CN116407465A - Application of high molecular polymer in improving stability of toothpaste product - Google Patents
Application of high molecular polymer in improving stability of toothpaste product Download PDFInfo
- Publication number
- CN116407465A CN116407465A CN202310683789.4A CN202310683789A CN116407465A CN 116407465 A CN116407465 A CN 116407465A CN 202310683789 A CN202310683789 A CN 202310683789A CN 116407465 A CN116407465 A CN 116407465A
- Authority
- CN
- China
- Prior art keywords
- toothpaste
- consistency
- high molecular
- mpq
- molecular polymer
- 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
- 229920000642 polymer Polymers 0.000 title claims abstract description 57
- 229940095688 toothpaste product Drugs 0.000 title description 4
- 239000000606 toothpaste Substances 0.000 claims abstract description 237
- 229940034610 toothpaste Drugs 0.000 claims abstract description 235
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 68
- 238000000034 method Methods 0.000 claims abstract description 21
- 238000002360 preparation method Methods 0.000 claims abstract description 20
- 239000003906 humectant Substances 0.000 claims abstract description 17
- 230000008719 thickening Effects 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 239000007864 aqueous solution Substances 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims abstract description 6
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 5
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims abstract description 3
- GQOKIYDTHHZSCJ-UHFFFAOYSA-M dimethyl-bis(prop-2-enyl)azanium;chloride Chemical compound [Cl-].C=CC[N+](C)(C)CC=C GQOKIYDTHHZSCJ-UHFFFAOYSA-M 0.000 claims abstract description 3
- 238000010528 free radical solution polymerization reaction Methods 0.000 claims abstract description 3
- 238000010557 suspension polymerization reaction Methods 0.000 claims abstract description 3
- 239000008367 deionised water Substances 0.000 claims description 40
- 229910021641 deionized water Inorganic materials 0.000 claims description 40
- 238000007865 diluting Methods 0.000 claims description 2
- 238000004132 cross linking Methods 0.000 abstract description 20
- 238000003756 stirring Methods 0.000 description 81
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 76
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 64
- 239000002994 raw material Substances 0.000 description 62
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 46
- QELSKZZBTMNZEB-UHFFFAOYSA-N propylparaben Chemical compound CCCOC(=O)C1=CC=C(O)C=C1 QELSKZZBTMNZEB-UHFFFAOYSA-N 0.000 description 44
- LRCFXGAMWKDGLA-UHFFFAOYSA-N dioxosilane;hydrate Chemical compound O.O=[Si]=O LRCFXGAMWKDGLA-UHFFFAOYSA-N 0.000 description 43
- 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 42
- LXCFILQKKLGQFO-UHFFFAOYSA-N methylparaben Chemical compound COC(=O)C1=CC=C(O)C=C1 LXCFILQKKLGQFO-UHFFFAOYSA-N 0.000 description 42
- 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 42
- 239000000600 sorbitol Substances 0.000 description 42
- 235000019818 tetrasodium diphosphate Nutrition 0.000 description 42
- 229920000289 Polyquaternium Polymers 0.000 description 40
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 38
- 229910000019 calcium carbonate Inorganic materials 0.000 description 38
- 235000019333 sodium laurylsulphate Nutrition 0.000 description 38
- 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 37
- 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 37
- 229940085605 saccharin sodium Drugs 0.000 description 37
- 229960004029 silicic acid Drugs 0.000 description 37
- 239000001768 carboxy methyl cellulose Substances 0.000 description 35
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 description 34
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 description 34
- 229920002565 Polyethylene Glycol 400 Polymers 0.000 description 33
- 229940068918 polyethylene glycol 400 Drugs 0.000 description 33
- 238000012360 testing method Methods 0.000 description 33
- 239000000377 silicon dioxide Substances 0.000 description 32
- 239000000463 material Substances 0.000 description 31
- 239000007787 solid Substances 0.000 description 29
- 239000006072 paste Substances 0.000 description 28
- 239000000843 powder Substances 0.000 description 28
- 229960003415 propylparaben Drugs 0.000 description 24
- 238000005516 engineering process Methods 0.000 description 22
- 239000004292 methyl p-hydroxybenzoate Substances 0.000 description 21
- 229960002216 methylparaben Drugs 0.000 description 21
- 239000004405 propyl p-hydroxybenzoate Substances 0.000 description 20
- 235000010232 propyl p-hydroxybenzoate Nutrition 0.000 description 20
- 239000003814 drug Substances 0.000 description 19
- 239000000126 substance Substances 0.000 description 19
- 239000002562 thickening agent Substances 0.000 description 19
- -1 abrasive Substances 0.000 description 17
- 241001673966 Magnolia officinalis Species 0.000 description 16
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 16
- 239000000047 product Substances 0.000 description 16
- 239000013543 active substance Substances 0.000 description 15
- YGSDEFSMJLZEOE-UHFFFAOYSA-M salicylate Chemical compound OC1=CC=CC=C1C([O-])=O YGSDEFSMJLZEOE-UHFFFAOYSA-M 0.000 description 14
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 description 14
- 239000000230 xanthan gum Substances 0.000 description 14
- 229920001285 xanthan gum Polymers 0.000 description 14
- 235000010493 xanthan gum Nutrition 0.000 description 14
- 229940082509 xanthan gum Drugs 0.000 description 14
- 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 12
- 241000209035 Ilex Species 0.000 description 12
- 235000003332 Ilex aquifolium Nutrition 0.000 description 12
- 235000002296 Ilex sandwicensis Nutrition 0.000 description 12
- 235000002294 Ilex volkensiana Nutrition 0.000 description 12
- 238000004519 manufacturing process Methods 0.000 description 11
- 235000010268 sodium methyl p-hydroxybenzoate Nutrition 0.000 description 11
- 235000010270 methyl p-hydroxybenzoate Nutrition 0.000 description 10
- 150000003839 salts Chemical class 0.000 description 9
- 230000008569 process Effects 0.000 description 8
- 239000011780 sodium chloride Substances 0.000 description 8
- 235000013024 sodium fluoride Nutrition 0.000 description 7
- 239000011775 sodium fluoride Substances 0.000 description 7
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 6
- 241000411851 herbal medicine Species 0.000 description 6
- 229910004298 SiO 2 Inorganic materials 0.000 description 5
- 150000003863 ammonium salts Chemical group 0.000 description 5
- 230000000903 blocking effect Effects 0.000 description 5
- 238000011161 development Methods 0.000 description 5
- 230000015784 hyperosmotic salinity response Effects 0.000 description 5
- 239000003755 preservative agent Substances 0.000 description 5
- CVHZOJJKTDOEJC-UHFFFAOYSA-N saccharin Chemical compound C1=CC=C2C(=O)NS(=O)(=O)C2=C1 CVHZOJJKTDOEJC-UHFFFAOYSA-N 0.000 description 5
- 238000013112 stability test Methods 0.000 description 5
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 4
- 239000004354 Hydroxyethyl cellulose Substances 0.000 description 4
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 description 4
- 239000004698 Polyethylene Substances 0.000 description 4
- 230000009471 action Effects 0.000 description 4
- 239000000654 additive Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000004088 foaming agent Substances 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 description 4
