CN114931540A - Carboxymethylated bagasse-containing composite material and preparation method and application thereof - Google Patents
Carboxymethylated bagasse-containing composite material and preparation method and application thereof Download PDFInfo
- Publication number
- CN114931540A CN114931540A CN202210631430.8A CN202210631430A CN114931540A CN 114931540 A CN114931540 A CN 114931540A CN 202210631430 A CN202210631430 A CN 202210631430A CN 114931540 A CN114931540 A CN 114931540A
- Authority
- CN
- China
- Prior art keywords
- bagasse
- composite material
- carboxymethylated
- toothpaste
- phosphate
- 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.)
- Granted
Links
- 241000609240 Ambelania acida Species 0.000 title claims abstract description 109
- 239000010905 bagasse Substances 0.000 title claims abstract description 109
- 239000002131 composite material Substances 0.000 title claims abstract description 66
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 239000000606 toothpaste Substances 0.000 claims abstract description 94
- 229940034610 toothpaste Drugs 0.000 claims abstract description 89
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 87
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 41
- 239000001506 calcium phosphate Substances 0.000 claims abstract description 28
- 229910000389 calcium phosphate Inorganic materials 0.000 claims abstract description 16
- 235000011010 calcium phosphates Nutrition 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 14
- FDRCDNZGSXJAFP-UHFFFAOYSA-M sodium chloroacetate Chemical compound [Na+].[O-]C(=O)CCl FDRCDNZGSXJAFP-UHFFFAOYSA-M 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- 238000000227 grinding Methods 0.000 claims abstract description 10
- 239000007864 aqueous solution Substances 0.000 claims abstract description 9
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 claims abstract description 6
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims abstract description 6
- 229940090898 Desensitizer Drugs 0.000 claims abstract description 6
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims abstract description 6
- 229910001424 calcium ion Inorganic materials 0.000 claims abstract description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims abstract description 6
- 229940085991 phosphate ion Drugs 0.000 claims abstract description 5
- -1 phosphate calcium salt Chemical class 0.000 claims abstract description 4
- 239000000920 calcium hydroxide Substances 0.000 claims abstract description 3
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims abstract description 3
- 238000000926 separation method Methods 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 27
- 239000002245 particle Substances 0.000 claims description 17
- 239000000843 powder Substances 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 11
- 239000000243 solution Substances 0.000 claims description 10
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 8
- 239000004088 foaming agent Substances 0.000 claims description 7
- 235000003599 food sweetener Nutrition 0.000 claims description 7
- 239000003755 preservative agent Substances 0.000 claims description 7
- 230000002335 preservative effect Effects 0.000 claims description 7
- 239000003765 sweetening agent Substances 0.000 claims description 7
- 239000003906 humectant Substances 0.000 claims description 6
- 238000002386 leaching Methods 0.000 claims description 6
- 240000000111 Saccharum officinarum Species 0.000 claims description 5
- 235000007201 Saccharum officinarum Nutrition 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 4
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 claims description 4
- 238000000498 ball milling Methods 0.000 claims description 3
- 238000010902 jet-milling Methods 0.000 claims description 3
- 229910000402 monopotassium phosphate Inorganic materials 0.000 claims description 3
- 235000019796 monopotassium phosphate Nutrition 0.000 claims description 3
- 239000001488 sodium phosphate Substances 0.000 claims description 3
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 3
- 229910000406 trisodium phosphate Inorganic materials 0.000 claims description 3
- 235000019801 trisodium phosphate Nutrition 0.000 claims description 3
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 claims description 2
- 239000011230 binding agent Substances 0.000 claims description 2
- 239000001569 carbon dioxide Substances 0.000 claims description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 2
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims description 2
- 229910000388 diammonium phosphate Inorganic materials 0.000 claims description 2
- 235000019838 diammonium phosphate Nutrition 0.000 claims description 2
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 claims description 2
- ZPWVASYFFYYZEW-UHFFFAOYSA-L dipotassium hydrogen phosphate Chemical compound [K+].[K+].OP([O-])([O-])=O ZPWVASYFFYYZEW-UHFFFAOYSA-L 0.000 claims description 2
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 claims description 2
- 239000004615 ingredient Substances 0.000 claims description 2
- 229910000403 monosodium phosphate Inorganic materials 0.000 claims description 2
- 235000019799 monosodium phosphate Nutrition 0.000 claims description 2
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 claims description 2
- 238000012216 screening Methods 0.000 claims description 2
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 claims description 2
- 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 abstract description 29
- 229910010272 inorganic material Inorganic materials 0.000 abstract description 5
- 239000011147 inorganic material Substances 0.000 abstract description 5
- 229910017053 inorganic salt Inorganic materials 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 41
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 30
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 26
- 238000002474 experimental method Methods 0.000 description 21
- 238000003756 stirring Methods 0.000 description 18
- 229920005610 lignin Polymers 0.000 description 14
- 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 13
- 239000001768 carboxy methyl cellulose Substances 0.000 description 13
- 239000000377 silicon dioxide Substances 0.000 description 13
- 239000000600 sorbitol Substances 0.000 description 13
- 235000010356 sorbitol Nutrition 0.000 description 13
- 238000012360 testing method Methods 0.000 description 13
- YYRMJZQKEFZXMX-UHFFFAOYSA-L calcium bis(dihydrogenphosphate) Chemical compound [Ca+2].OP(O)([O-])=O.OP(O)([O-])=O YYRMJZQKEFZXMX-UHFFFAOYSA-L 0.000 description 12
- 239000000686 essence Substances 0.000 description 12
- 235000019691 monocalcium phosphate Nutrition 0.000 description 12
- 235000012239 silicon dioxide Nutrition 0.000 description 12
- 229960001714 calcium phosphate Drugs 0.000 description 11
- 239000000679 carrageenan Substances 0.000 description 11
- 235000010418 carrageenan Nutrition 0.000 description 11
- 229920001525 carrageenan Polymers 0.000 description 11
- 229940113118 carrageenan Drugs 0.000 description 11
- 238000004140 cleaning Methods 0.000 description 11
- 235000011187 glycerol Nutrition 0.000 description 11
- 229910000150 monocalcium phosphate Inorganic materials 0.000 description 11
- 239000000230 xanthan gum Substances 0.000 description 11
