되었다. 그러나 비교예 E에서, 미처리된 카복시메틸 셀룰로즈는 매우 고속의 교반하에서만 소르비톨 용액내에서 분산되었다. 중합체의 수화는 1 내지 2분내에 시작되었다. 카복시메틸 셀룰로즈는 소르비톨/염 용액에서 약간의 덩어리를 형성하는 것으로 관찰되었다. In Comparative Example D, the untreated carboxymethyl cellulose was easily dispersed without lumping in anhydrous glycerol. In Comparative Example E, however, the untreated carboxymethyl cellulose was dispersed in the sorbitol solution only under very high speed agitation. Hydration of the polymer started within 1 to 2 minutes. Carboxymethyl cellulose was observed to form some lumps in the sorbitol / salt solution.
실시예 17 및 18과 비교예 F 및 GExamples 17 and 18 and Comparative Examples F and G
이 실시예는 55℃에서 소르비톨 또는 폴리에틸렌 글리콜로 처리함으로써 응집된 카복시메틸 셀룰로즈를 사용한 치약의 배합을 예시한다. 비교예는 미처리된 카복시메틸 셀룰로즈를 사용할 경우의 대조 조성물의 제형을 나타낸다. This example illustrates the formulation of toothpaste using carboxymethyl cellulose aggregated by treatment with sorbitol or polyethylene glycol at 55 ° C. The comparative example shows the formulation of the control composition when using untreated carboxymethyl cellulose.
실시예 17 및 18은 각각 9% 소르비톨 및 16% 폴리에틸렌 글리콜(PEG 1450)로 처리함으로써 응집된 카복시메틸 셀룰로즈 CMC 7MF를 사용하여 실온에서 치약을 제조하는 것을 예시한다. 비교예 F 및 G는 CMC 7MF가 처리되지 않을 경우의 유사한 제형을 나타낸다. 각각의 제형에 대한 성분 및 그의 농도는 표 4에 나타나 있다. Examples 17 and 18 illustrate the preparation of toothpaste at room temperature using aggregated carboxymethyl cellulose CMC 7MF by treatment with 9% sorbitol and 16% polyethylene glycol (PEG 1450), respectively. Comparative Examples F and G show similar formulations when CMC 7MF is not treated. The components and their concentrations for each formulation are shown in Table 4.
글리세롤이 없는 제형의 경우(실시예 17 및 18과 비교예 G), 하기 절차가 사용되었다: For formulations without glycerol (Examples 17 and 18 and Comparative Example G), the following procedure was used:
1. 테트라 소듐 피로포스페이트(0.42부), 소듐 사카린(0.20부), 소듐 모노플루오로포스페이트(0.76부) 및 벤조산 나트륨(0.50부)을 교반하에 6.25부의 물에 첨가하고, 약 60℃로 가열하여 용해시켰다. Tetrasodium pyrophosphate (0.42 parts), sodium saccharin (0.20 parts), sodium monofluorophosphate (0.76 parts) and sodium benzoate (0.50 parts) are added to 6.25 parts of water under stirring and heated to about 60 ° C. Dissolved.
2. 소르비톨 용액(35.43부)을 55℃로 가열한 후, 카복시메틸 셀룰로즈(1.00부)를 교반하에 첨가하고, 15분 동안 또는 적절하게 분산될 때까지 지속적으로 교반하였다. 그런 다음, 55℃로 가열된 물(8.89부)을 첨가하고, 15분 내지 30분 동안 지속적으로 교반하여 중합체가 완전히 수화(겔이 없음)되도록 하였다. 그런 다음, 단계 1로부터의 따뜻한 염 용액을 교반하에 첨가하였고, 이를 15분 동안 또는 균질화(덩어리 또는 겔이 없음)될 때까지 지속하였다. 그런 다음, 혼합물을 로스 이중 유성형 혼합기로 옮겼다. 2. The sorbitol solution (35.43 parts) was heated to 55 ° C., then carboxymethyl cellulose (1.00 parts) was added under stirring and stirring continued for 15 minutes or until properly dispersed. Water heated to 55 ° C. (8.89 parts) was then added and stirring continued for 15-30 minutes to allow the polymer to fully hydrate (no gel). Then the warm salt solution from step 1 was added under stirring and it was continued for 15 minutes or until homogenized (no lumps or gels). The mixture was then transferred to a Ross double planetary mixer.
