JPS62286916A - Composition for oral cavity - Google Patents
Composition for oral cavityInfo
- Publication number
- JPS62286916A JPS62286916A JP13117786A JP13117786A JPS62286916A JP S62286916 A JPS62286916 A JP S62286916A JP 13117786 A JP13117786 A JP 13117786A JP 13117786 A JP13117786 A JP 13117786A JP S62286916 A JPS62286916 A JP S62286916A
- Authority
- JP
- Japan
- Prior art keywords
- abrasive
- hydrogen phosphate
- calcium hydrogen
- sodium
- calcium
- 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.)
- Pending
Links
- 239000000203 mixture Substances 0.000 title claims abstract description 22
- 210000000214 mouth Anatomy 0.000 title claims abstract description 7
- 235000019700 dicalcium phosphate Nutrition 0.000 claims abstract description 44
- FUFJGUQYACFECW-UHFFFAOYSA-L calcium hydrogenphosphate Chemical compound [Ca+2].OP([O-])([O-])=O FUFJGUQYACFECW-UHFFFAOYSA-L 0.000 claims abstract description 43
- 150000002222 fluorine compounds Chemical class 0.000 claims abstract description 22
- 239000002245 particle Substances 0.000 claims abstract description 18
- 238000002441 X-ray diffraction Methods 0.000 claims abstract description 10
- -1 aluminum compound Chemical class 0.000 claims abstract description 7
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 6
- 238000010304 firing Methods 0.000 claims description 16
- 150000002681 magnesium compounds Chemical class 0.000 claims description 4
- 229910052783 alkali metal Inorganic materials 0.000 claims description 3
- 150000001340 alkali metals Chemical class 0.000 claims description 2
- 229940074371 monofluorophosphate Drugs 0.000 claims description 2
- 238000005498 polishing Methods 0.000 abstract description 23
- 238000000034 method Methods 0.000 abstract description 14
- 230000000694 effects Effects 0.000 abstract description 10
- 239000003795 chemical substances by application Substances 0.000 abstract description 9
- 238000011086 high cleaning Methods 0.000 abstract description 9
- 239000013078 crystal Substances 0.000 abstract description 8
- 230000007774 longterm Effects 0.000 abstract description 5
- 238000001354 calcination Methods 0.000 abstract description 4
- 150000003839 salts Chemical class 0.000 abstract description 4
- 238000002356 laser light scattering Methods 0.000 abstract description 3
- 238000004438 BET method Methods 0.000 abstract description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052749 magnesium Inorganic materials 0.000 abstract description 2
- 239000011777 magnesium Substances 0.000 abstract description 2
- DWYMPOCYEZONEA-UHFFFAOYSA-N fluorophosphoric acid Chemical compound OP(O)(F)=O DWYMPOCYEZONEA-UHFFFAOYSA-N 0.000 abstract 1
- 238000004321 preservation Methods 0.000 abstract 1
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 20
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 16
- XGRSAFKZAGGXJV-UHFFFAOYSA-N 3-azaniumyl-3-cyclohexylpropanoate Chemical compound OC(=O)CC(N)C1CCCCC1 XGRSAFKZAGGXJV-UHFFFAOYSA-N 0.000 description 15
- 238000004519 manufacturing process Methods 0.000 description 15
- 229960004711 sodium monofluorophosphate Drugs 0.000 description 15
- 229940034610 toothpaste Drugs 0.000 description 14
- 239000000606 toothpaste Substances 0.000 description 14
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 12
- 239000003205 fragrance Substances 0.000 description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 11
- 235000011187 glycerol Nutrition 0.000 description 10
- JUNWLZAGQLJVLR-UHFFFAOYSA-J calcium diphosphate Chemical compound [Ca+2].[Ca+2].[O-]P([O-])(=O)OP([O-])([O-])=O JUNWLZAGQLJVLR-UHFFFAOYSA-J 0.000 description 9
- 229940043256 calcium pyrophosphate Drugs 0.000 description 9
- 239000001768 carboxy methyl cellulose Substances 0.000 description 9
- 235000019821 dicalcium diphosphate Nutrition 0.000 description 9
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 8
- 239000003082 abrasive agent Substances 0.000 description 8
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 description 8
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 8
- 239000000920 calcium hydroxide Substances 0.000 description 8
- 235000011116 calcium hydroxide Nutrition 0.000 description 8
- GVALZJMUIHGIMD-UHFFFAOYSA-H magnesium phosphate Chemical compound [Mg+2].[Mg+2].[Mg+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O GVALZJMUIHGIMD-UHFFFAOYSA-H 0.000 description 8
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 description 8
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 description 8
- 235000019333 sodium laurylsulphate Nutrition 0.000 description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 7
- 238000004140 cleaning Methods 0.000 description 7
- XPPKVPWEQAFLFU-UHFFFAOYSA-N diphosphoric acid Chemical compound OP(O)(=O)OP(O)(O)=O XPPKVPWEQAFLFU-UHFFFAOYSA-N 0.000 description 7
- 239000000047 product Substances 0.000 description 7
- 229940005657 pyrophosphoric acid Drugs 0.000 description 7
- 239000002994 raw material Substances 0.000 description 6
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 5
- 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 5
- 239000002253 acid Substances 0.000 description 5
- 239000007900 aqueous suspension Substances 0.000 description 5
- 229910001424 calcium ion Inorganic materials 0.000 description 5
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 5
- 229910052708 sodium Inorganic materials 0.000 description 5
- 239000011734 sodium Substances 0.000 description 5
- GYDJEQRTZSCIOI-LJGSYFOKSA-N tranexamic acid Chemical compound NC[C@H]1CC[C@H](C(O)=O)CC1 GYDJEQRTZSCIOI-LJGSYFOKSA-N 0.000 description 5
- 229960000401 tranexamic acid Drugs 0.000 description 5
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 4
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 4
- ILRRQNADMUWWFW-UHFFFAOYSA-K aluminium phosphate Chemical compound O1[Al]2OP1(=O)O2 ILRRQNADMUWWFW-UHFFFAOYSA-K 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- VEJCUEBBRSCJRP-UHFFFAOYSA-L calcium;hydron;phosphonato phosphate Chemical compound [Ca+2].OP(O)(=O)OP([O-])([O-])=O VEJCUEBBRSCJRP-UHFFFAOYSA-L 0.000 description 4
- 210000003298 dental enamel Anatomy 0.000 description 4
- 229910052731 fluorine Inorganic materials 0.000 description 4
- 239000011737 fluorine Substances 0.000 description 4
- 210000004209 hair Anatomy 0.000 description 4
- 230000006872 improvement Effects 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- CVHZOJJKTDOEJC-UHFFFAOYSA-N saccharin Chemical compound C1=CC=C2C(=O)NS(=O)(=O)C2=C1 CVHZOJJKTDOEJC-UHFFFAOYSA-N 0.000 description 4
- FQENQNTWSFEDLI-UHFFFAOYSA-J sodium diphosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])([O-])=O FQENQNTWSFEDLI-UHFFFAOYSA-J 0.000 description 4
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 description 4
- 229940048086 sodium pyrophosphate Drugs 0.000 description 4
- 238000003860 storage Methods 0.000 description 4
- 239000000725 suspension Substances 0.000 description 4
- 235000019818 tetrasodium diphosphate Nutrition 0.000 description 4
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 description 4
- 239000002202 Polyethylene glycol Substances 0.000 description 3
- 230000001680 brushing effect Effects 0.000 description 3
- 229940043430 calcium compound Drugs 0.000 description 3
- 150000001674 calcium compounds Chemical class 0.000 description 3
- 239000000292 calcium oxide Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 239000004137 magnesium phosphate Substances 0.000 description 3
- 229910000157 magnesium phosphate Inorganic materials 0.000 description 3
- 229960002261 magnesium phosphate Drugs 0.000 description 3
- 229910000400 magnesium phosphate tribasic Inorganic materials 0.000 description 3
- 235000010994 magnesium phosphates Nutrition 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000003607 modifier Substances 0.000 description 3
- 238000006386 neutralization reaction Methods 0.000 description 3
- 229920001223 polyethylene glycol Polymers 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 230000006641 stabilisation Effects 0.000 description 3
- 238000011105 stabilization Methods 0.000 description 3
- MOMKYJPSVWEWPM-UHFFFAOYSA-N 4-(chloromethyl)-2-(4-methylphenyl)-1,3-thiazole Chemical compound C1=CC(C)=CC=C1C1=NC(CCl)=CS1 MOMKYJPSVWEWPM-UHFFFAOYSA-N 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 description 2
- 108010010803 Gelatin Proteins 0.000 description 2
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 2
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 2
- XLRMTAAGTMNKDL-UHFFFAOYSA-H O.O.OP([O-])(=O)OP(=O)([O-])[O-].[Ca+2].OP([O-])(=O)OP(=O)([O-])[O-].[Ca+2].[Ca+2] Chemical compound O.O.OP([O-])(=O)OP(=O)([O-])[O-].[Ca+2].OP([O-])(=O)OP(=O)([O-])[O-].[Ca+2].[Ca+2] XLRMTAAGTMNKDL-UHFFFAOYSA-H 0.000 description 2
- 239000004480 active ingredient Substances 0.000 description 2
- 239000012298 atmosphere Substances 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 229910000019 calcium carbonate Inorganic materials 0.000 description 2
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 description 2
- 238000010828 elution Methods 0.000 description 2