- 229920001285 xanthan gum Polymers 0.000 description 11
- 235000010493 xanthan gum Nutrition 0.000 description 11
- 229940082509 xanthan gum Drugs 0.000 description 11
- UHVMMEOXYDMDKI-JKYCWFKZSA-L zinc;1-(5-cyanopyridin-2-yl)-3-[(1s,2s)-2-(6-fluoro-2-hydroxy-3-propanoylphenyl)cyclopropyl]urea;diacetate Chemical compound [Zn+2].CC([O-])=O.CC([O-])=O.CCC(=O)C1=CC=C(F)C([C@H]2[C@H](C2)NC(=O)NC=2N=CC(=CC=2)C#N)=C1O UHVMMEOXYDMDKI-JKYCWFKZSA-L 0.000 description 11
- 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 10
- 125000002057 carboxymethyl group Chemical group [H]OC(=O)C([H])([H])[*] 0.000 description 10
- 229920002678 cellulose Polymers 0.000 description 10
- 239000001913 cellulose Substances 0.000 description 10
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 description 10
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 description 10
- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical compound [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 description 9
- 239000004299 sodium benzoate Substances 0.000 description 9
- 235000010234 sodium benzoate Nutrition 0.000 description 9
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 8
- 210000004268 dentin Anatomy 0.000 description 8
- 239000000203 mixture Substances 0.000 description 8
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 8
- 235000019333 sodium laurylsulphate Nutrition 0.000 description 8
- FTLYMKDSHNWQKD-UHFFFAOYSA-N (2,4,5-trichlorophenyl)boronic acid Chemical compound OB(O)C1=CC(Cl)=C(Cl)C=C1Cl FTLYMKDSHNWQKD-UHFFFAOYSA-N 0.000 description 7
- 239000000047 product Substances 0.000 description 7
- 229940085605 saccharin sodium Drugs 0.000 description 7
- 230000001680 brushing effect Effects 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- FBPFZTCFMRRESA-JGWLITMVSA-N D-glucitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-JGWLITMVSA-N 0.000 description 5
- 229920002488 Hemicellulose Polymers 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 5
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 5
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 5
- 239000008368 mint flavor Substances 0.000 description 5
- 238000007873 sieving Methods 0.000 description 5
- 210000005239 tubule Anatomy 0.000 description 5
- 238000005303 weighing Methods 0.000 description 5
- 239000000853 adhesive Substances 0.000 description 4
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- 229910003480 inorganic solid Inorganic materials 0.000 description 4
- 239000004323 potassium nitrate Substances 0.000 description 4
- 235000010333 potassium nitrate Nutrition 0.000 description 4
- NIXOWILDQLNWCW-UHFFFAOYSA-N Acrylic acid Chemical compound OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 3
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 3
- 239000004354 Hydroxyethyl cellulose Substances 0.000 description 3
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 3
- 229920002125 Sokalan® Polymers 0.000 description 3
- 230000000844 anti-bacterial effect Effects 0.000 description 3
- 229960001631 carbomer Drugs 0.000 description 3
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 3
- 239000007795 chemical reaction product Substances 0.000 description 3
- FOCAUTSVDIKZOP-UHFFFAOYSA-N chloroacetic acid Chemical compound OC(=O)CCl FOCAUTSVDIKZOP-UHFFFAOYSA-N 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 210000003298 dental enamel Anatomy 0.000 description 3
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- 235000015424 sodium Nutrition 0.000 description 3
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- 229910052708 sodium Inorganic materials 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical group [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- 208000036372 Sensitivity of teeth Diseases 0.000 description 2
- TVXBFESIOXBWNM-UHFFFAOYSA-N Xylitol Natural products OCCC(O)C(O)C(O)CCO TVXBFESIOXBWNM-UHFFFAOYSA-N 0.000 description 2
- 239000003082 abrasive agent Substances 0.000 description 2
- 230000000840 anti-viral effect Effects 0.000 description 2
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- 229960005069 calcium Drugs 0.000 description 2
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- 229910052791 calcium Inorganic materials 0.000 description 2
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 239000000551 dentifrice Substances 0.000 description 2
- 201000002170 dentin sensitivity Diseases 0.000 description 2
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- 229910052588 hydroxylapatite Inorganic materials 0.000 description 2
- HEBKCHPVOIAQTA-UHFFFAOYSA-N meso ribitol Natural products OCC(O)C(O)C(O)CO HEBKCHPVOIAQTA-UHFFFAOYSA-N 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
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- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- 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 2
- AYGJDUHQRFKLBG-UHFFFAOYSA-M sodium;1,1-dioxo-1,2-benzothiazol-3-olate;dihydrate Chemical compound O.O.[Na+].C1=CC=C2C(=O)[N-]S(=O)(=O)C2=C1 AYGJDUHQRFKLBG-UHFFFAOYSA-M 0.000 description 2
- 229940078499 tricalcium phosphate Drugs 0.000 description 2
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- 239000000811 xylitol Substances 0.000 description 2
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- HEBKCHPVOIAQTA-SCDXWVJYSA-N xylitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)CO HEBKCHPVOIAQTA-SCDXWVJYSA-N 0.000 description 2
- 229960002675 xylitol Drugs 0.000 description 2
- ZYPDJSJJXZWZJJ-UHFFFAOYSA-N 2-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]-3-piperidin-4-yloxypyrazol-1-yl]-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C=1C(=NN(C=1)CC(=O)N1CC2=C(CC1)NN=N2)OC1CCNCC1 ZYPDJSJJXZWZJJ-UHFFFAOYSA-N 0.000 description 1
- FJKROLUGYXJWQN-UHFFFAOYSA-N 4-hydroxybenzoic acid Chemical compound OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 description 1
- DEXFNLNNUZKHNO-UHFFFAOYSA-N 6-[3-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperidin-1-yl]-3-oxopropyl]-3H-1,3-benzoxazol-2-one Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C1CCN(CC1)C(CCC1=CC2=C(NC(O2)=O)C=C1)=O DEXFNLNNUZKHNO-UHFFFAOYSA-N 0.000 description 1
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- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 description 1
- OSWPMRLSEDHDFF-UHFFFAOYSA-N methyl salicylate Chemical compound COC(=O)C1=CC=CC=C1O OSWPMRLSEDHDFF-UHFFFAOYSA-N 0.000 description 1
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- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
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- GNSKLFRGEWLPPA-UHFFFAOYSA-M potassium dihydrogen phosphate Chemical compound [K+].OP(O)([O-])=O GNSKLFRGEWLPPA-UHFFFAOYSA-M 0.000 description 1
- LWIHDJKSTIGBAC-UHFFFAOYSA-K potassium phosphate Substances [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 description 1
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- KSAVQLQVUXSOCR-UHFFFAOYSA-M sodium lauroyl sarcosinate Chemical compound [Na+].CCCCCCCCCCCC(=O)N(C)CC([O-])=O KSAVQLQVUXSOCR-UHFFFAOYSA-M 0.000 description 1
- 229940045885 sodium lauroyl sarcosinate Drugs 0.000 description 1