3. 이수화 인산이칼슘(DCP)(45.00부)을 혼합기에 첨가하고, DCP를 완전히 습윤시키기 위해 10분 동안 지속적으로 혼합하였다. 그런 다음, 혼합기를 개방하고 교반기 및 용기 측면을 긁어내었다. 그런 다음, 혼합기를 닫고, 진공시키고, 20분 동안 또는 혼합물이 유연해 질때까지 지속적으로 고속하에 혼합하였다. 3. Dihydrate dicalcium phosphate (DCP) (45.00 parts) was added to the mixer and mixing was continued for 10 minutes to fully wet the DCP. Then the mixer was opened and the stirrer and vessel sides were scraped off. The mixer was then closed, vacuumed and mixed at high speed continuously for 20 minutes or until the mixture became soft.
4. 그런 다음, 소듐 라우릴 설페이트(1.00부)를 첨가하고, 진공없이 5분 동안 저속에서 지속적으로 혼합하였다. 그런 다음, 풍미제(0.55부)를 첨가한 후, 저속에서 2분 동안 혼합하였다. 그런 다음, 혼합기를 개방하고, 교반기 및 용기 측면을 긁어내었다. 그런 다음, 혼합기를 닫고, 진공시키고, 15분 동안 중간 속도에서 지속적으로 혼합하였다. 그런 다음, 혼합기의 작동을 중단시키고, 진공을 없애고, 치약을 충진시켰다. 4. Sodium lauryl sulfate (1.00 parts) was then added and mixing was continued at low speed for 5 minutes without vacuum. Then flavor (0.55 parts) was added and mixed for 2 minutes at low speed. The mixer was then opened and the stirrer and vessel sides scraped off. The mixer was then closed, vacuumed and mixed continuously at medium speed for 15 minutes. Then the mixer was shut down, the vacuum removed and the toothpaste filled.
비교예 F의 절차는 단지 단계 2에서만 상기와 상이하였다. 카복시메틸 셀룰로즈를 55℃에서 교반하에 글리세롤중에 분산시키고, 5분 동안 또는 적절하게 분산될 때까지 지속적으로 교반하였다. 그런 다음, 소르비톨 용액을 첨가하고, 추가로 10분 동안 지속적으로 교반하였다. 그런 다음, 55℃의 물을 첨가하고, 15 내지 30분 동안 지속적으로 교반하여 중합체가 완전히 수화(겔이 없음)되도록 한 후, 단계 1로부터의 따뜻한 염 용액을 교반하에 첨가하고, 15분 동안 또는 균질화(덩어리 또는 겔이 없음)될 때까지 지속적으로 교반하였다. 그런 다음, 혼합물을 로스 이중 유성형 혼합기로 옮겼다. The procedure of Comparative Example F differed from the above only in step 2. The carboxymethyl cellulose was dispersed in glycerol under stirring at 55 ° C. and stirred continuously for 5 minutes or until properly dispersed. Then, sorbitol solution was added and stirring continued for an additional 10 minutes. Then add water at 55 ° C. and stir continuously for 15 to 30 minutes to allow the polymer to fully hydrate (no gel), then add the warm salt solution from step 1 under stirring and for 15 minutes or Stirring was continued until homogenization (no lumps or gels). The mixture was then transferred to a Ross double planetary mixer.
실시예 17 및 18과 비교예 F에서, 카복시메틸 셀룰로즈 물질이 덩어리를 형성하지 않으면서 뜨거운 소르비톨에서 쉽고 균일하게 분산됨을 관찰하였다. 중합체의 수화는 약 1 내지 2분 후 시작되었고, 물과 염의 용액을 첨가한 후 신속하게 진행되었다. 생성된 겔 상은 매우 유연하였고, 생성된 페이스트는 유연한 크림이었다. 이와 반대로, 비교예 G에서, 미처리된 카복시메틸 셀룰로즈가 유연하게 분산되는 것은 불가능하였다. 고속의 교반하에서조차 중합체가 심하게 덩어리지는 것을 방지할 수 없었다. In Examples 17 and 18 and Comparative Example F, it was observed that the carboxymethyl cellulose material was easily and uniformly dispersed in hot sorbitol without forming agglomerates. Hydration of the polymer started after about 1 to 2 minutes and proceeded rapidly after addition of a solution of water and salt. The resulting gel phase was very flexible and the resulting paste was a flexible cream. In contrast, in Comparative Example G, it was not possible to flexibly disperse the untreated carboxymethyl cellulose. Even under high speed agitation, the polymer could not be prevented from severely clumping.