- 229920000159 gelatin Polymers 0.000 description 2
- 239000008273 gelatin Substances 0.000 description 2
- 235000019322 gelatine Nutrition 0.000 description 2
- 235000011852 gelatine desserts Nutrition 0.000 description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 2
- 229920000137 polyphosphoric acid Polymers 0.000 description 2
- 239000003755 preservative agent Substances 0.000 description 2
- 239000008213 purified water Substances 0.000 description 2
- 239000011775 sodium fluoride Substances 0.000 description 2
- 235000013024 sodium fluoride Nutrition 0.000 description 2
- 235000019983 sodium metaphosphate Nutrition 0.000 description 2
- 239000000600 sorbitol Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- AMGNHZVUZWILSB-UHFFFAOYSA-N 1,2-bis(2-chloroethylsulfanyl)ethane Chemical compound ClCCSCCSCCCl AMGNHZVUZWILSB-UHFFFAOYSA-N 0.000 description 1
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 description 1
- 239000004254 Ammonium phosphate Substances 0.000 description 1
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 1
- 244000025254 Cannabis sativa Species 0.000 description 1
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 1
- GHXZTYHSJHQHIJ-UHFFFAOYSA-N Chlorhexidine Chemical compound C=1C=C(Cl)C=CC=1NC(N)=NC(N)=NCCCCCCN=C(N)N=C(N)NC1=CC=C(Cl)C=C1 GHXZTYHSJHQHIJ-UHFFFAOYSA-N 0.000 description 1
- 108010001682 Dextranase Proteins 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 239000004354 Hydroxyethyl cellulose Substances 0.000 description 1
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 description 1
- 239000005639 Lauric acid Substances 0.000 description 1
- AOMUHOFOVNGZAN-UHFFFAOYSA-N N,N-bis(2-hydroxyethyl)dodecanamide Chemical compound CCCCCCCCCCCC(=O)N(CCO)CCO AOMUHOFOVNGZAN-UHFFFAOYSA-N 0.000 description 1
- 241000208125 Nicotiana Species 0.000 description 1
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 1
- 239000004677 Nylon Substances 0.000 description 1
- FWKJBIILMKHXEI-UHFFFAOYSA-L P.P(=O)(O)([O-])[O-].[Ca+2] Chemical compound P.P(=O)(O)([O-])[O-].[Ca+2] FWKJBIILMKHXEI-UHFFFAOYSA-L 0.000 description 1
- 101001004719 Phaseolus vulgaris Alpha-amylase inhibitor 2 Proteins 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-L Phosphate ion(2-) Chemical compound OP([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-L 0.000 description 1
- UEDUENGHJMELGK-HYDKPPNVSA-N Stevioside Chemical compound O([C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1O[C@]12C(=C)C[C@@]3(C1)CC[C@@H]1[C@@](C)(CCC[C@]1([C@@H]3CC2)C)C(=O)O[C@H]1[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O1)O)[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O UEDUENGHJMELGK-HYDKPPNVSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical compound [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 229910001515 alkali metal fluoride Inorganic materials 0.000 description 1
- 229910000318 alkali metal phosphate Inorganic materials 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical group [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- 229910000148 ammonium phosphate Inorganic materials 0.000 description 1
- 235000019289 ammonium phosphates Nutrition 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 235000019606 astringent taste Nutrition 0.000 description 1
- 238000001479 atomic absorption spectroscopy Methods 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000001110 calcium chloride Substances 0.000 description 1
- 229910001628 calcium chloride Inorganic materials 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- XAAHAAMILDNBPS-UHFFFAOYSA-L calcium hydrogenphosphate dihydrate Chemical compound O.O.[Ca+2].OP([O-])([O-])=O XAAHAAMILDNBPS-UHFFFAOYSA-L 0.000 description 1
- 229910001861 calcium hydroxide 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
- 239000003575 carbonaceous material Substances 0.000 description 1
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 1
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 1
- 239000004359 castor oil Substances 0.000 description 1
- 235000019438 castor oil Nutrition 0.000 description 1
- 229960003260 chlorhexidine Drugs 0.000 description 1
- 235000019504 cigarettes Nutrition 0.000 description 1
- 239000011362 coarse particle Substances 0.000 description 1
- 239000008119 colloidal silica Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000009849 deactivation Effects 0.000 description 1
- 208000002925 dental caries Diseases 0.000 description 1
- 210000004268 dentin Anatomy 0.000 description 1
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 description 1
- MHJAJDCZWVHCPF-UHFFFAOYSA-L dimagnesium phosphate Chemical compound [Mg+2].OP([O-])([O-])=O MHJAJDCZWVHCPF-UHFFFAOYSA-L 0.000 description 1
- 229910000395 dimagnesium phosphate Inorganic materials 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- MOTZDAYCYVMXPC-UHFFFAOYSA-N dodecyl hydrogen sulfate Chemical compound CCCCCCCCCCCCOS(O)(=O)=O MOTZDAYCYVMXPC-UHFFFAOYSA-N 0.000 description 1
- 229940043264 dodecyl sulfate Drugs 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000000635 electron micrograph Methods 0.000 description 1
- 210000000887 face Anatomy 0.000 description 1
- 235000003599 food sweetener Nutrition 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 description 1
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 description 1
- 229940031957 lauric acid diethanolamide Drugs 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910001629 magnesium chloride Inorganic materials 0.000 description 1
- 229910052943 magnesium sulfate Inorganic materials 0.000 description 1
- 235000019341 magnesium sulphate Nutrition 0.000 description 1
- QQFLQYOOQVLGTQ-UHFFFAOYSA-L magnesium;dihydrogen phosphate Chemical compound [Mg+2].OP(O)([O-])=O.OP(O)([O-])=O QQFLQYOOQVLGTQ-UHFFFAOYSA-L 0.000 description 1
- 229910000401 monomagnesium phosphate Inorganic materials 0.000 description 1
- 235000019785 monomagnesium phosphate Nutrition 0.000 description 1
- SKDZEPBJPGSFHS-UHFFFAOYSA-N n,n-bis(2-hydroxyethyl)tetradecanamide Chemical compound CCCCCCCCCCCCCC(=O)N(CCO)CCO SKDZEPBJPGSFHS-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 150000003016 phosphoric acids Chemical class 0.000 description 1
- 230000002335 preservative effect Effects 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 239000011163 secondary particle Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000010413 sodium alginate Nutrition 0.000 description 1
- 239000000661 sodium alginate Substances 0.000 description 1
- 229940005550 sodium alginate Drugs 0.000 description 1
- KSAVQLQVUXSOCR-UHFFFAOYSA-M sodium lauroyl sarcosinate Chemical compound [Na+].CCCCCCCCCCCC(=O)N(C)CC([O-])=O KSAVQLQVUXSOCR-UHFFFAOYSA-M 0.000 description 1
- AQMNWCRSESPIJM-UHFFFAOYSA-M sodium metaphosphate Chemical compound [Na+].[O-]P(=O)=O AQMNWCRSESPIJM-UHFFFAOYSA-M 0.000 description 1
- 235000019832 sodium triphosphate Nutrition 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- ANOBYBYXJXCGBS-UHFFFAOYSA-L stannous fluoride Chemical compound F[Sn]F ANOBYBYXJXCGBS-UHFFFAOYSA-L 0.000 description 1
- 229960002799 stannous fluoride Drugs 0.000 description 1
- 229940013618 stevioside Drugs 0.000 description 1
- OHHNJQXIOPOJSC-UHFFFAOYSA-N stevioside Natural products CC1(CCCC2(C)C3(C)CCC4(CC3(CCC12C)CC4=C)OC5OC(CO)C(O)C(O)C5OC6OC(CO)C(O)C(O)C6O)C(=O)OC7OC(CO)C(O)C(O)C7O OHHNJQXIOPOJSC-UHFFFAOYSA-N 0.000 description 1
- 235000019202 steviosides Nutrition 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 239000003765 sweetening agent Substances 0.000 description 1
- 239000002562 thickening agent Substances 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
- UNXRWKVEANCORM-UHFFFAOYSA-N triphosphoric acid Chemical compound OP(O)(=O)OP(O)(=O)OP(O)(O)=O UNXRWKVEANCORM-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 239000000230 xanthan gum Substances 0.000 description 1
- 235000010493 xanthan gum Nutrition 0.000 description 1
- 229920001285 xanthan gum Polymers 0.000 description 1
- 229940082509 xanthan gum Drugs 0.000 description 1
Classifications
-
- 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
-
- 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
- A61K8/24—Phosphorous; Compounds thereof
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1409—Abrasive particles per se
Landscapes
- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Veterinary Medicine (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Animal Behavior & Ethology (AREA)
- Oral & Maxillofacial Surgery (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Birds (AREA)
- Epidemiology (AREA)
- Cosmetics (AREA)
Abstract
Description
【発明の詳細な説明】
3、発明の詳細な説明
産業上の利用分野
本発明は、長期間に亘り可溶性フッ素化合物が安定に保
持されると共に、長期保存後も低研磨−高清掃効果が有
効に発揮される口腔用組成物に関する。Detailed Description of the Invention 3. Detailed Description of the Invention Industrial Field of Application The present invention maintains a soluble fluorine compound stably over a long period of time, and also has a low polishing and high cleaning effect even after long-term storage. The present invention relates to an oral composition that exhibits the following properties.