- YWIVKILSMZOHHF-QJZPQSOGSA-N sodium;(2s,3s,4s,5r,6r)-6-[(2s,3r,4r,5s,6r)-3-acetamido-2-[(2s,3s,4r,5r,6r)-6-[(2r,3r,4r,5s,6r)-3-acetamido-2,5-dihydroxy-6-(hydroxymethyl)oxan-4-yl]oxy-2-carboxy-4,5-dihydroxyoxan-3-yl]oxy-5-hydroxy-6-(hydroxymethyl)oxan-4-yl]oxy-3,4,5-trihydroxyoxane-2- Chemical compound [Na+].CC(=O)N[C@H]1[C@H](O)O[C@H](CO)[C@@H](O)[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@H](O[C@H]2[C@@H]([C@@H](O[C@H]3[C@@H]([C@@H](O)[C@H](O)[C@H](O3)C(O)=O)O)[C@H](O)[C@@H](CO)O2)NC(C)=O)[C@@H](C(O)=O)O1 YWIVKILSMZOHHF-QJZPQSOGSA-N 0.000 description 1
- 229960002920 sorbitol Drugs 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000006277 sulfonation reaction Methods 0.000 description 1
- 235000013616 tea Nutrition 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- 210000001519 tissue Anatomy 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
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- 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
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
- A61K8/9783—Angiosperms [Magnoliophyta]
- A61K8/9794—Liliopsida [monocotyledons]
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P1/00—Drugs for disorders of the alimentary tract or the digestive system
- A61P1/02—Stomatological preparations, e.g. drugs for caries, aphtae, periodontitis
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P29/00—Non-central analgesic, antipyretic or antiinflammatory agents, e.g. antirheumatic agents; Non-steroidal antiinflammatory drugs [NSAID]
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P31/00—Antiinfectives, i.e. antibiotics, antiseptics, chemotherapeutics
- A61P31/02—Local antiseptics
-
- 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
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/20—Chemical, physico-chemical or functional or structural properties of the composition as a whole
- A61K2800/28—Rubbing or scrubbing compositions; Peeling or abrasive compositions; Containing exfoliants
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/41—Particular ingredients further characterized by their size
- A61K2800/412—Microsized, i.e. having sizes between 0.1 and 100 microns
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/30—Fuel from waste, e.g. synthetic alcohol or diesel
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- Oncology (AREA)
- Biotechnology (AREA)
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Abstract
The embodiment of the invention discloses a composite material containing carboxymethylated bagasse as well as a preparation method and application thereof. The preparation method comprises the following steps: adding sodium chloroacetate aqueous solution into bagasse for carboxymethylation reaction, after the reaction is finished, adding calcium hydroxide to adjust the pH value to be alkaline, then adding carbonate ion source/phosphate ion source until calcium ions in the system are completely converted into calcium carbonate/phosphate calcium salt, and then carrying out centrifugal separation, drying and grinding to obtain the carboxymethylation bagasse-containing composite material. The composite material containing carboxymethylated bagasse fully exerts the advantages of bagasse, has the biocompatibility of inorganic materials, and can replace calcium carbonate or calcium phosphate inorganic salt to be used as a toothpaste abrasive and/or a tooth desensitizer.
Description
Technical Field
The embodiment of the invention relates to the technical field of daily chemical products, oral medical treatment, nursing and cleaning products, and particularly relates to a composite material containing carboxymethylated bagasse as well as a preparation method and application thereof.
Background
Toothpaste generally takes calcium carbonate and calcium phosphate inorganic salt as abrasive. Among them, calcium carbonate is the most widely existing inorganic material in nature, and is also the main component of bones and shells of aquatic animals, has good biocompatibility, and in the field of oral care, calcium carbonate is used as an abrasive for toothpaste and tooth powder and a tooth desensitizer. The performance of calcium carbonate is directly related to the crystallization form and appearance of the calcium carbonate, usually, natural calcium carbonate ore is calcite-type crystal and has a hexahedral structure, even if the natural calcium carbonate ore is processed by adopting a physical crushing process, the natural calcium carbonate ore still has an irregular hexahedral structure, the hardness of microscopic particles is high, and the natural calcium carbonate ore has a certain abrasion risk on enamel after long-term use.
The calcium phosphate inorganic solid particles and hydrates thereof are the abrasive material of the toothpaste with the best mouthfeel and biocompatibility, the element composition of calcium hydrophosphate dihydrate, tricalcium phosphate and hydroxyapatite is similar to the element composition of the surface of enamel, the toothpaste prepared by the abrasive material has unique and fine mouthfeel, and the performance of the toothpaste is outstanding in the aspects of remineralization of the enamel and dentin desensitization. However, the production cost of the calcium phosphate inorganic solid particles is relatively high, and the particle size of the solid particles directly prepared by the precipitation method is large, so that the cleaning effect of the calcium phosphate inorganic solid particles on the slits between teeth is prevented, the calcium phosphate inorganic solid particles are prevented from entering dentin tubules, and the anti-sensitivity performance of the calcium phosphate abrasive is reduced. In addition, the slightly soluble calcium phosphate inorganic substance can cause eutrophication pollution to water bodies.
Therefore, how to develop an abrasive and/or a tooth desensitizer which can replace calcium carbonate or calcium phosphate inorganic salts is a technical problem to be solved in the field.
Disclosure of Invention
Bagasse is a solid organic waste after sugar production of sugarcane, is usually used as fuel for power generation, papermaking, cellulose extraction, xylitol preparation and the like, and deep processing of bagasse in the processes often causes secondary pollution, so that the requirements of energy conservation, emission reduction and carbon neutralization are difficult to realize. The bagasse mainly comprises lignin, cellulose and hemicellulose, and is non-toxic to human bodies. The lignin has certain antibacterial and antiviral properties, the edible cellulose can help digestion, and the hemicellulose polysaccharide is a good prebiotic; the lignin in the bagasse wraps the cellulose and hemicellulose to form a bundle-shaped fiber structure with certain strength; the dried bagasse is easy to swell in water at normal temperature, and the volume is increased.
Because Lignin, cellulose, hemicellulose and the like are often connected with each other in nature to form a Lignin-Carbohydrate Complex (Lignin-Carbohydrate Complex), there is no way to separate and obtain the original Lignin with a completely undamaged structure at present. From the viewpoint of materials science, bagasse is a material with certain mechanical rigidity (lignin) and elasticity (cellulose), and if the bagasse is directly used in toothpaste, the use taste is poor due to poor compatibility of organic matter composition on the surface of the bagasse and inorganic materials on the surface of teeth.