- 230000007794 irritation Effects 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000000049 pigment Substances 0.000 description 4
- 229920000573 polyethylene Polymers 0.000 description 4
- 230000002335 preservative effect Effects 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 229940048086 sodium pyrophosphate Drugs 0.000 description 4
- 230000000087 stabilizing effect Effects 0.000 description 4
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 description 4
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 3
- 241000218378 Magnolia Species 0.000 description 3
- 241001465754 Metazoa Species 0.000 description 3
- 240000000249 Morus alba Species 0.000 description 3
- 235000008708 Morus alba Nutrition 0.000 description 3
- 230000001154 acute effect Effects 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 229920003123 carboxymethyl cellulose sodium Polymers 0.000 description 3
- 229940063834 carboxymethylcellulose sodium Drugs 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 239000002537 cosmetic Substances 0.000 description 3
- 239000004615 ingredient Substances 0.000 description 3
- 210000000214 mouth Anatomy 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- 229960001866 silicon dioxide Drugs 0.000 description 3
- 235000012239 silicon dioxide Nutrition 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 235000017557 sodium bicarbonate Nutrition 0.000 description 3
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 3
- 229920004934 Dacron® Polymers 0.000 description 2
- 229920002125 Sokalan® Polymers 0.000 description 2
- 229960001631 carbomer Drugs 0.000 description 2
- 239000000679 carrageenan Substances 0.000 description 2
- 235000010418 carrageenan Nutrition 0.000 description 2
- 229920001525 carrageenan Polymers 0.000 description 2
- 229940113118 carrageenan Drugs 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 239000000686 essence Substances 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 239000003205 fragrance Substances 0.000 description 2
- 239000013538 functional additive Substances 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- 125000001165 hydrophobic group Chemical group 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 239000005020 polyethylene terephthalate Substances 0.000 description 2
- 230000002265 prevention Effects 0.000 description 2
- 239000000523 sample Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 150000005846 sugar alcohols Polymers 0.000 description 2
- 230000008961 swelling Effects 0.000 description 2
- 230000002110 toxicologic effect Effects 0.000 description 2
- 231100000027 toxicology Toxicity 0.000 description 2
- 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 2
- 239000005995 Aluminium silicate Substances 0.000 description 1
- 206010051625 Conjunctival hyperaemia Diseases 0.000 description 1
- 206010010726 Conjunctival oedema Diseases 0.000 description 1
- 206010015946 Eye irritation Diseases 0.000 description 1
- 206010061218 Inflammation Diseases 0.000 description 1
- 241000588653 Neisseria Species 0.000 description 1
- 206010067482 No adverse event Diseases 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 239000003082 abrasive agent Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 231100000460 acute oral toxicity Toxicity 0.000 description 1
- 231100000403 acute toxicity Toxicity 0.000 description 1
- 230000007059 acute toxicity Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 235000012211 aluminium silicate Nutrition 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 1
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 1
- 229940105329 carboxymethylcellulose Drugs 0.000 description 1
- 210000000170 cell membrane Anatomy 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 210000004087 cornea Anatomy 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 208000002925 dental caries Diseases 0.000 description 1
- 238000000586 desensitisation Methods 0.000 description 1
- 230000003467 diminishing effect Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 231100000013 eye irritation Toxicity 0.000 description 1
- 210000000887 face Anatomy 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000013355 food flavoring agent Nutrition 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 230000023597 hemostasis Effects 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 230000004054 inflammatory process Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 230000010534 mechanism of action Effects 0.000 description 1
- 210000002200 mouth mucosa Anatomy 0.000 description 1
- 231100000286 mucous membrane, eye irritation or corrosion testing Toxicity 0.000 description 1
- 231100000344 non-irritating Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229940081974 saccharin Drugs 0.000 description 1
- 235000019204 saccharin Nutrition 0.000 description 1
- 239000000901 saccharin and its Na,K and Ca salt Substances 0.000 description 1
- 238000011076 safety test Methods 0.000 description 1
- 239000011265 semifinished product Substances 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 229940072774 sodium fluoride toothpaste Drugs 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000012430 stability testing Methods 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 230000004936 stimulating effect Effects 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 230000002087 whitening effect Effects 0.000 description 1
Images
Classifications
-
- 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
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/81—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
- A61K8/817—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen; Compositions or derivatives of such polymers, e.g. vinylimidazol, vinylcaprolactame, allylamines (Polyquaternium 6)
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/04—Acids; Metal salts or ammonium salts thereof
- C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F226/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen
- C08F226/02—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen by a single or double bond to nitrogen
-
- 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
- A61K2800/52—Stabilizers
Abstract
The application of the high polymer in improving the stability of toothpaste products is that the high polymer is prepared by acrylic acid and dimethyl diallyl ammonium chloride through aqueous solution polymerization or suspension polymerization, and the molecular weight of the high polymer is 500-2000 ten thousand of micro-crosslinking amphiphilic/associating type high polymer. The application method of the high molecular polymer comprises the following steps: (1) adding directly to a toothpaste system; or (2) dissolving in water to prepare a dilute solution preparation, and adding the dilute solution preparation into a toothpaste system; or (3) mixing with water and water-soluble humectant to obtain thickening component, and adding into toothpaste system; or (4) adding the high molecular polymer, an aqueous solution of the high molecular polymer, or a thickening component obtained by mixing the high molecular polymer with water and a water-soluble humectant as a consistency adjusting component to the produced toothpaste body to adjust the consistency of the toothpaste body. The high molecular polymer can improve the stability of the toothpaste system in the toothpaste system.