菜」録Uえ4
従来、低研磨−高清掃効果を有する口腔用組成物用の研
磨剤として、X線回折法により測定した結晶子の大きさ
の平均値が300〜3500人である結晶子からなるリ
ン酸水素カルシウム・無水和物が有用であることが知ら
れている(特開昭60−188309号)。4. Conventionally, crystallites having an average crystallite size of 300 to 3500 as measured by X-ray diffraction method have been used as abrasives for oral compositions having low abrasiveness and high cleaning effects. Calcium hydrogen phosphate anhydrate consisting of the following is known to be useful (Japanese Patent Application Laid-open No. 188309/1983).
また従来より、モノフルオロリン酸ナトリウ11等の可
溶性フッ素化合物が歯質を強化し、う蝕予防の有効成分
として使用されることも知られている。It has also been known that soluble fluorine compounds such as sodium monofluorophosphate 11 strengthen tooth structure and are used as active ingredients for caries prevention.
日が しよ゛とする山 占
しかしながら、本発明者らの検討によると、X線回折法
により測定した結晶子の大きさの平均値が200〜35
00人である結晶子からなるリン酸水素カルシウム・無
水和物は、水に対する溶解度が比較的高く、水懸濁系で
カルシウムイオンの溶出が生じる問題があり、またその
結晶子の大きさの平均値が1000Å以下の場合には歯
磨組成物などに配合した場合に経時的に粒子表面が溶解
し、清掃力が経時的に低下して、せっかくの低研磨−高
清掃機能が損なわれる場合もあった。However, according to studies by the present inventors, the average crystallite size measured by X-ray diffraction is 200 to 35.
Calcium hydrogen phosphate anhydrate, which consists of 0.00 crystallites, has a relatively high solubility in water, and has the problem of elution of calcium ions in an aqueous suspension system. If the value is less than 1000 Å, the particle surface will dissolve over time when added to toothpaste compositions, the cleaning power will decrease over time, and the low-polishing and high-cleaning properties may be lost. Ta.
また、このリン酸水素カルシウムをモノフルオロリン酸
ナトリウム等の可溶性フッ素化合物と併用した場合、溶
出したカルシウムイオンの作用で可溶性フッ素化合物を
失活させ易く、可溶性フッ素化合物の安定化配合に問題
を生じさせる場合があった。Furthermore, when this calcium hydrogen phosphate is used in combination with a soluble fluorine compound such as sodium monofluorophosphate, the soluble fluorine compound is likely to be deactivated by the action of the eluted calcium ions, causing problems in the stabilization of the soluble fluorine compound. There were cases where I was forced to do so.
本発明は上記事情に鑑みなされたもので、低研磨−高清
掃効果が長期保存した後でも有効に発揮され、かつ可溶
性フッ素化合物が長期間安定して保持される口腔用組成
物を提供することを目的とする。The present invention was made in view of the above circumstances, and it is an object of the present invention to provide an oral composition that exhibits a low abrasive and high cleaning effect even after long-term storage, and in which a soluble fluorine compound is stably retained for a long period of time. With the goal.
。 古を するための手 び“
本発明者らは、上記目的を達成するため鋭意検討を行な
った結果、X線回折法により測定した結晶子の大きさの
平均値が200〜3500人である結晶子を有するリン
酸水素カルシウム・無水和物を70℃〜1200℃の温
度で焼成することによって得られた研磨剤が、元のリン
酸水素カルシウム・無水和物の性状が損なわれることが
なく、優れた低研磨−高清掃機能を有していると共に、
水に対する溶解度が低く、水懸濁系においても長期間安
定で、経時的に粒子表面が溶解して清掃力が低下するよ
うな不都合がなく、水懸濁系で長期保存した後でも低研
磨−高清掃機能を有効に発揮し、しかも前記リン酸水素
カルシウム・無水和物を350℃以上で焼成したときに
は、得られた研磨剤は非常に高い琢磨効果を与え、歯牙
エナメル質表面に優れた光沢を付与し、またこの研磨基
材を歯磨等に配合した場合に収れん味を改善し、使用感
を向上させることを知見した。. As a result of intensive studies to achieve the above object, the present inventors have developed a crystal with an average crystallite size of 200 to 3,500 crystallites measured by X-ray diffraction method. The abrasive obtained by firing the calcium hydrogen phosphate anhydrate having a carbonaceous substance at a temperature of 70°C to 1200°C does not impair the properties of the original calcium hydrogen phosphate anhydrate. It has excellent low-abrasive and high-cleaning properties, and
It has low solubility in water, is stable for a long time even in an aqueous suspension system, does not have the disadvantage of reducing cleaning power due to dissolution of the particle surface over time, and has low abrasiveness even after long-term storage in an aqueous suspension system. It effectively exhibits a high cleaning function, and when the above-mentioned calcium hydrogen phosphate anhydrate is fired at 350°C or higher, the resulting abrasive has a very high polishing effect and leaves the tooth enamel surface with an excellent gloss. It has been found that when this abrasive base material is blended into toothpaste, etc., the astringent taste is improved and the feeling of use is improved.
そして、この研磨剤はカルシウムイオンの溶出が少なく
、モノフルオロリン酸ナトリウム等の可溶性フッ素化合
物と併用した場合、可溶性フッ素化合物の失活が可及的
に防止され、可溶性フッ素化合物の安定化配合が可能で
あることを見い出した。This abrasive has a low elution of calcium ions, and when used together with a soluble fluorine compound such as sodium monofluorophosphate, the deactivation of the soluble fluorine compound is prevented as much as possible, and the stabilization of the soluble fluorine compound is prevented. I found out that it is possible.
更に、X線回折法により測定した結晶子の大きさの平均
値が200〜3500人である結晶子を有するリン酸水
素カルシウム・無水和物を70℃〜1200℃の温度で
焼成する際、マグネシウム化合物やアルミニウム化合物
を添加すると、得られた研磨剤は水に対する安定性が更
に向上し、フッ素化合物の安定配合がより効果的に達成
されることを知見し、本発明をなすに至ったものである
。Furthermore, when calcining calcium hydrogen phosphate anhydrate having crystallites with an average crystallite size of 200 to 3,500 as measured by X-ray diffraction at a temperature of 70°C to 1200°C, magnesium The inventors discovered that by adding a compound or an aluminum compound, the stability of the resulting abrasive to water is further improved, and a stable combination of fluorine compounds can be achieved more effectively, leading to the creation of the present invention. be.
従って、本発明はX線回折法により測定した結晶子の大
きさの平均値が200〜3500人である結晶子を有す
るリン酸水素カルシウム・無水和物を70℃〜1200
℃の温度で焼成してなる研磨剤と可溶性フッ素化合物と
を併用したことを特徴とする口腔用組成物を提供する。Therefore, the present invention provides calcium hydrogen phosphate anhydrate having an average crystallite size of 200 to 3,500 crystallites measured by X-ray diffraction at a temperature of 70°C to 1,200°C.
Provided is an oral cavity composition characterized in that an abrasive fired at a temperature of 0.degree. C. and a soluble fluorine compound are used in combination.
以下、本発明につき更に詳しく説明する。The present invention will be explained in more detail below.
本発明に用いる研磨剤は、X線回折法により測定した結
晶子の大きさの平均値が200〜3500人である結晶
子を有するリン酸水素カルシウム・無水和物を70℃〜
1200℃の温度で焼成してなるものである。The abrasive used in the present invention is calcium hydrogen phosphate anhydrate having crystallites with an average crystallite size of 200 to 3,500 as measured by X-ray diffraction method.
It is fired at a temperature of 1200°C.
ここで、本発明において使用するリン酸水素カルシウム
・無水和物は平均結晶子の大きさが200〜3500人
のものであるが、特に300〜3000人のものが本発
明研磨剤の清掃力等の点で好適に用いられる。Here, the calcium hydrogen phosphate anhydrate used in the present invention has an average crystallite size of 200 to 3,500 crystallites. It is suitably used in this respect.
また1本発明において用いるリン酸水素カルシウム・無
水和物としては、20”Cにおける密度が2.500〜
2.885g/aI?であり、比表面積がBET法で2
.5〜50rd’/g、特に5〜3゜d7gであり、か
つレーザー光散乱法で測定した平均粒子径が2〜30声
、特に5〜2574111であるものが好ましい。In addition, the calcium hydrogen phosphate anhydrate used in the present invention has a density of 2.500 to 2.500 at 20"C.
2.885g/aI? , and the specific surface area is 2 by the BET method.
.. 5 to 50 rd'/g, particularly 5 to 3 rd'/g, and the average particle diameter measured by laser light scattering method is preferably 2 to 30 tones, particularly 5 to 2574111.
更に、本発明に用いるリン酸水素カルシウム・無水和物
としては、−次粒子の大きさの平均値が0.03〜5I
JIMである板状結晶体が固着集合したものが好ましい
、なお、ここでいう−次粒子の大きさの平均値は電子顕
微鏡写真から測定計算した値である。Furthermore, the calcium hydrogen phosphate anhydrate used in the present invention has an average particle size of 0.03 to 5I.
It is preferable to use JIM, which is a fixed aggregation of plate-like crystals. Note that the average size of the secondary particles referred to herein is a value measured and calculated from electron micrographs.
これらの中では、特に球状のリン酸水素カルシウム・無
水和物が最適である。Among these, spherical calcium hydrogen phosphate anhydrate is particularly suitable.