Because the molecular structure of the lignin has active groups such as aromatic group, phenolic hydroxyl group, alcoholic hydroxyl group, carbon-based conjugated double bond and the like, the lignin can be subjected to a plurality of chemical reactions such as oxidation, reduction, hydrolysis, alcoholysis, acid hydrolysis methoxy group, carboxyl group, photolysis, phthalylation, sulfonation, alkylation, halogenation, nitration, polycondensation or graft copolymerization and the like, and the lignin provides powerful conditions for modifying the lignin.
The reaction of cellulose with monochloroacetic acid to prepare carboxymethyl cellulose with different degrees of substitution is a well-established process, and carboxymethyl cellulose is a commonly used thickening agent in toothpaste. The differentiation of lignin and cellulose in bagasse is difficult, but both the lignin and the cellulose are nontoxic to human bodies and have terminal hydroxyl groups with similar structures, and the bagasse-acetic ether structure formed by monochloroacetic acid and the lignin, the cellulose and hemicellulose in the bagasse can carboxyl the terminal hydroxyl groups on the surface of the bagasse, and the carboxyl groups have negative charges and can adsorb calcium ions.
In order to fully exert the application of bagasse in toothpaste, reduce environmental pollution and improve the biocompatibility and taste of bagasse applied in toothpaste, chloroacetic acid is adopted to convert hydroxyl on the surface of bagasse into carboxyl, negative charges at the carboxyl end are utilized to adsorb calcium ions with positive charges, and then carbonate or phosphate with good biocompatibility is respectively used to react with the calcium ions to form carboxymethylated bagasse/calcium carbonate or carboxymethylated bagasse/calcium phosphate salt core-shell composite material, so that the material fully exerts the advantages of bagasse and has the biocompatibility of inorganic materials.
Specifically, the embodiment of the invention provides the following technical scheme:
according to the first aspect of the embodiment of the invention, the embodiment of the invention provides a preparation method of a bagasse composite material containing carboxymethylation, wherein an aqueous solution of sodium chloroacetate is added into bagasse to carry out carboxymethylation reaction, calcium hydroxide is added after the reaction is finished to adjust the pH value to be alkaline, then carbonate ion source/phosphate ion source is added until calcium ions in the system are completely converted into calcium carbonate/phosphate calcium salt, and then centrifugal separation, drying and grinding are carried out to obtain the bagasse composite material containing carboxymethylation.
In the invention, the concentration of the sodium chloroacetate aqueous solution is 0.1-80%, and the mass volume ratio of the bagasse to the sodium chloroacetate aqueous solution is 1: 3 to 50.
In the invention, the sodium chloroacetate aqueous solution is added in a dropping manner, and the dropping speed is 3-5 drops/s.
In the invention, the temperature of the carboxymethylation reaction is 35-80 ℃, and the time is 1-3 h.
In the invention, the pH value is 7.5-9.
In the present invention, the carbonate ion source is selected from one or more selected from sodium carbonate, sodium bicarbonate, dimethyl carbonate, carbon dioxide.
In the present invention, the phosphate ion source is one or more selected from the group consisting of trisodium phosphate, sodium dihydrogen phosphate, potassium dihydrogen phosphate, disodium hydrogen phosphate, dipotassium hydrogen phosphate, diammonium hydrogen phosphate, and phosphorus pentoxide.
In the invention, the phosphate calcium salt is selected from one or more of tricalcium phosphate, calcium hydrophosphate and hydroxyapatite.
In the invention, the particle size of the composite material containing carboxymethylated bagasse is 0.1-100 microns.
In the invention, the preparation method of the bagasse comprises the following steps: the method comprises the steps of squeezing sugar from sugarcane, adding water, carrying out ball milling until a leaching solution is clear and transparent, screening the leaching solution with a water screen of more than 40 meshes to remove large particles, drying undersize materials, and carrying out jet milling to obtain powder with the particle size of 0.1-50 microns.
According to a second aspect of embodiments of the present invention, there is provided a carboxymethylated bagasse-containing composite material, produced by the production method as described above.
According to a third aspect of embodiments of the present invention there is provided the use of a carboxymethylated bagasse-containing composite as described above as at least one of an abrasive, anti-sensitivity ingredient in an oral care product.
In the present invention, the oral care product is a toothpaste, a dentifrice or a tooth desensitizer.
According to a fourth aspect of embodiments of the present invention there is provided a toothpaste comprising a carboxymethylated bagasse-containing composite material as described above.
In the invention, the composite material containing carboxymethylated bagasse accounts for 0.1-70 wt% of the toothpaste, preferably 10-70 wt%.
In the invention, the toothpaste also comprises at least one of a humectant, a binder, an abrasive, essence, a preservative, a sweetener, a foaming agent and water.
Wherein the humectant is a humectant conventionally used in the field, such as glycerin, sorbitol, sodium hyaluronate and the like; the adhesive is adhesive conventionally used in the field, such as xanthan gum, carrageenan, sodium carboxymethylcellulose, sodium hydroxyethylcellulose, carbomer and the like; the abrasive is an abrasive conventionally used in the field, such as calcium carbonate, calcium phosphate salts, silica, and the like; the essence is of the type conventionally used in the field, such as mint, spearmint, wintergreen, fruit, tea, drug, etc.; the preservative is a preservative conventionally used in the field, such as sodium benzoate, paraben and the like; the sweetening agent is a sweetening agent conventionally used in the art, such as sorbitol, xylitol, saccharin sodium, and the like. The foaming agent is a foaming agent conventionally used in the art, such as sodium lauryl sulfate, sodium lauroyl sarcosinate, and the like.
In a specific embodiment of the invention, when the toothpaste takes the carboxymethylated bagasse-containing composite material as an abrasive, the toothpaste comprises the following components in percentage by weight: 1 to 70 percent of sorbitol; 0.3 to 2 percent of cellulose gum; 0.1 to 2 percent of xanthan gum; 0.1-2% of carrageenan; 1% -50% of glycerol; 0.1 to 70 percent of composite material containing carboxymethylated bagasse; essence, preservative, sweetener, foaming agent and water are supplemented to 100 percent.