Description
Technical Field
The invention relates to the technical field of daily chemical industry, in particular to application of a high molecular polymer in improving stability of toothpaste products.
Background
Toothpaste is a daily necessity for cleaning teeth and protecting oral hygiene, and is usually a paste substance formed by mixing raw materials such as an abrasive, a humectant, a thickener, a foaming agent, a flavoring agent, water and other functional additives (effective components for improving oral health conditions).
With the increase of consumption level, the demands of consumers on the toothpaste are not only kept on the simple oral cavity cleaning level, but also the toothpaste with the effects of whitening, caries prevention, moth prevention, desensitization, inflammation diminishing, hemostasis and the like becomes a wind vane leading the future development of the toothpaste. Along with the diversification of consumer demands, various electrolytes, active substances and traditional Chinese medicine powder are added into the functional toothpaste, so that new challenges are brought to the stability of a toothpaste formula system; secondly, in the face of the increasingly strong competition, how to effectively improve the cost performance of the product and optimize the toothpaste process is a common problem faced by all toothpaste enterprises.
In order to improve the core competitiveness of enterprises, toothpaste manufacturers currently face the following four common industry demands:
stabilization requirement: in recent years, the requirements of consumers on the efficacy type toothpaste are higher and higher, and the stability of the traditional toothpaste system faces higher challenges after various salt components, active substance components and traditional Chinese medicine powder components are added; how to effectively improve the tolerance of the toothpaste system to the ingredients such as salts, active substances, traditional Chinese medicine powder and the like, ensure the quality of products and is a common requirement in the toothpaste industry.
The process requirement is as follows: how to avoid the problems of paste consistency fluctuation, paste swelling and the like caused by various reasons, improves the production efficiency of enterprises, and is a common requirement to be solved in the toothpaste industry. Firstly, in the toothpaste manufacturing process, the paste consistency is mainly provided by various thickening agents, but in the production process, when the paste consistency is disqualified such as thinner, the thickening agents cannot be directly added to adjust the paste consistency, and the common method is to adjust the paste consistency by supplementing a humectant, however, the thickening effect of the method is limited, and the paste has long-term stability and poor operability. Secondly, the toothpaste is a raw material kneading process, the thickening effect of various thickening agents cannot be completely expressed in the first time, the thickening agents are required to be placed for a period of time, the paste consistency can be maximized after the polymer chain segments are completely stretched, the macroscopic appearance is that the paste has a delayed expansion property (called as a stagnant expansion property), the stagnant expansion property can cause that the paste cannot be immediately filled after the paste is finished, the paste is required to be stored for 24-48 hours and then is detected to be qualified, and the filling is performed, so that a large pressure is formed on the continuity of production and the storage cost.
Cost requirements: in the face of vigorous industry competition, continuously increased production cost and social consumption to be vibrated, how to reduce the production cost of toothpaste and improve the product quality and profit is a common problem which needs to be solved by the toothpaste enterprises at present.
Application requirements: the application requirements of the toothpaste comprise rheological property, adhesion and dispersibility of the toothpaste, which affect the use feeling of consumers, and are important common indexes in the toothpaste industry. The good extrusion rheological property of the toothpaste is an important index for evaluating the quality of the toothpaste, and in the toothpaste production process, the too high consistency of a paste rack (measured by a rack consistometer) can cause the difficult operations of discharging, filling, extruding and the like of the toothpaste, thereby seriously affecting the production and use links of the product and reducing the use experience of consumers. The toothpaste has good adhesive force, is not easy to fall off from the toothbrush, and can bring better experience to consumers; the existing toothpaste of the calcium carbonate system has poor adhesion in winter and is easy to fall off from the toothbrush, thus influencing the use of the toothpaste by consumers. The toothpaste has good dispersibility in the oral cavity, is an important standard for measuring the toothpaste quality by consumers, is difficult to disperse and agglomerate in the oral cavity, and can seriously influence the product experience of consumers.
In summary, with the continuous development of the toothpaste industry, the common demands of stability, technology, cost, application and the like in the toothpaste industry are solved, so that the core competitiveness of enterprises can be effectively improved, and the method stands out in the vigorous market competition.
Disclosure of Invention
The technical problem to be solved by the invention is to provide an application of a high polymer in improving the stability of a toothpaste product, wherein the high polymer can improve the stability of the toothpaste system in the toothpaste system.