なお、平均結晶子の大きさが300〜3500人のリン
酸水素カルシウム・無水和物は、通常の方法1例えば米
国特許第2287699号(1942)、同第3012
852号(1961)、同第3066056号(196
2)、同第3169096号(1965)、特公昭39
−3272.3273等に記載されたリン酸と石灰乳と
の中和反応において結晶の生長をコントロールするかま
たは結晶特性及び個々の結晶面の比成長速度に効果を与
えるための媒晶剤を添加することにより製造することが
できる。この場合、媒晶剤としては、例えばリン酸縮合
物及びその塩が好適に使用し得、またその添加はリン酸
と石灰乳との中和反応の間に一行なうことが好ましい。Calcium hydrogen phosphate anhydrate having an average crystallite size of 300 to 3,500 people can be prepared using conventional methods 1, such as U.S. Pat. No. 2,287,699 (1942) and U.S. Pat.
No. 852 (1961), No. 3066056 (196
2), No. 3169096 (1965), Special Publication No. 39
In the neutralization reaction between phosphoric acid and milk of lime described in -3272.3273, etc., a modifier is added to control the growth of crystals or to affect the crystal properties and specific growth rate of individual crystal faces. It can be manufactured by In this case, as the crystal modifier, for example, a phosphoric acid condensate and its salt can be suitably used, and it is preferable that the addition is carried out once during the neutralization reaction between phosphoric acid and milk of lime.
また、媒晶剤の添加量は生成されるリン酸水素カルシウ
ム・無水和物の0.1〜40重量%、特に0.5〜30
重量%とすることが好ましく、その添加量が多くなるほ
ど結晶の生長が阻害され、結晶子が小さくなる傾向を示
す、このリン酸水素カルシウム・無水和物は、その製造
工程において上記媒晶剤の添加量、添加時期、添加速度
、リン酸濃度、反応温度、反応時間、攪拌速度等を適宜
コントロールすることにより、種々のグレードのものを
得ることができる0例えば、電解質を混合したカルシウ
ム化合物とリン酸化合物を50〜90℃の温度で反応さ
せると共にリン酸縮合物を添加することにより、本発明
に用いるリン酸水素カルシウム・無水和物を好適に得る
ことができる。The amount of crystallizing agent added is 0.1 to 40% by weight of the produced calcium hydrogen phosphate anhydrate, especially 0.5 to 30% by weight.
This calcium hydrogen phosphate anhydrate, which is preferably expressed as a percentage by weight, tends to inhibit the growth of crystals and reduce the size of crystallites as the amount added increases. By appropriately controlling the addition amount, addition timing, addition rate, phosphoric acid concentration, reaction temperature, reaction time, stirring speed, etc., various grades can be obtained. For example, calcium compounds mixed with electrolytes and phosphorus Calcium hydrogen phosphate anhydrate used in the present invention can be suitably obtained by reacting acid compounds at a temperature of 50 to 90°C and adding a phosphoric acid condensate.
本発明の研磨剤は、上述した平均結晶子の大きさが20
0〜3500人のリン酸水素カルシウム・無水和物、よ
り好ましくは球状ものを70℃〜1200℃の温度で焼
成したものである。なお、焼成時間は通常1分〜24時
間である。The abrasive of the present invention has an average crystallite size of 20
Calcium hydrogen phosphate anhydrate of 0 to 3500 people, more preferably spherical, is calcined at a temperature of 70°C to 1200°C. Note that the firing time is usually 1 minute to 24 hours.
ここで、焼成温度を70℃〜400℃で焼成時間を1分
〜S時間とした場合、焼成品はリン酸水素カルシウム・
無水和物を主体としたものであり、また焼成温度を40
0℃〜1200℃で焼成時間3分〜24時間とした場合
、焼成品はピロリン酸カルシウムを主体としたものとな
る。この場合。Here, when the firing temperature is 70°C to 400°C and the firing time is 1 minute to S hours, the fired product is made of calcium hydrogen phosphate.
It is mainly composed of anhydrous products, and the firing temperature is 40°C.
When the firing time is 3 minutes to 24 hours at 0° C. to 1200° C., the fired product will be mainly composed of calcium pyrophosphate. in this case.
特には700℃以下で焼成したものを使用することが好
ましく、焼成温度が高いと焼成品の硬度が高くなり、歯
牙を損傷するおそれが生じる。In particular, it is preferable to use a product fired at a temperature of 700° C. or lower; if the firing temperature is high, the hardness of the fired product will increase and there is a risk of damaging the tooth.
なお、その他の焼成条件は特に制限されず、例えば焼成
雰囲気としては空気中でも窒素、アルゴン等の不活性雰
囲気中でもよい。Note that other firing conditions are not particularly limited, and for example, the firing atmosphere may be air or an inert atmosphere such as nitrogen or argon.
また、焼成原料は上述したように平均結晶子の大きさが
200〜3500人のリン酸水素カルシウム・無水和物
であり、これは上述した製造法により得ることができる
が、特に上述した製造法において、酸化カルシウム、水
酸化カルシウム、炭酸カルシウム、塩化カルシウム等の
カルシウム化合物と正すン酸、リン酸アンモニウム、リ
ン酸アルカリ金属塩等のリン酸化合物とをごピロリン酸
。In addition, as mentioned above, the firing raw material is calcium hydrogen phosphate anhydrate with an average crystallite size of 200 to 3,500 people, and this can be obtained by the above-mentioned production method, but especially the above-mentioned production method. In the process, calcium compounds such as calcium oxide, calcium hydroxide, calcium carbonate, and calcium chloride and phosphoric acid compounds such as phosphoric acid, ammonium phosphate, and alkali metal phosphates are combined with pyrophosphoric acid.
トリポリリン酸、テトラポリリン酸、ヘキサポリリン酸
、デカポリリン酸等のポリリン酸、これらポリリン酸と
アルカリ金属、アルカリ土類金属、アルミニウム族との
塩といったリン酸縮合物及びその塩から選ばれる1種又
は2種以上の媒晶剤を前記カルシウム化合物のCa○換
算で0.1〜50重景%重責り好ましくは0.5〜40
重量%、更に好ましくは1〜30重量%添加し、60℃
以上の温度で反応させることにより得られたリン酸水素
カルシウム・無水和物を焼成原料とすることが好ましく
、かかる焼成原料を使用することにより、丸み度のより
高い研磨剤が確実に得られる。One or two selected from polyphosphoric acids such as tripolyphosphoric acid, tetrapolyphosphoric acid, hexapolyphosphoric acid, and decapolyphosphoric acid, phosphoric acid condensates and salts thereof such as salts of these polyphosphoric acids with alkali metals, alkaline earth metals, and aluminum group. The amount of crystallizing modifier at least 0.1% to 50%, preferably 0.5% to 40%, in terms of Ca○ of the calcium compound.
Add % by weight, more preferably 1 to 30% by weight, and heat at 60°C.
It is preferable to use calcium hydrogen phosphate anhydrate obtained by reacting at the above temperature as a firing raw material, and by using such a firing raw material, a polishing slurry with a higher degree of roundness can be reliably obtained.
更に、本発明においては、焼成時にマグネシウム化合物
及び/又はアルミニウム化合物を原料リン酸水素カルシ
ウム・無水和物に添加して焼成することが好ましく、こ
れにより水に対してより安定な研磨剤が得られる。この
場合、マグネシウム化合物としては第1リン酸マグネシ
ウム、第2リン酸マグネシウム、第3リン酸マグネシウ
ム、塩化マグネシウム、硫酸マグネシウム等の1種又は
2種以上が使用できるが、特に第3リン酸マグネシウム
の効果が高く、好適に用いられる。また、アルミニウム
化合物としてはリン酸アルミニウム、ケイ酸アルミニウ
ム等が好適に使用できる。これらマグネシウム化合物、
アルミニウム化合物の使用量は、原料リン酸水素カルシ
ウム・無水和物に対して0〜20重量%、好ましくは0
.5〜1゜重量%である。Furthermore, in the present invention, it is preferable to add a magnesium compound and/or an aluminum compound to the raw material calcium hydrogen phosphate anhydrate during firing, thereby obtaining an abrasive that is more stable against water. . In this case, as the magnesium compound, one or more types of magnesium phosphate monobasic, magnesium phosphate dibasic, magnesium phosphate tertiary, magnesium chloride, magnesium sulfate, etc. can be used, but in particular magnesium phosphate tertiary. It is highly effective and suitable for use. Further, as the aluminum compound, aluminum phosphate, aluminum silicate, etc. can be suitably used. These magnesium compounds,
The amount of aluminum compound used is 0 to 20% by weight, preferably 0% by weight, based on the raw material calcium hydrogen phosphate anhydrate.
.. It is 5 to 1% by weight.
なお、焼成後は、目的に応じて適度な粒子径に解砕する
が、レーザー光散乱法で測定した平均粒子径が2〜30
7Jl、特に5〜25声のものが研磨剤として好ましい
。After firing, it is crushed to an appropriate particle size depending on the purpose, but the average particle size measured by laser light scattering method is 2 to 30.
7Jl, especially those with 5 to 25 tones are preferred as abrasives.
この場合、本発明に用いる研磨剤の平均結晶子の大きさ
、密度、比表面積、丸み度等は、上述したように焼成す
る原料リン酸水素カルシラ11・無水和物の性状に依存
するが、特に本発明に用いる研磨剤としては、吸液量0
.2〜2d/g、比表面積2.5〜50m/gのものが
好ましい。In this case, the average crystallite size, density, specific surface area, roundness, etc. of the abrasive used in the present invention depend on the properties of the raw material Calcilla hydrogen phosphate 11 anhydrate to be fired as described above. In particular, as the abrasive used in the present invention, the liquid absorption amount is 0.
.. Those having a specific surface area of 2 to 2 d/g and a specific surface area of 2.5 to 50 m/g are preferable.