실시예 19Example 19
이 실시예는 20% 소르비톨로 처리함으로써 응집된 카라기난을 함유하는 치약의 제조를 예시한다. This example illustrates the preparation of a toothpaste containing aggregated carrageenan by treatment with 20% sorbitol.
성분: ingredient:
글리세롤 22부 Glycerol 22 parts
카라기난(20% 소르비톨로 0.96부 Carrageenan (0.96 parts of 20% sorbitol)
처리함으로써 응집됨) Agglomerated by treatment)
벤조산 나트륨 0.50부 Sodium benzoate0.50part
소듐 사카린 0.2부 Sodium Saccharin 0.2Part
테트라소듐 피로포스페이트 0.25부 0.25 parts tetrasodium pyrophosphate
소듐 모노플루오로포스페이트 0.76부 Sodium monofluorophosphate 0.76 parts
탈이온수 21.28부 Deionized Water 21.28
인산이칼슘 51.75부 Dicalcium phosphate 51.75 parts
소듐 라우릴 설페이트 1.50부 Sodium Lauryl Sulfate1.50
박하유(peppermint oil) 0.80부 0.80 parts of peppermint oil
절차:step:
소듐 사카린, 벤조산 나트륨, 응집된 카라기난, 소듐 모노플루오로포스페이트, 테트라소듐 피로포스페이트의 무수 블렌드를 글리세롤과 혼합하고, 5분 동안 교반하였다. 그런 다음, 물을 첨가하고, 생성된 혼합물을 15분 동안 66 내지 71℃에서 가열하였다. 증류수를 첨가함으로써 중량을 본래의 중량으로 재조정하였다. 혼합물을 호바트(Hobart) 혼합기로 옮기고, 인산이칼슘을 첨가하고, 생성된 혼합물을 혼합기 속도 1에서 2분 동안 교반하였다. 혼합기를 중단시키고, 용기 및 블레이드를 긁어낸 다음, 속도 2에서 10분 동안 다시 혼합하였다. Anhydrous blends of sodium saccharin, sodium benzoate, aggregated carrageenan, sodium monofluorophosphate, tetrasodium pyrophosphate were mixed with glycerol and stirred for 5 minutes. Then water was added and the resulting mixture was heated at 66-71 ° C. for 15 minutes. The weight was readjusted to the original weight by adding distilled water. The mixture was transferred to a Hobart mixer, dicalcium phosphate was added and the resulting mixture was stirred at mixer speed 1 for 2 minutes. The mixer was stopped, the vessel and the blades were scraped off, and mixed again at speed 2 for 10 minutes.
페이스트를 진공 탈기 패들(vaccum deaerating paddle)로 옮기고, 소듐 라우릴 설페이트 및 풍미유(flavor oil)를 혼합하에 첨가한 다음, 혼합물을 5분 동안 0.98bar에서 탈기하였다. 그런 다음, 생성된 치약을 저장하기 위해 튜브내로 충진하였다. The paste was transferred to a vacuum deaerating paddle, sodium lauryl sulfate and flavor oil were added under mixing, and then the mixture was degassed at 0.98 bar for 5 minutes. Then, the resulting toothpaste was filled into a tube to store it.
상기 제조 동안에, 응집된 카라기난은 덩어리를 형성하지 않으면서 신속하게 분산되었다. During the preparation, the aggregated carrageenan dispersed rapidly without forming a lump.
본원에 제시된 실시예는 본 발명을 제한하는 것으로 해석되어서는 않되며, 이는 오히려 본 발명의 특정 실시태양의 일부를 예시하기 위해 제시된 것이다. 본 발명은 첨부된 특허청구범위의 범주로부터 벗어나지 않고 다양하게 변화되고 변형될 수 있다. The examples presented herein should not be construed as limiting the invention, but rather are intended to illustrate some of the specific embodiments of the invention. The invention can be variously changed and modified without departing from the scope of the appended claims.
본 발명에 따르면, 덩어리를 형성하지 않으면서 용매에 신속하게 분산될 수 있는 중합체 조성물 및 이의 제조 방법, 및 이에 의해 제조된 치약을 제공할 수 있다. According to the present invention, it is possible to provide a polymer composition which can be rapidly dispersed in a solvent without forming a lump, a method for preparing the same, and a toothpaste produced thereby.
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