The application of the high molecular polymer in improving the stability of toothpaste products is characterized in that:
the high polymer is prepared by acrylic acid and dimethyl diallyl ammonium chloride through aqueous solution polymerization or suspension polymerization, and has a molecular weight of 500-2000 ten thousand;
the application method of the high molecular polymer comprises the following steps: (1) The high molecular polymer is directly added into a toothpaste system (the high molecular polymer is added in the form of a thickening agent according to the production process sequence of the toothpaste); or (2) diluting the high molecular polymer with water to prepare a dilute solution preparation, and adding the dilute solution preparation into a toothpaste system; or (3) mixing the high molecular polymer with water and water-soluble humectant (such as sorbitol, glycerol, etc.) to obtain thickening component, and adding into toothpaste system; or (4) adding the high molecular polymer, an aqueous solution of the high molecular polymer, or a thickening component obtained by mixing the high molecular polymer with water and a water-soluble humectant as a consistency adjusting component to the produced toothpaste body to adjust the consistency of the toothpaste body.
In the preferred scheme, the commodity name of the high polymer is micro-crosslinked polyquaternium MPQ-22 or micro-crosslinked polyquaternium SMPQ-22 (the average molecular weight of the SMPQ-22 is higher than that of the MPQ-22, and the high polymer has the advantages of improving the performances of system stability, thickening property, salt resistance, chinese herbal medicine resistance, active substance resistance and the like compared with that of the MPQ-22, the quality indexes of the high polymer are the same, the SMPQ-22 also has various performances of the MPQ-22, and is an upgrade product of the MPQ-22), and the high polymer is produced by Shandong Jitai new material science and technology development Co.
The mass indexes of the micro-crosslinked polyquaternium MPQ-22 and the micro-crosslinked polyquaternium SMPQ-22 are as follows:
in a preferred embodiment, the water is deionized water.
In a preferred embodiment, the polymer (such as micro-crosslinked polyquaternium MPQ-22 or micro-crosslinked polyquaternium SMPQ-22) is added to the toothpaste system in an amount of 0.05-5.0% by weight. More preferably, the polymer (such as micro-crosslinked polyquaternium MPQ-22 or micro-crosslinked polyquaternium SMPQ-22) is added to the toothpaste system in an amount of 0.4 to 2.0% by weight.
The toothpaste system is generally formed by mixing main raw materials such as an abrasive, a humectant, a thickener, a foaming agent, water and the like; on the basis of the above, aromatic and other functional additives (effective components for improving oral health condition such as salts, active substances and Chinese herbal medicine powder) can be added. In the process of preparing the toothpaste by utilizing the micro-crosslinked polyquaternium MPQ-22, the micro-crosslinked polyquaternium MPQ-22 can be used as a thickening agent (namely, replaces traditional thickening agents such as hydroxyethyl cellulose (HEC), carrageenan and carbomer) or part of the thickening agent (namely, replaces traditional thickening agents such as carboxymethyl cellulose (CMC), hydroxyethyl cellulose (HEC), carrageenan and carbomer).
The paste making process of the toothpaste body is generally divided into a wet paste making process and a dry paste making process.
When the wet method paste preparation process is adopted to prepare the toothpaste paste, the method comprises the following steps: (1a) Adding the high molecular polymer (such as micro cross-linked polyquaternium MPQ-22 or micro cross-linked polyquaternium SMPQ-22), humectant, other thickeners (if any), water soluble additives and the like into a paste making machine together, vacuumizing, stirring and homogenizing to obtain toothpaste slurry; (2a) Adding abrasive, foaming agent and other additives into the toothpaste slurry, and stirring uniformly to obtain toothpaste. In the case that the toothpaste further contains other ingredients such as saccharin sodium, sodium pyrophosphate, preservative, essence, pigment, salt, active substance, chinese herbal medicine powder and the like, the adding timing thereof can be determined according to the conventional industry, for example: sodium saccharin, sodium pyrophosphate, water soluble preservative, pigment may be in step (1 a); other preservatives, fragrances, actives, herbal powders and the like may be added to the toothpaste slurry in step (2 a) along with the abrasive.
In a preferred embodiment, after the toothpaste body is obtained in the step (2 a), the consistency of the toothpaste body is detected, if the consistency of the toothpaste body is insufficient, the high molecular polymer (such as micro-crosslinked polyquaternium MPQ-22 or micro-crosslinked polyquaternium SMPQ-22) is added into the toothpaste body, or the high molecular polymer (such as micro-crosslinked polyquaternium MPQ-22 or micro-crosslinked polyquaternium SMPQ-22) diluted by water or a water-soluble humectant is subjected to consistency adjustment until the consistency of the toothpaste body meets the requirements.
When the dry method paste preparation process is adopted to prepare the toothpaste paste, the method comprises the following steps: (1b) Adding the high molecular polymer (such as micro cross-linked polyquaternium MPQ-22 or micro cross-linked polyquaternium SMPQ-22), humectant, abrasive, foaming agent, preservative, water-soluble preparation and other thickening agent (if any) into a paste making machine together, vacuumizing, stirring and homogenizing to obtain a semi-finished product material body; (2b) And (3) adding other liquid additives, essence and the like through a flavoring port while maintaining the vacuum state, vacuumizing again, stirring and homogenizing to obtain the toothpaste. In the case that the toothpaste further contains other ingredients such as saccharin sodium, sodium pyrophosphate, preservative, essence, pigment, salt, active substance, chinese herbal medicine powder and the like, the adding timing thereof can be determined according to the conventional industry, for example: sodium saccharin, sodium pyrophosphate, pigment, salt, active substance, chinese herbal medicine powder, etc. can be added in the step (1 b); small molecule additives, actives, fragrances, etc. that are easily evacuated in vacuo may be added in step (2 b).