In another specific embodiment of the invention, when the toothpaste takes the carboxymethylated bagasse-containing composite material as a partial abrasive, the toothpaste comprises the following components in percentage by weight: 15 to 80 percent of humectant (glycerin, sorbitol and mixture thereof in any proportion); 0.4 to 3 percent of adhesive (xanthan gum, carrageenan, sodium carboxymethyl cellulose, sodium hydroxyethyl cellulose, carbomer and mixture of any proportion thereof); 7-60% of abrasive (besides the composite material containing carboxymethylated bagasse, at least one of calcium carbonate, calcium phosphate salts and silicon dioxide); essence, preservative, sweetening agent, foaming agent and water are added to make up 100 percent.
In another embodiment of the invention, when the carboxymethylated bagasse-containing composite material is used as an abrasive and an anti-sensitivity component, the tooth anti-sensitivity toothpaste comprises the following components in percentage by weight: 15 to 80 percent of humectant (glycerin, sorbitol and mixture thereof in any proportion); 0.4 to 3 percent of adhesive (xanthan gum, carrageenan, sodium carboxymethyl cellulose, sodium hydroxyethyl cellulose, carbomer and mixture of any proportion thereof); 7-60% of abrasive (besides the composite material containing carboxymethylated bagasse, at least one of calcium carbonate, calcium phosphate salts and silicon dioxide); 0.5-7% of potassium nitrate; essence, preservative, sweetener, foaming agent and water are supplemented to 100 percent.
The embodiment of the invention has the following advantages:
1. the composite material containing carboxymethylated bagasse, which is prepared by taking bagasse as a raw material, fully exerts the advantages of the bagasse, has the biocompatibility of inorganic materials, and can replace calcium carbonate or calcium phosphate inorganic salt to be used as a toothpaste abrasive and/or a tooth desensitizer.
2. The bagasse is applied to the oral care product, so that the anti-inflammatory and antibacterial properties of the lignin can be fully exerted, and natural and safe antibacterial and antiviral properties are provided for the oral care product; the carbon neutralization is really realized, and other toxic chemical substances are not required to be introduced; the carbon captured by the sugarcane from the air is stored in the oral care product for a long time, and the release period of the carbon is delayed.
3. The preparation method provided by the invention has the advantages of simple and convenient operation of steps, simple process flow, great reduction of cost and contribution to industrial production.
Detailed Description
The present invention is described in terms of particular embodiments, other advantages and features of the invention will become apparent to those skilled in the art from the following disclosure, and it is to be understood that the described embodiments are merely exemplary of the invention and that it is not intended to limit the invention to the particular embodiments disclosed. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention. The test methods used in the examples are, unless otherwise specified, regarded as conventional methods; the materials, reagents and the like used are commercially available unless otherwise specified.
Grinding material calcium carbonate: particle size 5-70 microns, manufacturer: guangxi Ruiyun;
abrasive monocalcium phosphate: particle size 5-100 microns, manufacturer: creating in south China.
In the following examples and comparative examples, bagasse was prepared as follows: after sugar squeezing, adding water with the volume 15 times of that of sugar cane for 5 times, ball-milling for 3 hours at the rotating speed of 200r/min until a leaching solution is clear and transparent, sieving the leaching solution by a water sieve with more than 40 meshes to remove large particles, drying undersize materials, and carrying out jet milling to obtain powder with the particle size of 0.1-50 microns.
Example 1
The preparation method of the carboxymethylated bagasse/calcium carbonate composite material provided by this example is as follows:
1) weighing 100g of bagasse powder, placing the bagasse powder into a 5000ml round-bottom flask, dropwise adding 2L of 20% sodium chloroacetate solution into the round-bottom flask at the speed of 3-5 drops/s by using a dropping funnel, adjusting the temperature of a water bath kettle to 75 ℃ after the dropwise adding, stirring for 2.0 hours,
2) dripping 0.1% calcium hydroxide solution until the pH value is 7.5-9 to obtain carboxymethyl calcified bagasse, then adding 35g of sodium carbonate, and stirring for 20 min;
3) centrifuging at 1000r/min for 20min, drying the obtained solid in a drying oven at 105 deg.C for 2h, grinding, and sieving with 80 mesh sieve to obtain carboxymethylated bagasse/calcium carbonate composite material.
Example 2
The preparation method of the carboxymethylated bagasse/calcium carbonate composite material provided in this example is as follows:
1) weighing 100g of bagasse powder, placing the bagasse powder into a round-bottom flask with the volume of 5L, dropwise adding 2L of 35% sodium chloroacetate solution into the round-bottom flask at the speed of 3-5 drops/s by using a dropping funnel, adjusting the temperature of a water bath kettle to 70 ℃ after dropwise adding, and stirring for 3 hours;
2) after the reaction is finished, titrating the mixture by using 0.1% calcium hydroxide solution until the ph is 7.5-9 to obtain carboxymethyl calcified bagasse;
3) adding 50g of sodium carbonate into the carboxymethyl calcified bagasse obtained in the step 2), stirring for 30min, centrifuging the reaction product for 10min at the rotating speed of 1000r/min, drying the obtained solid in a drying box at 105 ℃ for 2h, grinding, and sieving by a 100-mesh sieve to obtain the carboxymethyl bagasse/calcium carbonate composite material.
Example 3
The preparation method of the composite material containing carboxymethylated bagasse provided by the embodiment comprises the following steps:
1) weighing 100g of bagasse powder, placing the bagasse powder into a 5L round-bottom flask, dropwise adding 2L of 45% sodium chloroacetate solution into the round-bottom flask at a speed of 3-5 drops/s by using a dropping funnel, adjusting the temperature of a water bath kettle to 80 ℃ after dropwise adding, and stirring for 3 hours;
2) after the reaction is finished, 0.1 percent of calcium hydroxide solution is added dropwise until the pH value is 8, and then the carboxymethyl calcified bagasse is obtained;
3) adding 200g of trisodium phosphate into the carboxymethyl calcified bagasse obtained in the step 2), stirring for 50min, centrifuging the reaction product for 10min at the rotating speed of 1000r/min, drying the obtained solid in a drying oven at 105 ℃ for 2h, grinding, and sieving by a 100-mesh sieve to obtain the carboxymethyl bagasse/calcium phosphate salt composite material.