本発明に係る口腔用組成物は、上述した研磨剤に可溶性
フッ素化合物を併用するものである。The oral composition according to the present invention uses a soluble fluorine compound in combination with the above-mentioned abrasive.
ここで、可溶性フッ素化合物としては、モノフルオロリ
ン酸ナトリウム等のモノフルオロリン酸アルカリ金属塩
、フッ化ナトリウム等のアルカリ金属フッ化物、フッ化
第1錫等の第1錫含有フフ化物などが挙げられ、これら
の1種又は2種以上が使用される。Here, examples of the soluble fluorine compound include alkali metal salts of monofluorophosphate such as sodium monofluorophosphate, alkali metal fluorides such as sodium fluoride, and tin-containing fluorides such as stannous fluoride. One or more of these may be used.
なお1本発明の口腔用組成物中における前記研磨剤の配
合量は10〜80%(重量%、以下同じ)。Note that the amount of the abrasive compounded in the oral cavity composition of the present invention is 10 to 80% (weight %, the same applies hereinafter).
特に15〜50%とすることが好ましく、また可溶性フ
ッ素化合物の配合量は0.1〜3%、特に0.45〜2
%とすることが好ましい。In particular, it is preferably 15 to 50%, and the content of the soluble fluorine compound is 0.1 to 3%, particularly 0.45 to 2.
% is preferable.
本発明の口腔用組成物のその他の成分としては、口腔用
組成物の種類等に応じた適宜な成分が使用される6例え
ば、歯磨組成物を調製する場合であれば、粘稠剤、粘結
剤、界面活性剤、香料、甘味剤、防腐剤、各種有効成分
等を配合し得、また必要により本発明研磨剤に加えて他
の研磨剤を配合し得る。As other components of the oral composition of the present invention, appropriate components are used depending on the type of the oral composition.6For example, when preparing a toothpaste composition, a thickening agent, a viscous Binders, surfactants, fragrances, sweeteners, preservatives, various active ingredients, etc. may be blended, and if necessary, other abrasives may be blended in addition to the abrasive of the present invention.
mυ九米
本発明の口腔用組成物は、可溶性フッ素化合物が長期間
安定して保持され、しかも低研磨−高清掃機能が長期間
保存後も発揮されるものである。The oral composition of the present invention maintains a soluble fluorine compound stably for a long period of time, and exhibits low abrasive and high cleaning functions even after long-term storage.
次に、実験例を示し、本発明の効果を具体的に説明する
。Next, experimental examples will be shown to specifically explain the effects of the present invention.
なお、実験例の説明に先立ち、本発明研磨剤の製造に用
いるリン酸水素カルシウム・無水和物及び本発明研磨剤
の製造例を示す。Before explaining the experimental examples, calcium hydrogen phosphate anhydrate used in the production of the abrasive of the present invention and production examples of the abrasive of the present invention will be shown.
〔製造例1〕
石灰乳を100メツシユの篩でふるって粗粒物を除去し
、酸化カルシウム換算で128g/Qの石灰乳を得る。[Production Example 1] Milk of lime is sieved through a 100-mesh sieve to remove coarse particles to obtain milk of lime weighing 128 g/Q in terms of calcium oxide.
次いで、75%のリン酸水溶液IQを78℃に加熱し、
攪拌上毎時570ntQの速度で前記石灰乳を添加する
。中和反応開始60分後にピロリン酸135gを投入し
1石灰乳の添加は引き続き行ない、反応後のpHが6.
0になる時点まで続ける(石灰乳の全添加量は5.3息
。Then, 75% phosphoric acid aqueous solution IQ was heated to 78°C,
The milk of lime is added at a rate of 570 ntQ per hour while stirring. 60 minutes after the start of the neutralization reaction, 135 g of pyrophosphoric acid was added, followed by the addition of milk of lime, and the pH after the reaction was 6.
Continue until it reaches 0 (the total amount of milk of lime added is 5.3 breaths).
Ca0100重量部に対するピロリン酸の添加量は20
.0重量部に相当する)。その後1反応液を一過し、水
で洗浄したのち、P塊を乾燥、粉砕してリン酸水素カル
シウム・無水和物を得る。The amount of pyrophosphoric acid added to 100 parts by weight of Ca0 is 20
.. (equivalent to 0 parts by weight). After that, one reaction solution is passed through and washed with water, and then the P lump is dried and crushed to obtain calcium hydrogen phosphate anhydrate.
〔製造例2〕
製造側例1で得られたリン酸水素カルシウム・無水和物
を450℃で2時間焼成し、本発明研磨剤を得る。[Production Example 2] Calcium hydrogen phosphate anhydrate obtained in Production Example 1 was calcined at 450° C. for 2 hours to obtain a polishing slurry of the present invention.
〔製造例3〕
製造例1で得られたリン酸水素カルシウム・無水和物を
700 ℃で2時間焼成し、本発明研磨剤(球状のピロ
リン酸カルシウム)を得る。[Production Example 3] Calcium hydrogen phosphate anhydrate obtained in Production Example 1 was calcined at 700° C. for 2 hours to obtain an abrasive of the present invention (spherical calcium pyrophosphate).
〔製造例4〕
製造例1で得られたリン酸水素カルシウム・無水和物1
00重量部に第3リン酸マグネシウム1重量部を添加混
合し、180℃で2時間焼成し、本発明研磨剤を得る。[Production Example 4] Calcium hydrogen phosphate anhydrate 1 obtained in Production Example 1
00 parts by weight and 1 part by weight of tertiary magnesium phosphate were added and mixed, and the mixture was fired at 180° C. for 2 hours to obtain a polishing slurry of the present invention.
〔実験例13
下記に示す性状の研磨剤の研磨力(RDA値)及び清掃
力を下記方法により調べた。結果を第1表及び図面に示
す。[Experimental Example 13] The polishing power (RDA value) and cleaning power of abrasives having the properties shown below were investigated by the following method. The results are shown in Table 1 and the drawings.
更肚五嵐
Aニリン酸水素カルシウム・2水和物(DCP−D)平
均凝集粒子径 14IJn
Bニリン酸水素カルシウム・無水和物(D CP−A)
平均結晶子の大きさ 4550人
平均凝集粒子径 16−
密度 2.89g/aJ比表面積
1.2ボ/g
Cニリン酸水素カルシウム・無水和物
(前記製造例1において、ピロリン酸添加量をCaO1
00重量部に対し20重量部とすることによって得られ
たリン酸水素カルシウム・無水和物)
平均結晶子の大きさ 450人
平均凝集粒子径 23戸
密度 2.60g/cd比表面積
23 rd/ gDニリン酸水素カルシウム・無
水和物
(前記製造例1において、ピロリン酸添加量をCaO1
00重量部に対し5重量部とすることによって得られた
リン酸水素カルシウム・無水和物)
平均結晶子の大きさ 700人
平均凝集粒子径 211Jn
密度 2.84g/aj比表面積
9.2ボ/g
E:研磨剤Cを150℃で2時間焼成したもの。Sarazugoran A Calcium hydrogen diphosphate dihydrate (DCP-D) Average aggregate particle size 14IJn B Calcium hydrogen diphosphate anhydrate (D CP-A)
Average crystallite size: 4550 people Average aggregate particle size: 16- Density: 2.89 g/aJ Specific surface area
1.2 bo/g C calcium hydrogen diphosphate anhydrate (in the above Production Example 1, the amount of pyrophosphoric acid added was
Calcium hydrogen phosphate anhydrate obtained by adjusting 20 parts by weight to 00 parts by weight) Average crystallite size 450 people Average agglomerated particle size 23 houses Density 2.60 g/cd Specific surface area
23rd/gD Calcium hydrogen diphosphate anhydrate (in the above Production Example 1, the amount of pyrophosphoric acid added was changed to CaO1
Calcium hydrogen phosphate anhydrate obtained by adding 5 parts by weight to 00 parts by weight) Average crystallite size 700 people Average agglomerated particle diameter 211 Jn Density 2.84 g/aj Specific surface area
9.2 bo/g E: Abrasive C baked at 150°C for 2 hours.
(この研磨剤Eは実質的にリン酸水素カルシウム・無水
和物からなる。)
F:研磨剤りを150℃で2時間焼成したもの。(This abrasive E essentially consists of calcium hydrogen phosphate anhydrate.) F: An abrasive sintered at 150° C. for 2 hours.
(この研磨剤Fは実質的にリン酸水素カルシウム・無水
和物からなる。)
G:研磨剤Cを500℃で2時間焼成したもの。(This polishing agent F essentially consists of calcium hydrogen phosphate anhydrate.) G: Polishing agent C baked at 500° C. for 2 hours.
(この研磨剤Gは実質的にピロリン酸カルシウムからな
る。)
H:研磨剤りを500℃で2時間焼成したもの。(This polishing agent G essentially consists of calcium pyrophosphate.) H: Abrasive agent baked at 500° C. for 2 hours.
(この研磨剤Hは実質的にピロリン酸カルシウムからな
る。)
■=研磨剤0100重量部に第3リン酸マグネシウ・
ム1重量部を添加混合し、150’cで2時間焼成した
もの。(This abrasive H essentially consists of calcium pyrophosphate.) ■=Abrasive 0 100 parts by weight and magnesium phosphate tertiary.
1 part by weight was added and mixed and baked at 150'c for 2 hours.