In a preferred embodiment, after the toothpaste body is obtained in the step (2 b), the consistency of the toothpaste body is detected, if the consistency of the toothpaste body is insufficient, the high molecular polymer (such as micro-crosslinked polyquaternium MPQ-22 or micro-crosslinked polyquaternium SMPQ-22) is added into the toothpaste body, or the high molecular polymer (such as micro-crosslinked polyquaternium MPQ-22 or micro-crosslinked polyquaternium SMPQ-22) diluted by water or a water-soluble humectant is subjected to consistency adjustment until the consistency of the toothpaste body meets the requirements.
The conventional toothpaste body mainly has the functions of thickening and stabilizing by absorbing water and swelling by a thickening agent (such as carboxymethyl cellulose (CMC), xanthan gum and the like), and the thickening agent is easy to change the water absorption coefficient along with the change of temperature, so that the phenomenon of excessive thickening (pipe expansion, hardening and the like) or thinning (flowing, water seepage, pipe separation and the like) of a product appears, and the product is macroscopically unstable; the toothpaste system containing the high molecular polymer (such as micro-crosslinked polyquaternium MPQ-22 or micro-crosslinked polyquaternium SMPQ-22) not only absorbs water and swells the high molecular polymer and reduces the fluidity of water phase in the system to play a role in thickening and stabilizing, but also fixes the relative position of powder in the toothpaste system by the interaction of the micro-crosslinked structure (space network, hydrogen bonding and association) of the high molecular polymer (such as micro-crosslinked polyquaternium MPQ-22 or micro-crosslinked polyquaternium SMPQ-22) and the surface charge of powder (friction agent), thereby achieving the aim of stabilizing the product and reducing the influence of temperature change on the product system. Even if electrolytes such as sodium chloride, sodium fluoride and the like or active substances such as holly bark extract, magnolia bark extract and the like are added into a toothpaste system containing the high molecular polymer (such as micro-crosslinked polyquaternium MPQ-22 or micro-crosslinked polyquaternium SMPQ-22), the toothpaste can be circulated for fifteen times at high and low temperatures (-25 to 50 ℃), water seepage is avoided, and the glossiness and the fineness of the paste are basically kept unchanged.
In addition, the toothpaste system constructed by the high molecular polymer (such as micro cross-linked poly quaternary ammonium salt MPQ-22) can meet the industry requirement of reducing the cost of toothpaste by reducing the dosage of humectant and thickener. Compared with the traditional toothpaste system (whether a silicon dioxide system or a calcium carbonate system), the toothpaste system constructed by the micro-crosslinked poly-quaternary ammonium salt MPQ-22 reduces the consumption of humectant and traditional toothpaste thickener, has higher toothpaste cost controllability, reduces the production cost, effectively improves the profits of toothpaste enterprises, shows excellent cost advantages, and solves the cost requirements of the toothpaste industry.
Drawings
FIG. 1 is a molecular weight distribution curve of the micro-crosslinked polyquaternium MPQ-22/SMPQ-22.
Detailed Description
EXAMPLE 1 SiO 2 Toothpaste (conventional system)
Raw material formula (% wt): 6.0% of hydrated silica (MIC type, zhaoqing Jin Sanjiang), 4.1% of hydrated silica (MIA type, zhaoqing Jin Sanjiang), 9.3% of hydrated silica (165 type, zhaoqing Jin Sanjiang), 10.0% of sorbitol (Lianyuangang Luo Gaite), 1.3% of micro-crosslinked poly-quaternary ammonium salt MPQ-22 (MPQ-22 of Shanzhi advanced New Material technology development Co., ltd., solid content of 60%), 2.5% of sodium lauryl sulfate, 3.0% of polyethylene glycol-400, 4.9% of Dow chemical, 0.9% of sodium carboxymethyl cellulose (Chongqing macro), 0.3% of tetrasodium pyrophosphate (Tianjin metallocene), 0.1% of saccharin sodium (Kappy), 0.15% of hydroxybenzoate (Beijing sangpi), 0.05% of hydroxypropyl ester (Kunshan double friends), 1.0% of essence and the balance of deionized water. The cost of the raw materials is about 5.0 yuan/KG.
The preparation method of the toothpaste body comprises the following steps:
1. dissolving saccharin sodium and tetrasodium pyrophosphate in deionized water, and pouring into a stirring pot;
2. adding sorbitol and hydrated silica (MIC type, MIA type, 165 type) into stirring pot, stirring, homogenizing for 5 min, and dispersing uniformly;
3. dispersing sodium carboxymethyl cellulose, methylparaben and propylparaben in polyethylene glycol-400, pouring into a stirring pot, stirring, homogenizing, and dispersing uniformly;
4. adding micro-crosslinking poly quaternary ammonium salt MPQ-22, stirring and homogenizing until the micro-crosslinking poly quaternary ammonium salt MPQ-22 is completely dissolved;
5. adding sodium laurylsulfate and essence, stirring, and homogenizing to obtain toothpaste.
Toothpaste bench consistency test:
consistency at normal temperature: instant consistency 15, 24h consistency 18,7d consistency 18,1 month consistency 18,2 month consistency 18.