Example 4
The preparation method of the composite material containing carboxymethylated bagasse provided by the embodiment comprises the following steps:
1) weighing 100g of bagasse powder, placing the bagasse powder into a 5L round-bottom flask, dropwise adding a 60% sodium chloroacetate solution into the round-bottom flask at a speed of 3-5 drops/s by using a dropping funnel, adjusting the temperature of a water bath to 45 ℃ after dropwise adding, and stirring for 5 hours;
2) adding into a flaskInto CaCl 2 Stirring for 1 hour for 110g to obtain carboxymethyl calcified bagasse;
3) adding 135g of monopotassium phosphate into the carboxymethyl calcified bagasse obtained in the step 2), stirring for 90min, centrifuging the reaction product for 20min at the rotating speed of 1000r/min, drying the obtained solid in a drying oven at 105 ℃ for 2h, grinding, and sieving by a 100-mesh sieve to obtain the carboxymethyl bagasse/calcium phosphate salt composite material.
Example 5
The embodiment provides toothpaste, which comprises the following components in percentage by weight:
the carboxymethylated bagasse/calcium carbonate composite material of example 1, 20% of silicon dioxide, 35% of glycerol, 15% of sorbitol, 0.3% of xanthan gum, 0.5% of carrageenan, 0.5% of sodium carboxymethylcellulose, 1.5% of mint-flavored essence, 0.5% of sodium benzoate, 0.3% of saccharin sodium, 2% of sodium lauryl sulfate, and the balance of water.
The preparation method of the toothpaste comprises the following steps:
1) adding water, sodium benzoate, saccharin sodium and sorbitol into a water phase pot of homogenizing and emulsifying equipment, and stirring until the sodium benzoate, the saccharin sodium and the sorbitol are dissolved for later use;
2) adding glycerol into an oil phase pot of homogenizing and emulsifying equipment, starting stirring at a rotating speed of 100r/min, and putting xanthan gum, carrageenan and sodium carboxymethylcellulose into the oil phase pot until the components are uniformly dispersed for later use;
3) sucking the materials in the oil phase pot into a homogenizing pot under negative pressure, starting wall hanging and stirring (rotating speed 100r/min), sucking the materials in the water phase pot into the homogenizing pot under negative pressure, starting homogenizing and stirring at a rotating speed of 2000r/min, and stirring for 5 minutes until the materials are uniformly dispersed and fully swelled;
4) sucking carboxymethylated bagasse/calcium carbonate composite material and silicon dioxide into a homogenizing pot under negative pressure, and stirring for 30 minutes until the system is uniform;
5) adding the mint flavor essence into a homogenizing pot, uniformly stirring, and starting vacuum till the negative pressure is less than-0.06 Mp;
6) sucking sodium lauryl sulfate into a homogenizing pot under negative pressure, continuing stirring for 10 minutes, starting vacuum till the negative pressure is less than-0.08 MP, continuing stirring till the system is uniform, and discharging.
Example 6
The embodiment provides an anti-allergic toothpaste for teeth, which comprises the following components in percentage by weight:
10% of the carboxymethylated bagasse/calcium carbonate salt composite material of example 1, 10% of silicon dioxide, 35% of glycerol, 15% of sorbitol, 0.4% of xanthan gum, 0.4% of carrageenan, 0.5% of sodium carboxymethylcellulose, 1.5% of mint-flavor essence, 0.5% of sodium benzoate, 0.3% of saccharin sodium, 2% of sodium lauryl sulfate, 3% of potassium nitrate, and the balance of water.
This example provides a dental anti-sensitivity toothpaste prepared substantially as in example 5, wherein potassium nitrate is added in step 1).
Example 7
The embodiment provides toothpaste, which comprises the following components in percentage by weight:
5% of the carboxymethylated bagasse/calcium carbonate composite material of example 2, 15% of silicon dioxide, 35% of glycerol, 15% of sorbitol, 5% of silicon dioxide, 0.5% of xanthan gum, 0.3% of carrageenan, 0.5% of sodium carboxymethylcellulose, 1.5% of mint-flavor essence, 0.5% of sodium benzoate, 0.3% of saccharin sodium, 2% of sodium lauryl sulfate, and the balance of water.
The preparation method of the toothpaste provided in this example is the same as that of example 5.
Example 8
The embodiment provides a toothpaste, which comprises the following components in percentage by weight:
the carboxymethylated bagasse/calcium phosphate salt composite material of example 3 comprises 20% of silicon dioxide, 35% of glycerol, 15% of sorbitol, 0.4% of xanthan gum, 0.4% of carrageenan, 0.3% of sodium carboxymethylcellulose, 1.5% of mint-flavor essence, 0.5% of sodium benzoate, 0.3% of saccharin sodium, 2% of sodium lauryl sulfate, 3% of potassium nitrate, and the balance of water.
The preparation method of the toothpaste provided in this example is the same as that of example 5.
Example 9
The embodiment provides toothpaste, which comprises the following components in percentage by weight:
the carboxymethylated bagasse/calcium phosphate salt composite material of example 3 is 10%, silicon dioxide 15%, glycerol 35%, sorbitol 15%, silicon dioxide 5%, xanthan gum 0.5%, carrageenan 0.3%, sodium carboxymethylcellulose 0.5%, mint-flavored essence 1.5%, sodium benzoate 0.5%, sodium saccharin 0.3%, sodium lauryl sulfate 2%, and the balance of water.
The preparation method of the toothpaste provided in this example is the same as that of example 6.
Example 10
The embodiment provides a toothpaste, which comprises the following components in percentage by weight:
5% of carboxymethylated bagasse/calcium phosphate salt composite material of example 4, 15% of silicon dioxide, 35% of glycerol, 15% of sorbitol, 5% of silicon dioxide, 0.5% of xanthan gum, 0.3% of carrageenan, 0.5% of sodium carboxymethylcellulose, 1.5% of mint-flavor essence, 0.5% of sodium benzoate, 0.3% of sodium saccharin, 2% of sodium lauryl sulfate, and the balance of water.
The preparation method of the toothpaste provided in this example is the same as that of example 5.
Comparative example 1
This comparative example provides a toothpaste which differs from example 5 only in that the carboxymethylated bagasse/calcium carbonate composite was replaced by an equal amount of abrasive calcium carbonate.
The toothpaste provided in this comparative example was prepared as in example 5.
Comparative example 2
This comparative example provides a tooth anti-sensitivity toothpaste which differs from example 6 only in that the carboxymethylated bagasse/calcium carbonate composite was replaced with an equal amount of abrasive calcium carbonate.
This comparative example provides the same preparation method as example 6 for a dental anti-sensitivity toothpaste.
Comparative example 3
This comparative example provides a toothpaste which differs from example 7 in that the carboxymethylated bagasse/calcium carbonate composite was replaced with an equal amount of abrasive calcium carbonate.
The toothpaste provided in this comparative example was prepared as in example 7.
Comparative example 4
This comparative example provides a toothpaste which differs from example 8 only in that the carboxymethylated bagasse/calcium phosphate salt composite was replaced with an equal amount of abrasive monocalcium phosphate.