J:研磨剤0100重量部に第3リン酸マグネシウム1
重量部を添加混合し、500”Cで2時間焼成したもの
。J: 100 parts by weight of polishing agent and 1 part by weight of tertiary magnesium phosphate
Parts by weight were added and mixed and fired at 500"C for 2 hours.
K:研磨剤C100重量部にリン酸アルミニウム1重量
部を添加混合し、150℃で2時間焼成したもの。K: 100 parts by weight of abrasive C was mixed with 1 part by weight of aluminum phosphate and fired at 150°C for 2 hours.
L:研磨剤C100重量部にリン酸アルミニウム1重量
部を添加混合し、500℃で2時間焼成したもの。L: 100 parts by weight of abrasive C was mixed with 1 part by weight of aluminum phosphate and fired at 500°C for 2 hours.
M:ピロリン酸カルシウム(従来品)
なお、上述した性状のうち、平均結晶子の大きさの測定
は、粉体のX線回折を行ない、ピークのブロードニング
から粉体の結晶性を結晶子の大きさを指標として定量的
に表わした。ここで。M: Calcium pyrophosphate (conventional product) Among the above properties, the average crystallite size is measured by performing X-ray diffraction of the powder, and determining the crystallinity of the powder from the peak broadening. It was expressed quantitatively using the index as an index. here.
X線源はCu−にα線を用いて測定し、X線回折のデー
タをS cherrerの式D=にλ/βCO5θを用
いて重なりのない主なピークについて解析し、平均結晶
子の大きさを求めた。この場合、主なピークとしては2
θ=53.1’ 、36.1” 。The X-ray source was measured using alpha rays for Cu-, and the X-ray diffraction data was analyzed for non-overlapping main peaks using Scherrer's equation D = λ/βCO5θ, and the average crystallite size was determined. I asked for In this case, the main peaks are 2
θ=53.1', 36.1".
32.6’ 、30.25’ 、13.15’について
平均をとった。ここでDは結晶子の大きさ〔人〕。The average was taken for 32.6', 30.25', and 13.15'. Here, D is the size of the crystallite [person].
λは測定X線波長〔人〕、βは純粋に結晶子の大きさに
基づく回折線の広がり(r a d)(α−AI2.○
。λ is the measured X-ray wavelength [human], β is the spread of the diffraction line (ra d) purely based on the size of the crystallite (α-AI2.○
.
粉体を1100℃で24時間焼成したものを基準として
用いた)、には形状因子(定数=0.9とした)、θは
回折線のブラッグ角とした。また、βは実験的に求めた
半価幅から同じ条件下における結晶性の非常に良い物質
によって与えられる半価幅を差し引いた値である。A powder obtained by firing the powder at 1100° C. for 24 hours was used as a reference), where was the shape factor (constant = 0.9), and θ was the Bragg angle of the diffraction line. Further, β is the value obtained by subtracting the half-value width given by a material with very good crystallinity under the same conditions from the experimentally determined half-value width.
また、平均凝集粒子径はL eed F!t N or
thrup社の粒度分布測定装置(商品名Microt
rac)により測定した(レーザー法)。In addition, the average aggregate particle size is L eed F! t N or
Thrup's particle size distribution analyzer (product name: Microt)
rac) (laser method).
旦腹ユ皿定遣
J 、Dent、Res、Vol、55.No、4.
563〜573 by Hefferenに記載されて
いる方法によりRD A (Radioactive
Dentin Abrasion)値を測定した。Danpuku Yusara Teikyou J, Dent, Res, Vol, 55. No, 4.
563-573 by Hefferen.
Dentin abrasion) values were measured.
清掃力測定法
理草ヤニを通常の方法にて収集し、これを溶液状として
タイル上に均一に塗布し、加温乾燥したのち、これを研
磨容器にセットし、研磨剤5gを0.3%カルボキシメ
チルセルロースナトリウムを含む60%グリセリン水溶
液15gに懸濁してなるサスペンションを用い、荷重2
00gにおいて2000回ブラッシングし、研磨後タイ
ルの煙草ヤニの除去率を肉眼にて評価した。Method for Measuring Cleaning Power Grass tar was collected in the usual manner, applied as a solution evenly on the tiles, heated and dried, set in a polishing container, and mixed with 5g of polishing agent at 0.3%. Using a suspension suspended in 15 g of a 60% glycerin aqueous solution containing sodium carboxymethyl cellulose, a load of 2 was applied.
The tiles were brushed 2000 times at 00 g, and the removal rate of tobacco tar from the tiles was visually evaluated after polishing.
なお、ブラッシングのブラシとしては1毛東数44個、
毛の太さ8ミル(約0.2mm)、毛の長さ12m+a
のナイロン(62)材質で、材質の硬さが家庭用品品質
表示法でMのものを使用した。In addition, as a brushing brush, there are 44 hairs per hair,
Hair thickness: 8 mil (approximately 0.2 mm), hair length: 12 m+a
The material used was nylon (62) with a hardness of M according to the Household Goods Quality Indication Law.
評価基準
評点1:煙草ヤニ除去率 0〜10%2:
11 11〜20%3: 2
1〜30%
4: 31〜40%
5: 41〜50%
6: 51〜60%
7: 61〜70%
8: 71〜80%
9: 81〜90%
10: II 91〜100%第
1 表
嘲混合比 1量地
第1表及び図面の結果より、本発明に係る研磨剤は低研
磨−高清掃効果を有することが認められる。Evaluation Criteria Score 1: Cigarette tar removal rate 0-10% 2:
11 11~20%3: 2
1-30% 4: 31-40% 5: 41-50% 6: 51-60% 7: 61-70% 8: 71-80% 9: 81-90% 10: II 91-100%
From the results shown in Table 1 and the drawings, it is recognized that the abrasive according to the present invention has a low polishing and high cleaning effect.
〔実験例2〕
上述した研磨剤B、C,G、M並びに下記Nの歯牙エナ
メル質光沢向上効果を下記方法により評価した。結果を
第2表に示す。[Experimental Example 2] The tooth enamel gloss improvement effects of the above-mentioned abrasives B, C, G, M and the following N were evaluated by the following method. The results are shown in Table 2.
皿讃盪IN 研磨剤Cを900℃で2時間焼成したもの。Praise IN Abrasive C was fired at 900°C for 2 hours.
(この研磨剤Nは実質的にピロリン酸カルシウムからな
る。)
平均凝集粒子径 25IJ!B
密度 3.09g/aJ比表面積
20rX?/g
又仮血上皮
5X5mmの大きさにカットした生歯を樹脂に包埋し、
生歯エナメル表面を回転研磨機で平滑にし、次いで、N
o、1200のエメリー紙研磨、パフ研磨により光沢計
(日本重色工業社(GLO5SMETERVG−10)
)(7)光沢度1’80.0±2.0にエナメル表面を
処理した。(This abrasive N essentially consists of calcium pyrophosphate.) Average aggregate particle size 25IJ! B Density 3.09g/aJ specific surface area
20rX? /g In addition, a raw tooth cut into a size of 5 x 5 mm was embedded in resin.
The tooth enamel surface was smoothed with a rotary polisher, and then N
Gloss meter (Nippon Heavy Industries Co., Ltd. (GLO5SMETERVG-10)
) (7) The enamel surface was treated to a gloss level of 1'80.0±2.0.
次に、研磨剤5gを60%グリセリン水溶液15IIQ
に懸濁してなるサスペンションを上記生歯テストピース
をセットした研磨容器に注入し、水平型研磨試験機によ
り荷重200g、7000ストロ一ク/40分の条件で
ブラッシングした。ブラッシングのブラシとしては実験
例1と同じものを使用した。7000ストロークのブラ
ッシング後、前記光沢計により光沢度の増減を測定し、
初期光沢度からの差を光沢向上度とし、下記評価基準に
基いて評価した。Next, add 5 g of abrasive to 60% glycerin aqueous solution 15IIQ.
The suspension prepared by suspending the test piece was poured into a polishing container set with the above-mentioned natural tooth test piece, and brushed using a horizontal polishing tester under the conditions of a load of 200 g and 7000 strokes/40 minutes. The same brush as in Experimental Example 1 was used for brushing. After 7,000 strokes of brushing, the gloss meter measures the increase or decrease in gloss,
The difference from the initial glossiness was defined as the degree of gloss improvement, and evaluation was made based on the following evaluation criteria.
O:光沢向上度+20以上
0: rJ +15以上+20未満x:
tt +ts未満
この場合、目視で十分に光沢があると認められるレベル
は+20以上、光沢があると認められるレベルは+15
以上である。O: Gloss improvement degree +20 or more 0: rJ +15 or more + less than +20 x:
tt Less than +ts In this case, the level that is visually recognized as sufficiently glossy is +20 or higher, and the level that is recognized as glossy is +15.
That's all.
第 2 表
第2表の結果より、本発明に係る研磨剤は光沢向上効果
が優れていることが認められる。Table 2 From the results shown in Table 2, it is recognized that the polishing agent according to the present invention has an excellent gloss improvement effect.
〔実験例3〕
第3表に示す研磨剤5gを水50mNにS濁し、これを
20℃の恒温槽中に3日間放置した後、No、5Cの7
紙で一過し、P液中のカルシウムイオン量を原子吸光分
析法によって測定することにより、各研磨基剤からのカ
ルシウムイオン溶出量を評価した。[Experimental Example 3] 5 g of the abrasive shown in Table 3 was suspended in 50 mN of water and left in a constant temperature bath at 20°C for 3 days.
The amount of calcium ions eluted from each polishing base was evaluated by passing it through paper and measuring the amount of calcium ions in the P solution by atomic absorption spectrometry.