15. Day cycle consistency (-25/50 ℃). 3d consistency 21,7d consistency 21, 15d consistency 21.
EXAMPLE 2 SiO 2 Toothpaste (JiuBiying toothpaste)
Raw material formula (% wt): 6.0% of hydrated silica (MIC type, zhaoqing Jin Sanjiang), 4.1% of hydrated silica (MIA type, zhaoqing Jin Sanjiang), 9.3% of hydrated silica (165 type, zhaoqing Jin Sanjiang), 1.0% of holly bark extract (Guangzhou hong), 10.0% of sorbitol (Liyun Kong Luo Gaite), 1.3% of micro-crosslinked poly-quaternary ammonium salt MPQ-22 (MPQ-22 of Shanzhi Jiedu new material technology development Co., ltd., solid content of 60%), 2.5% of sodium lauryl sulfate (Changzhi Australian), 3.0% of polyethylene glycol-400 (Dow chemical), 0.9% of carboxymethylcellulose sodium (Chongqing macro), 0.3% of tetrasodium pyrophosphate (Tianjin metallocene), 0.1% of saccharin sodium (Kappy), 0.15% of hydroxybenzoate (North Morgan, 0.05% of hydroxybenzoate (Kunshan Shuangyou), 1.0% of essence, and the balance deionized water. The cost of the raw materials is about 7.4 yuan/KG.
The preparation method of the toothpaste body comprises the following steps:
1. dissolving saccharin sodium and tetrasodium pyrophosphate in deionized water, and pouring into a stirring pot;
2. adding sorbitol, hydrated silica (MIC type, MIA type, 165 type) and cortex Ilicis Rotundae extract into stirring pot, stirring, homogenizing for 5 min, and dispersing uniformly;
3. dispersing sodium carboxymethyl cellulose, methylparaben and propylparaben in polyethylene glycol-400, pouring into a stirring pot, stirring, homogenizing, and dispersing uniformly;
4. adding micro-crosslinking poly quaternary ammonium salt MPQ-22, stirring and homogenizing until the micro-crosslinking poly quaternary ammonium salt MPQ-22 is completely dissolved;
5. adding sodium laurylsulfate and essence, stirring, and homogenizing to obtain toothpaste.
Toothpaste bench consistency test:
consistency at normal temperature: an immediate consistency of 15, a 24h consistency of 15, a 7d consistency of 15, a 1 month consistency of 15, a 2 month consistency of 15.
15. Day cycle consistency (-25/50 ℃). 3d consistency 18,7d consistency 18, 15d consistency 18.
EXAMPLE 3 SiO 2 Toothpaste (Magnolia officinalis toothpaste)
Raw material formula (% wt): 6.0% of hydrated silica (MIC type, zhaoqing Jin Sanjiang), 4.1% of hydrated silica (MIA type, zhaoqing Jin Sanjiang), 9.3% of hydrated silica (165 type, zhaoqing Jin Sanjiang), 0.2% of magnolia extract (Guangzhou Chengcheng Cheng), 40.0% of sorbitol (Lian Yungang Luo Gaite), 1.0% of micro-crosslinked poly-quaternary ammonium salt SMPQ-22 (SMPQ-22 of Shanzhao Jiechi new material technology development Co., ltd., solid content of which is 60%), 0.2% of xanthan gum (Nerngzhong), 2.5% of sodium lauryl sulfate (Changzhi Australiang), 0.3.0% of polyethylene glycol-400 (Dow chemical), 0.9% of carboxymethylcellulose sodium (Chongqing macro), 0.3% of tetrasodium pyrophosphate (Tianjin Dazu metallocene), 0.1% of saccharin sodium (Kappy chemical), 0.15% of hydroxybenzoate (Beijing mulberry), 0.05 (Kunshiyou), 1.0% of essence, and the balance of deionized water. The cost of raw materials is about 8.8 yuan/KG.
The preparation method of the toothpaste body comprises the following steps:
1. dissolving saccharin sodium and tetrasodium pyrophosphate in deionized water, and pouring into a stirring pot;
2. adding sorbitol, hydrated silica (MIC type, MIA type, 165 type) and Magnolia cortex extract into stirring pot, stirring, homogenizing for 5 min, and dispersing uniformly;
3. dispersing sodium carboxymethyl cellulose, methylparaben and propylparaben in polyethylene glycol-400, pouring into a stirring pot, stirring, homogenizing, and dispersing uniformly;
4. adding micro-crosslinked polyquaternium SMPQ-22, stirring and homogenizing until the mixture is completely dissolved;
5. adding sodium laurylsulfate and essence, stirring, and homogenizing to obtain toothpaste.
Toothpaste bench consistency test:
consistency at normal temperature: an immediate consistency of 12, a 24h consistency of 12, a 7d consistency of 12, a 1 month consistency of 15, a 2 month consistency of 15.
15. Day cycle consistency (-25/50 ℃). 3d consistency 15,7d consistency 15, 15d consistency 21.
EXAMPLE 4 SiO 2 Toothpaste (sodium fluoride toothpaste)
Raw material formula (% wt): 6.0% of hydrated silica (MIC type, zhaoqing Jin Sanjiang), 4.1% of hydrated silica (MIA type, zhaoqing Jin Sanjiang), 9.3% of hydrated silica (165 type, zhaoqing Jin Sanjiang), 0.2% of sodium fluoride (Shandong Gao Ming), 10.0% of sorbitol (Liyun Kong Luo Gaite), 1.5% of micro-crosslinked poly-quaternary ammonium salt MPQ-22 (MPQ-22 of Shanzhi advanced New Material science development Co., ltd., solid content of 60%), 2.5% of sodium lauryl sulfate (Changzhi Australian Ke), 3.0% of polyethylene glycol-400 (Dow chemical), 0.9% of carboxymethyl cellulose sodium (Chongqing macro), 0.3% of tetrasodium pyrophosphate (Tianjin metallocene), 0.1% of saccharin (Kappy), 0.15% of hydroxybenzoate (Beijing mulberry), 0.05% of hydroxypropyl ester (mountain double friends), 1.0% of essence and the balance deionized water. The cost of the raw materials is about 5.1 yuan/KG.