The toothpaste provided in this comparative example was prepared as in example 8.
Comparative example 5
This comparative example provides a dentifrice of tooth desensitization which differs from example 9 only in that the carboxymethylated bagasse/calcium phosphate salt composite was replaced with the equivalent amount of abrasive monocalcium phosphate.
This comparative example provides a dental anti-sensitivity toothpaste prepared according to the same method as example 9.
Comparative example 6
This comparative example provides a toothpaste which differs from example 10 in that the carboxymethylated bagasse/calcium phosphate salt composite was replaced with an equal amount of abrasive monocalcium phosphate.
The toothpaste provided in this comparative example was prepared as in example 10.
Test example 1
Whiteness detection
The whiteness of the toothpaste was tested using a WSD-III automatic whiteness meter. The results of whiteness testing of the toothpastes of example 5 and comparative example 1, and example 8 and comparative example 4 are shown in table 1.
TABLE 1
Toothpaste sample | Whiteness degree | Toothpaste sample | Whiteness degree |
Example 5 | 91 | Example 8 | 94 |
Comparative example 1 | 91 | Comparative example 4 | 95 |
The results show that: the whiteness of the toothpastes of example 5 and comparative example 1 is basically consistent, and the whiteness of the toothpastes of example 8 and comparative example 4 is basically consistent, which shows that the carboxymethylated bagasse-containing composite material of the invention as an abrasive for toothpastes can realize the appearance performance of the paste which is basically the same as the abrasive calcium carbonate or calcium dihydrogen phosphate.
Test example 2
Cleaning force test
Weighing 1.0g of toothpaste sample, placing on a white organic glass plate attached with special dirt on a cleaning value tester, putting down a machine head provided with a soft-bristle toothbrush, enabling the bristles to be in close contact with the organic glass plate, starting the tester, and then enabling the toothbrush to move back and forth to rub the organic glass plate. After rubbing 20 times, 50 times, 100 times, 150 times, 200 times and 300 times in sequence, the organic glass plate was taken out and put into a colorimeter to measure the corresponding data. The 6 data are converted into a cleaning value CV. Higher CV values indicate greater cleaning power of the toothpaste. The results of the cleaning value tests for the toothpastes of example 5 and comparative example 1, and example 8 and comparative example 4 are shown in table 2.
TABLE 2
Toothpaste sample | CV value | Toothpaste sample | CV value |
Example 5 | 15 | Example 8 | 24 |
Comparative example 1 | 12 | Comparative example 4 | 18 |
The results show that: when 20% of abrasive calcium carbonate in the toothpaste is replaced by the carboxymethylated bagasse/calcium carbonate composite material in the embodiment of the invention, the cleaning value of the toothpaste is improved by more than 20%; when 20% of the abrasive monocalcium phosphate in the toothpaste replaced the carboxymethylated bagasse/calcium phosphate composite of the present example, the cleaning value of the toothpaste increased from 18 to 24, an improvement of more than 30%. The above description demonstrates that the carboxymethylated bagasse-containing composite material of the present invention, as an abrasive for toothpaste, has superior tooth cleaning performance as compared to the existing abrasive calcium carbonate or monocalcium phosphate.
Test example 3
Isolated dentin tubule experiment
Cutting dentin slices with the thickness of about 3mm at a position 1-4mm below a glazed dentin boundary by using a hard tissue cutting machine perpendicular to the long axis direction of a tooth body, sequentially grinding and polishing by using sand paper on a horizontal grinding instrument to prepare dentin slices with the thickness of about 2mm, ultrasonically cleaning for later use, carrying out acid etching for 2min by using 6% citric acid, washing by using distilled water for 30S, and blow-drying to prepare the sensitive dentin. Tooth brushing test of sensitive dentin with the same toothbrush was performed for the same concentration of toothpaste slurry, and then SEM observation was performed on the surface and longitudinal section of the isolated dentin to calculate the occlusion rate (PR) of the isolated dentin tubules. The results of the test for the clogging rate of the tooth anti-sensitivity toothpaste of example 6 and comparative example 2, and example 9 and comparative example 5 are shown in table 3.
TABLE 3
Toothpaste sample | PR value | Toothpaste sample | PR value |
Example 6 | 96% | Example 9 | 95.4% |
Comparative example 2 | 15% | Comparative example 5 | 20% |
The results show that: when 10% of abrasive calcium carbonate in the tooth anti-sensitivity toothpaste replaces the carboxymethylated bagasse/calcium carbonate composite material in the embodiment of the invention, the blocking rate of the isolated dentinal tubules of the tooth anti-sensitivity toothpaste reaches more than 95%; when 10% of abrasive monocalcium phosphate in the tooth anti-sensitivity toothpaste is replaced by the carboxymethylated bagasse/calcium phosphate salt composite material in the embodiment of the invention, the blocking rate of isolated dentinal tubules of the tooth anti-sensitivity toothpaste reaches more than 95%. The above description shows that the composite material containing carboxymethylated bagasse of the embodiment of the present invention has more excellent desensitizing effect as an abrasive and an anti-sensitivity component for tooth anti-sensitivity toothpaste, compared with abrasive calcium carbonate or monocalcium phosphate.
Test example 4
Taste test brush
60 volunteers with healthy oral cavity were randomly selected and divided into experiment 1-4 groups of 15 individuals. Wherein the volunteers of experiment 1 group used the toothpaste of example 6, the volunteers of experiment 2 group used the toothpaste of comparative example 2, the volunteers of experiment 3 group used the toothpaste of example 7, and the volunteers of experiment 4 group used the toothpaste of comparative example 3. All volunteers used a toothbrush provided by Yunnan white drug group, Inc. in a unified manner to adopt a personal habit tooth brushing method. After 3 days, questionnaires are filled in according to the toothpaste taste, and the results are obtained through statistics. Wherein:
like: the taste is fine and smooth, and no granular feeling is generated;
in general: the taste is rough, and the granule friction feeling is obvious;
dislike: has rough mouthfeel and obvious granular rubbing feeling.
The test results are shown in Table 4.