結果を第3表に示す。The results are shown in Table 3.
第 3 表
第3表の結果より、本発明に係る研磨剤は水懸濁系にお
いてCa”“の溶出量が少ないことが認められる。Table 3 From the results shown in Table 3, it is recognized that the abrasive according to the present invention has a small amount of Ca"" eluted in an aqueous suspension system.
〔実験例4〕
下記に示す研磨剤を使用した下記処方の練歯磨を調衷し
、これを40℃で所定期間保存した後の清掃力を下記方
法によって調べ、清掃効果の経時安定性を評価した。結
果を第4表に示す。[Experimental Example 4] A toothpaste with the following formulation using the abrasive shown below was prepared, and after storing it at 40°C for a specified period, the cleaning power was examined using the following method, and the stability of the cleaning effect over time was evaluated. did. The results are shown in Table 4.
豊豊皇蓋方
研磨剤 30.0
%無定形研磨性シリカ 5.0
カルボキシメチルセルロースナトリウム 1.0コ
ロイド状シリカ 1.5プ
ロピレングリコール 2.0グリ
セリン 18・0ラウリル
硫酸ナトリウム 1.5サツカリン
ナトリウム 0.1゜香料
1.0
防腐剤 微 量モ
ノフルオロリン酸ナトリウム o、741
00.0%
班匿剋
Oニリン酸水素カルシウム・無水和物
(前記製造例1において、ピロリン酸添加量をCaO1
00重量部に対し10ffl!部とすることによって得
られたリン酸水素カルシウム・無水和物)
平均結晶子の大きさ 540人
平均凝集粒子径 25μs
密度 2.70g/ci比表面積
18ボ/gP:研磨剤0を150℃
で2時間焼成したもの。Hoho-no-Katata Abrasive 30.0
%Amorphous abrasive silica 5.0
Sodium carboxymethylcellulose 1.0 Colloidal silica 1.5 Propylene glycol 2.0 Glycerin 18.0 Sodium lauryl sulfate 1.5 Sodium saccharin 0.1°Fragrance
1.0 Preservative Trace amount of sodium monofluorophosphate o, 741
00.0% Calcium hydrogen diphosphate anhydrate (In the above Production Example 1, the amount of pyrophosphoric acid added was
10ffl for 00 parts by weight! Calcium hydrogen phosphate (anhydrate) obtained by dividing the sample into 100% of the average crystallite size: 540 people Average agglomerated particle size: 25 μs Density: 2.70 g/ci Specific surface area: 18 bo/gP: Abrasive 0 at 150°C
Baked for 2 hours.
(この研磨剤0は実質的にリン酸水素カルシウム・無水
和物からなる。)
Q:研磨剤0を500℃で2時間焼成したもの。(This abrasive 0 essentially consists of calcium hydrogen phosphate anhydrate.) Q: Abrasive 0 is baked at 500°C for 2 hours.
(この研磨剤Qは実質的にピロリン酸カルシウムからな
る。)
R:新溶剤0100重量部に第3リン酸マグネシウム1
重量部を添加混合し、500℃で2時間焼成したもの。(This polishing agent Q essentially consists of calcium pyrophosphate.) R: 100 parts by weight of new solvent to 1 part by weight of tertiary magnesium phosphate
Parts by weight were added and mixed and baked at 500°C for 2 hours.
S:研磨剤0100重足部にリン酸アルミニウム1重示
部を添加混合し、500℃で2時間焼成したもの。S: One part of aluminum phosphate was added to and mixed with one part of abrasive 0100, and the mixture was fired at 500°C for 2 hours.
逍1JjLξ囚
サスペンションとして歯磨Logを60%グリセリン水
溶液に懸濁分散させたものを用いた以外は実験例1と同
様である。The procedure was the same as in Experimental Example 1 except that a suspension of toothpaste Log in a 60% glycerin aqueous solution was used as the suspension.
第 4 表
第4表の結果より、本発明に係る研磨剤は水懸濁系にお
いて経時安定性が良好であることが認められる。Table 4 From the results shown in Table 4, it is recognized that the abrasive according to the present invention has good stability over time in an aqueous suspension system.
〔実験例5〕
第5表に示す研磨剤5gを水50mQに懸濁し、これに
モノフルオロリン酸ナトリウムをフッ素として1100
0ppを添加した後、これを50℃の恒温槽中に7日間
振盪放置した0次いで、その上澄液中の水溶性フッ素量
をフッ素電極で測定した。その結果を第5表に示す。[Experimental Example 5] 5 g of the abrasive shown in Table 5 was suspended in 50 mQ of water, and sodium monofluorophosphate was added as fluorine to 1100 mQ of water.
After adding 0pp, this was left to shake for 7 days in a constant temperature bath at 50°C.Then, the amount of water-soluble fluorine in the supernatant was measured using a fluorine electrode. The results are shown in Table 5.
第 5 表
〔実験例6〕
下記の研磨剤を使用し、実験例5と同様にして水溶性フ
ッ素量を調べた。結果を第6表に示す。Table 5 [Experimental Example 6] The amount of water-soluble fluorine was investigated in the same manner as in Experimental Example 5 using the following abrasives. The results are shown in Table 6.
研磨剤Tニリン酸水素カルシウム・無水和物前記製造例
1において、ピロリン酸添加量をCaO100重量部に
対し2重量部とすることによって得られたリン酸水素カ
ルシウム・無水和物
平均結晶子の大きさ 2200人平均凝集粒子径
16.5μs密度
2.86g/aI!比表面積 2.0
イ/g研m剤U:
研磨剤Tを150℃で2時間焼成したもの。Abrasive T Calcium hydrogen phosphate anhydrate In the above Production Example 1, the average crystallite size of calcium hydrogen phosphate anhydrate obtained by adding pyrophosphoric acid to 2 parts by weight per 100 parts by weight of CaO 2200 people average aggregate particle size 16.5μs density
2.86g/aI! Specific surface area 2.0
A/g Abrasive U: Abrasive T baked at 150°C for 2 hours.
(この研磨剤Uは実質的にリン酸水素カルシウム・無水
和物からなる。)
研磨剤V:
研磨剤Tを500℃で2時間焼成したもの。(This abrasive U essentially consists of calcium hydrogen phosphate anhydrate.) Abrasive V: Abrasive T baked at 500° C. for 2 hours.
(この研磨剤Vは実質的にピロリン酸カルシウムからな
る。)
第 6 表
第5,6表の結果より、本発明に係る研磨剤はフッ素化
合物の安定化配合を可能にすることが認められる。(This abrasive V essentially consists of calcium pyrophosphate.) Table 6 From the results shown in Tables 5 and 6, it is recognized that the abrasive according to the present invention enables the stabilization of a fluorine compound.
以下、本発明の実施例を示す。Examples of the present invention will be shown below.