The preparation method of the toothpaste body comprises the following steps:
1. dissolving saccharin sodium and tetrasodium pyrophosphate in deionized water, and pouring into a stirring pot;
2. adding sorbitol, hydrated silica (MIC type, MIA type, 165 type) and sodium fluoride into a stirring pot, stirring, homogenizing for 5 min, and dispersing uniformly;
3. dispersing sodium carboxymethyl cellulose, methylparaben and propylparaben in polyethylene glycol-400, pouring into a stirring pot, stirring, homogenizing, and dispersing uniformly;
4. adding micro-crosslinking poly quaternary ammonium salt MPQ-22, stirring and homogenizing until the micro-crosslinking poly quaternary ammonium salt MPQ-22 is completely dissolved;
5. adding sodium laurylsulfate and essence, stirring, and homogenizing to obtain toothpaste.
Toothpaste bench consistency test:
consistency at normal temperature: an immediate consistency of 15, a 24h consistency of 15, a 7d consistency of 15, a 1 month consistency of 18, a 2 month consistency of 21.
15. Day cycle consistency (-25/50 ℃). 3d consistency 21,7d consistency 21, 15d consistency 24.
EXAMPLE 5 SiO 2 Toothpaste (sodium chloride toothpaste)
Raw material formula (% wt): 6.0% of hydrated silica (MIC type, zhaoqing Jin Sanjiang), 4.1% of hydrated silica (MIA type, zhaoqing Jin Sanjiang), 9.3% of hydrated silica (165 type, zhaoqing Jin Sanjiang), 1.0% of sodium chloride, 40.0% of sorbitol (Lianyuang Kong Luo Gaite), 1.5% of micro-crosslinked polyquaternium SMPQ-22 (solid content of SMPQ-22, shanzhi advanced New material technology development Co., ltd., 60%), 0.2% of xanthan gum (Neisseria, xuangzhong), 2.5% of sodium laurylsulfate (Du's Australiang), 3.0% of polyethylene glycol-400 (Dow chemical), 0.9% of carboxymethylcellulose (Chongqing macro), 0.3% of tetrasodium pyrophosphate (Tianjin metallocene), 0.1% of saccharin sodium (Kappy), 0.15% of methylparaben (Beijing mulberry), 0.05 (Kunshend), 1.0% of essence and the balance deionized water. The cost of the raw materials is about 6.2 yuan/KG.
The preparation method of the toothpaste body comprises the following steps:
1. dissolving saccharin sodium, tetrasodium pyrophosphate and sodium chloride in deionized water, and pouring into a stirring pot;
2. adding sorbitol and hydrated silica (MIC type, MIA type, 165 type) into stirring pot, stirring, homogenizing for 5 min, and dispersing uniformly;
3. dispersing sodium carboxymethyl cellulose, methylparaben and propylparaben in polyethylene glycol-400, pouring into a stirring pot, stirring, homogenizing, and dispersing uniformly;
4. adding micro-crosslinked polyquaternium SMPQ-22, stirring and homogenizing until the mixture is completely dissolved;
5. adding sodium laurylsulfate and essence, stirring, and homogenizing to obtain toothpaste.
Toothpaste bench consistency test:
consistency at normal temperature: instant consistency 15, 24h consistency 18,7d consistency 18,1 month consistency 18,2 month consistency 18.
15. Day cycle consistency (-25/50 ℃). 3d consistency 18,7d consistency 18, 15d consistency 18.
EXAMPLE 6 CaCO 3 Toothpaste (conventional system)
Raw material formula (% wt): 58.0 of calcium carbonate (Huasheng in West bay), 10.0 of sorbitol (Luo Gaite of Lian Yungang), 0.8 of micro-crosslinked poly-quaternary ammonium salt MPQ-22 (MPQ-22 of deep Tai new material science and technology development Co., ltd., the solid content of which is 60%), 2.1 of sodium lauryl sulfate (Changzhi Australian), 3.0 of polyethylene glycol-400, 3.0 of Dow chemical, 0.9 of sodium carboxymethyl cellulose (Chongqing force macro), 0.3 of tetrasodium pyrophosphate (Tianjin metallocene), 0.2 of saccharin sodium (Kaikovia ), 0.15 of hydroxybenzoate (Beijing sanpu), 0.05 of hydroxypropyl, 1.0 of essence and the balance of deionized water. The cost of the raw materials is about 2.4 yuan/KG.
The preparation method of the toothpaste body comprises the following steps:
1. dissolving saccharin sodium and tetrasodium pyrophosphate in deionized water, and pouring into a stirring pot;
2. adding sorbitol and calcium carbonate into a stirring pot, starting stirring, homogenizing for 5 minutes, and uniformly dispersing;
3. dispersing sodium carboxymethyl cellulose, methylparaben and propylparaben in polyethylene glycol-400, pouring into a stirring pot, stirring, homogenizing, and dispersing uniformly;
4. adding micro-crosslinking poly quaternary ammonium salt MPQ-22, stirring and homogenizing until the micro-crosslinking poly quaternary ammonium salt MPQ-22 is completely dissolved;
5. adding sodium laurylsulfate and essence, stirring, and homogenizing to obtain toothpaste.
Toothpaste bench consistency test:
consistency at normal temperature: instant consistency 9, 24h consistency 12,7d consistency 15.