TABLE 4
Group of | Toothpaste sample | Xi Huan | In general terms | Dislike of | Preference degree |
Experiment 1 group | Examples6 | 10 | 3 | 2 | 66.7% |
Experiment 2 groups | Comparative example 2 | 5 | 8 | 2 | 33.3% |
Experiment 3 groups | Example 7 | 6 | 6 | 3 | 40% |
Experiment 4 groups | Comparative example 3 | 5 | 7 | 3 | 33.3% |
The results show that: when 5% of abrasive calcium carbonate in the toothpaste was substituted for the carboxymethylated bagasse/calcium carbonate composite material of the examples of the present invention, there was essentially no difference in the brushing taste of the toothpaste; when 10% of the abrasive calcium carbonate in the toothpaste was substituted for the carboxymethylated bagasse/calcium carbonate composite material of the examples of the invention, the brushing taste preference of the toothpaste was increased by more than 30%.
60 volunteers with healthy oral cavity were randomly selected and divided into experiment 1-4 groups of 15 individuals. Wherein the volunteers of experiment 1 group used the toothpaste of example 9, the volunteers of experiment 2 group used the toothpaste of comparative example 5, the volunteers of experiment 3 group used the toothpaste of example 10, and the volunteers of experiment 4 group used the toothpaste of comparative example 6. All volunteers used a toothbrush provided by Yunnan white drug group, Inc. in a unified manner to adopt a personal habit tooth brushing method. After 3 days, questionnaires are filled in according to the toothpaste taste, and the results are obtained through statistics. Wherein:
like: the taste is fine and smooth, and no granular feeling is generated;
in general: the taste is rough, and the granule friction feeling is obvious;
dislike: has rough mouthfeel and obvious granular rubbing feeling.
The test results are shown in Table 5.
TABLE 5
Group of | Toothpaste sample | Xi Huan | In general terms | Dislike of | Preference degree |
Experiment 1 group | Example 9 | 12 | 2 | 1 | 80% |
Experiment 2 groups | Comparative example 5 | 8 | 2 | 5 | 53.3% |
Experiment 3 groups | Example 10 | 9 | 4 | 2 | 60% |
Experiment 4 groups | Comparative example 6 | 8 | 3 | 4 | 53.3% |
The results show that: when 5% of the abrasive monocalcium phosphate in the toothpaste was substituted for the carboxymethylated bagasse/calcium phosphate composite of the present examples, there was essentially no difference in the brush test mouthfeel of the toothpaste (see experiment 3-4); when 10% of the abrasive monocalcium phosphate in the toothpaste was substituted for the carboxymethylated bagasse/calcium phosphate salt composite of the examples of the invention, the brushing taste preference of the toothpaste was increased by more than 20% (see experiment 1-2).
The above description shows that the composite material containing carboxymethylated bagasse of the embodiment of the present invention is more acceptable and favored by the public when added to toothpaste than the abrasive calcium carbonate or monocalcium phosphate.
Although the invention has been described in detail above with reference to a general description and specific examples, it will be apparent to one skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (10)
1. A preparation method of a bagasse composite material containing carboxymethylation is characterized in that a sodium chloroacetate aqueous solution is added into bagasse to carry out carboxymethylation reaction, calcium hydroxide is added after the reaction is finished to adjust the pH value to be alkaline, then carbonate ion source/phosphate ion source is added until calcium ions in the system are completely converted into calcium carbonate/phosphate calcium salt, and then centrifugal separation, drying and grinding are carried out to obtain the bagasse composite material containing carboxymethylation.
2. The preparation method of the carboxymethylated bagasse composite material according to claim 1, characterized in that the concentration of the sodium chloroacetate aqueous solution is 0.1% -80%, and the mass volume ratio of the bagasse to the sodium chloroacetate aqueous solution is 1: 3-50;
and/or adding the sodium chloroacetate aqueous solution in a dropping manner, wherein the dropping speed is 3-5 drops/s;
and/or the temperature of the carboxymethylation reaction is 35-80 ℃, and the time is 1-3 h.
3. The preparation method of the carboxymethylated bagasse-containing composite material according to claim 1, characterized in that the pH value is 7.5-9.
4. A process for the preparation of carboxymethylated bagasse composite material according to claim 1, characterized in that the source of carbonate ions is selected from one or more of sodium carbonate, sodium bicarbonate, dimethyl carbonate, carbon dioxide;
and/or the phosphate ion source is selected from one or more of trisodium phosphate, sodium dihydrogen phosphate, potassium dihydrogen phosphate, disodium hydrogen phosphate, dipotassium hydrogen phosphate, diammonium hydrogen phosphate and phosphorus pentoxide.
5. The preparation method of the carboxymethylated bagasse-containing composite material according to claim 1, characterized in that the particle size of the carboxymethylated bagasse-containing composite material is 0.1-100 μm.
6. A method for preparing a carboxymethylated bagasse-containing composite material according to any one of claims 1 to 5, characterized in that bagasse is prepared as follows: the method comprises the steps of squeezing sugar from sugarcane, adding water, carrying out ball milling until a leaching solution is clear and transparent, screening the leaching solution with a water screen of more than 40 meshes, removing large particles, drying undersize materials, and carrying out jet milling to obtain powder with the particle size of 0.1-50 microns.
7. A carboxymethylated bagasse-containing composite material, characterized in that it is produced by the production method as set forth in any one of claims 1 to 6.
8. Use of a carboxymethylated bagasse-containing composite material as claimed in claim 7 in an oral care product, wherein the carboxymethylated bagasse-containing composite material is used as at least one of an abrasive, anti-sensitivity ingredient.
9. The use of claim 8 wherein the oral care product is a toothpaste, a tooth powder, or a tooth desensitizer.
10. A toothpaste, characterized in that it comprises carboxymethylated bagasse-containing composite material as claimed in claim 7, which is 0.1% -70% by mass of the toothpaste;
and/or the toothpaste further comprises at least one of a humectant, a binder, an abrasive, an essence, a preservative, a sweetener, a foaming agent and water.
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WO2016011978A1 (en) * | 2014-07-24 | 2016-01-28 | 北京大清生物技术有限公司 | Composition with multiple oral treatment and healthcare functions and preparation method therefor |
CN106074195A (en) * | 2016-07-06 | 2016-11-09 | 杭州皎洁口腔保健用品有限公司 | A kind of toothpaste of hydroxyl apatite and calcium carbonate and preparation method thereof |
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WO2016011978A1 (en) * | 2014-07-24 | 2016-01-28 | 北京大清生物技术有限公司 | Composition with multiple oral treatment and healthcare functions and preparation method therefor |
CN106074195A (en) * | 2016-07-06 | 2016-11-09 | 杭州皎洁口腔保健用品有限公司 | A kind of toothpaste of hydroxyl apatite and calcium carbonate and preparation method thereof |
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CN115504610A (en) * | 2022-11-16 | 2022-12-23 | 山东海化集团有限公司 | Preparation method and application of concentrated seawater calcium remover |
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