〔実施例1〕 練 歯 磨
本発明研磨剤 5o%無水
ケイa 1.5カル
ボキシメチルセルロースナトリウム 1.0力ラゲ
ナン 。、2ソルビツ
ト 18プロピレングリ
コール 2ラウリル硫酸ナトリウ
ム 1.5サッカリンナトリウム
0.2トラネキサム酸
0.2モノフルオロリン酸ナトリ
ウム 0.76ピロリン酸ナトリウム
1.0香料 1
.0
100、0%
〔実施例2〕 練 歯 磨
本発明研磨剤 30%ピロ
リン酸カルシウム 10無水ケイ
酸 2・Oカルボキ
シメチルセルロースナトリウム 0.8アルギン酸
ナトリウム 0.4ソルビツト
30グリセリン
10プロピレングリコール
3ラウリル硫酸ナトリウム
1.5POE(20)硬化ヒマシ油
1.0サツカリンナトリウム
0.1デキストラナーゼ
0.2モノフルオロリン酸ナトリウム
0.76ピロリン酸ナトリウム
1.5香料 1.5
100.0%
〔実施例3〕 練 歯 磨
本発明研磨剤 20%凝集
無水リン酸カルシウム 30無水ケイ酸
2・0キサンタン
ガム 0.5ゼラチン
0・5ソルビツト
20グリセリン
5ポリエチレングリコール
4ラウリル硫酸ナトリウム
1.0ミリスチン酸ジエタノールアミド
0.3サツカリンナトリウム
0.1トラネキサム酸
0・2塩酸クロルヘキシジン
0.01モノフルオロリン酸ナトリウム
0.76ヘキサメタリン酸
2.0香料 0.8
精製水 残100
.0%
〔実施例4〕 練 歯 磨
本発明研磨剤 30%リン
酸水素カルシウム・無水和物 20カルボキシ
メチルセルロースナトリウム 0.9力ラゲナン
0.3ソルビツト
2゜ポリエチレングリコ
ール 3ラウリル硫酸ナトリウム
1.2サツカリンナトリウム
0.1ステビオサイド
0.1トラネキサム酸
0.05モノフルオロリン酸ナトリウム
0.76ピロリン酸ナトリウム
1゜5香料 1・0
100、0%
〔実施例5〕 練 歯 磨
本発明研磨剤 30%リン
酸水素カルシウム・2水和物 2゜カルボキシ
メチルセルロースナトリウム 1.2ソルビツト
15グリセリン
10プロピレングリコール
3ラウリル硫酸ナトリウム
1.0ラウリン酸ジエタノールアミド
0.5サツカリンナトリウム
0.1モノフルオロリン酸ナトリウム
0.76第3リン酸マグネシウム
1.0香料 1.0
100、0%
〔実施例6〕 練 歯 磨
本発明研磨剤 20%水酸
化アルミニウム 10無水ケイ酸
30カルボキシメチル
セルロースナトリウム 0.8ヒドロキシエチルセ
ルロース 0.3グリセリン
25ポリエチレングリコール
3ラウリル硫酸ナトリウム
1.0ラウロイルサルコシンナトリウム
0.3サツカリンナトi功ム
0.2モノフルオロリン酸ナトリウム
。、76メタリン酸ナトリウム
0.5香料 0.5
100.0%
〔実施例7〕 練 歯 磨
本発明研磨剤 30%炭酸
カルシウム 1゜無水ケイ
酸 2゜カルボキシメチ
ルセルロースナトリウム 1.0ゼラチン
0.3ソルビツト
1゜グリセリン
10゜ポリエチレングリコール
3ラウリル硫酸ナトリウム
1.5サツカリンナトリウム
0.2トラネキサム酸
0.05モノフルオロリン酸ナトリウム
0.76ピロリン酸ナトリウム
0.3メタリン酸ナトリウム
0.5香料 1.0
〔実施例8〕 練 歯 磨
本発明研磨剤 30%不溶
性メタリン酸ナトリウム 20カルボキシ
メチルセルロースナトリウム 1.0力ラゲナン
0・1ソルビツト
10グリセリン
15ポリエチレングリコール
3アルコール
ラウリル硫酸ナトリウム 1.2サ
ツカリンナトリウム 0.1ト
ラネキサム酸 0.1モ
ノフルオロリン酸ナトリウム 0.56フ
ツ化ナトリウム 0.2トリ
ポリリン酸ナトリウム 。、2香料
0.5
精製水 残10
0、0%
〔実施例9〕 潤製歯磨
本発明研磨剤 80%グリ
セリン 1。[Example 1] Toothpaste Invention Abrasive: 50% anhydrous silicon, 1.5 sodium carboxymethyl cellulose, 1.0 lagenane. , 2 sorbitol 18 propylene glycol 2 sodium lauryl sulfate 1.5 sodium saccharin
0.2 tranexamic acid
0.2 Sodium monofluorophosphate 0.76 Sodium pyrophosphate
1.0 fragrance 1
.. 0 100, 0% [Example 2] Toothpaste Invention Abrasive 30% Calcium pyrophosphate 10 Silicic anhydride 2.O Sodium carboxymethylcellulose 0.8 Sodium alginate 0.4 Sorbit 30 Glycerin
10 propylene glycol
3 Sodium lauryl sulfate
1.5POE (20) hydrogenated castor oil
1.0 Satucalin Sodium
0.1 dextranase
0.2 Sodium monofluorophosphate
0.76 Sodium pyrophosphate
1.5 Fragrance 1.5 100.0% [Example 3] Toothpaste Invention Abrasive 20% Agglomerated Anhydrous Calcium Phosphate 30 Silicic Anhydride 2.0 Xanthan Gum 0.5 Gelatin
0.5 sorbit
20 glycerin
5 polyethylene glycol
4 Sodium lauryl sulfate
1.0 myristic acid diethanolamide
0.3 Satucalin Sodium
0.1 tranexamic acid
Chlorhexidine 0.2 hydrochloride
0.01 Sodium monofluorophosphate
0.76 hexametaphosphoric acid
2.0 fragrance 0.8 purified water remaining 100
.. 0% [Example 4] Toothpaste Invention abrasive 30% Calcium hydrogen phosphate anhydrate 20 Sodium carboxymethylcellulose 0.9 Lagenan
0.3 sorbit
2゜Polyethylene glycol 3Sodium lauryl sulfate
1.2 Satucalin Sodium
0.1 Stevioside
0.1 tranexamic acid
0.05 Sodium monofluorophosphate 0.76 Sodium pyrophosphate
1゜5 Fragrance 1.0 100.0% [Example 5] Toothpaste Abrasive of the present invention 30% Calcium hydrogen phosphate dihydrate 2゜Sodium carboxymethyl cellulose 1.2 Sorbit
15 Glycerin
10 propylene glycol
3 Sodium lauryl sulfate
1.0 Lauric acid diethanolamide
0.5 Satucalin Sodium
0.1 Sodium monofluorophosphate
0.76 tertiary magnesium phosphate
1.0 Fragrance 1.0 100, 0% [Example 6] Toothpaste Invention Abrasive 20% Aluminum hydroxide 10 Silicic anhydride 30 Sodium carboxymethyl cellulose 0.8 Hydroxyethyl cellulose 0.3 Glycerin
25 polyethylene glycol
3 Sodium lauryl sulfate
1.0 Sodium lauroyl sarcosine
0.3 Satsukarinnato i merit
0.2 Sodium monofluorophosphate
. , 76 sodium metaphosphate
0.5 Fragrance 0.5 100.0% [Example 7] Toothpaste Invention Abrasive 30% Calcium Carbonate 1° Silicic Anhydride 2° Sodium Carboxymethyl Cellulose 1.0 Gelatin
0.3 sorbit
1゜glycerin
10゜Polyethylene glycol
3 Sodium lauryl sulfate
1.5 Satucalin Sodium
0.2 tranexamic acid
0.05 Sodium monofluorophosphate
0.76 Sodium pyrophosphate
0.3 Sodium metaphosphate
0.5 Fragrance 1.0 [Example 8] Toothpaste Invention Abrasive 30% Insoluble Sodium Metaphosphate 20 Sodium Carboxymethyl Cellulose 1.0 Lagenan
0.1 sorbitol
10 glycerin
15 polyethylene glycol
3 Alcohol Sodium Lauryl Sulfate 1.2 Sodium Saccharin 0.1 Tranexamic Acid 0.1 Sodium Monofluorophosphate 0.56 Sodium Fluoride 0.2 Sodium Tripolyphosphate. , 2 fragrance 0.5 purified water remaining 10
0.0% [Example 9] Junsei Toothpaste Invention Abrasive 80% Glycerin 1.
ラウリン酸ジェタノールアミド 0.1サ
ツカリンナトリウム 0.1モ
ノフルオロリン酸ナトリウム 。、76第
3リン酸マグネシウム 0.5香料
1.0
M製水 残10
0、0%Lauric acid jetanolamide 0.1 Sodium saccharin 0.1 Sodium monofluorophosphate. , 76 tertiary magnesium phosphate 0.5 fragrance 1.0 M water remaining 10
0,0%
図面は種々の研磨剤の研磨力と清掃力との関係を示すグ
ラフである。The drawing is a graph showing the relationship between the polishing power and cleaning power of various abrasives.
Claims (1)
が200〜3500Åである結晶子を有するリン酸水素
カルシウム・無水和物を70℃〜1200℃の温度で焼
成してなる研磨剤と可溶性フッ素化合物とを併用したこ
とを特徴とする口腔用組成物。 2、リン酸水素カルシウム・無水和物の密度が2.50
0〜2.885g/cm^3であり、比表面積がBET
法で2.5〜50m^2/gであり、かつ平均粒子径が
2〜30μmである特許請求の範囲第1項記載の口腔用
組成物。 3、研磨剤がリン酸水素カルシウム・無水和物にマグネ
シウム化合物及び/又はアルミニウム化合物を添加して
焼成することにより得られたものである特許請求の範囲
第1項又は第2項記載の口腔用組成物。 4、可溶性フッ素化合物がモノフルオロリン酸アルカリ
金属塩である特許請求の範囲第1項乃至第3項のいずれ
か1項に記載の口腔用組成物。[Claims] 1. Calcium hydrogen phosphate anhydrate having crystallites with an average crystallite size of 200 to 3500 Å measured by X-ray diffraction at a temperature of 70°C to 1200°C. An oral cavity composition characterized by using a fired abrasive and a soluble fluorine compound in combination. 2. Density of calcium hydrogen phosphate anhydrate is 2.50
0 to 2.885g/cm^3, and the specific surface area is BET
2. The oral cavity composition according to claim 1, which has an average particle diameter of 2.5 to 50 m^2/g and an average particle diameter of 2 to 30 μm. 3. The oral cavity according to claim 1 or 2, wherein the abrasive is obtained by adding a magnesium compound and/or an aluminum compound to calcium hydrogen phosphate anhydrate and firing the mixture. Composition. 4. The oral composition according to any one of claims 1 to 3, wherein the soluble fluorine compound is an alkali metal monofluorophosphate.
Priority Applications (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP13117786A JPS62286916A (en) | 1986-06-06 | 1986-06-06 | Composition for oral cavity |
ES8701846A ES2004429A6 (en) | 1986-06-06 | 1987-06-05 | Abrasive and compositions containing it |
FR8707957A FR2599749A1 (en) | 1986-06-06 | 1987-06-05 | Abrasive and compositions containing it |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP13117786A JPS62286916A (en) | 1986-06-06 | 1986-06-06 | Composition for oral cavity |
Publications (1)
Publication Number | Publication Date |
---|---|
JPS62286916A true JPS62286916A (en) | 1987-12-12 |
Family
ID=15051806
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP13117786A Pending JPS62286916A (en) | 1986-06-06 | 1986-06-06 | Composition for oral cavity |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPS62286916A (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2018104376A (en) * | 2016-12-27 | 2018-07-05 | サンスター株式会社 | Dentifrice composition |
-
1986
- 1986-06-06 JP JP13117786A patent/JPS62286916A/en active Pending
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2018104376A (en) * | 2016-12-27 | 2018-07-05 | サンスター株式会社 | Dentifrice composition |
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