15. Day cycle consistency (-25/50 ℃). 3d consistency 15,7d consistency 18, 15d consistency 21.
EXAMPLE 7 CaCO 3 Toothpaste (Magnolia officinalis toothpaste)
Raw material formula (% wt): 58.0 of calcium carbonate (Huasheng in West bay), 10.0 of sorbitol (Luo Gaite of Lian Yungang), 0.8 of micro-crosslinked poly-quaternary ammonium salt MPQ-22 (MPQ-22 of deep Tai new material science development Co., ltd., the solid content of which is 60%), 2.1 of sodium lauryl sulfate (Changzhi Australian), 400.0 of polyethylene glycol (Dow chemical), 0.9 of sodium carboxymethylcellulose (Chongqing Lihong), 0.3 of tetrasodium pyrophosphate (Tianjin metallocene), 0.2 of saccharin sodium (Kaikovia), 0.2 of magnolia extract (Guangzhou hongzhou), 0.15 of hydroxybenzoate (Beijing sangpu), 0.05 of hydroxypropyl (Kunshan double friends), 1.0 of essence and the balance of deionized water. The cost of the raw materials is about 5.0 yuan/KG.
The preparation method of the toothpaste body comprises the following steps:
1. dissolving saccharin sodium and tetrasodium pyrophosphate in deionized water, and pouring into a stirring pot;
2. adding sorbitol, calcium carbonate and cortex Magnolia officinalis extract into stirring pot, stirring, homogenizing for 5 min, and dispersing uniformly;
3. dispersing sodium carboxymethyl cellulose, methylparaben and propylparaben in polyethylene glycol-400, pouring into a stirring pot, stirring, homogenizing, and dispersing uniformly;
4. adding micro-crosslinking poly quaternary ammonium salt MPQ-22, stirring and homogenizing until the micro-crosslinking poly quaternary ammonium salt MPQ-22 is completely dissolved;
5. adding sodium laurylsulfate and essence, stirring, and homogenizing to obtain toothpaste.
Toothpaste bench consistency test:
consistency at normal temperature: instant consistency 9, 24h consistency 12,7d consistency 15.
15. Day cycle consistency (-25/50 ℃). 3d consistency 18,7d consistency 18, 15d consistency 21.
EXAMPLE 8 CaCO 3 Toothpaste (JiuBiying toothpaste)
Raw material formula (% wt): 58.0 of calcium carbonate (Siwan Huasheng), 25.0 of sorbitol (Lian Yungang Luo Gaite), 0.8 of micro-crosslinked polyquaternium SMPQ-22 (SMPQ-22 of Shandou Jitai new material science and technology development Co., ltd., solid content of which is 60%), 2.1 of sodium lauryl sulfate (Changzhi Australian Nike), 400.0 of polyethylene glycol-400 (Dow chemical), 0.6 of sodium carboxymethyl cellulose (Chongqing Lihong), 0.2 of xanthan gum (Nernzhong Xuang), 0.3 of tetrasodium pyrophosphate (Tianjin Dacron), 0.2 of saccharin sodium (Kaschin Kangzhi), 1.0 of cortex holly extract (Guangzhong Chengcheng Cheng), 0.15 of hydroxybenzoate (North Morgan Praeparata), 0.05 of hydroxybenzoate (Kunshan Shuangyou), 1.0 of essence and the balance of deionized water. The cost of the raw materials is about 5.5 yuan/KG.
The preparation method of the toothpaste body comprises the following steps:
1. dissolving saccharin sodium and tetrasodium pyrophosphate in deionized water, and pouring into a stirring pot;
2. adding sorbitol, calcium carbonate and cortex Ilicis Rotundae extract into stirring pot, stirring, homogenizing for 5 min, and dispersing uniformly;
3. dispersing sodium carboxymethyl cellulose, methylparaben and propylparaben in polyethylene glycol-400, pouring into a stirring pot, stirring, homogenizing, and dispersing uniformly;
4. adding micro-crosslinked polyquaternium SMPQ-22, stirring and homogenizing until the mixture is completely dissolved;
5. adding sodium laurylsulfate and essence, stirring, and homogenizing to obtain toothpaste.
Toothpaste bench consistency test:
consistency at normal temperature: instant consistency 9, 24h consistency 15,7d consistency 18.
15. Day cycle consistency (-25/50 ℃). 3d consistency 18,7d consistency 21, 15d consistency 24.
EXAMPLE 9 CaCO 3 Toothpaste (travel product toothpaste 1)
Raw material formula (% wt): 62.0 percent of calcium carbonate (Huasheng in West bay), 8.0 percent of sorbitol (Luo Gaite percent of Lian Yungang), 0.7 percent of micro-crosslinked poly-quaternary ammonium salt MPQ-22 (MPQ-22 of Shandong Jitai new material science and technology development Co., ltd., solid content of 60 percent), 1.0 percent of sodium lauryl sulfate (Changzhi Australian), 3.0 percent of polyethylene glycol-400, 7 percent of sodium carboxymethyl cellulose (Chongqing macro), 0.3 percent of tetrasodium pyrophosphate (Tianjin, metallocene), 0.2 percent of saccharin sodium (Kaikovia, kyowa), 0.15 percent of hydroxybenzoate, 0.05 percent of hydroxypropyl, 0.5 percent of essence, and the balance of deionized water. The cost of the raw materials is about 2.1 yuan/KG.
The preparation method of the toothpaste body comprises the following steps:
1. dissolving saccharin sodium and tetrasodium pyrophosphate in deionized water, and pouring into a stirring pot;
2. adding sorbitol and calcium carbonate into a stirring pot, starting stirring, homogenizing for 5 minutes, and uniformly dispersing;
3. dispersing sodium carboxymethyl cellulose, methylparaben and propylparaben in polyethylene glycol-400, pouring into a stirring pot, stirring, homogenizing, and dispersing uniformly;
4. adding micro-crosslinking poly quaternary ammonium salt MPQ-22, stirring and homogenizing until the micro-crosslinking poly quaternary ammonium salt MPQ-22 is completely dissolved;
5. adding sodium laurylsulfate and essence, stirring, and homogenizing to obtain toothpaste.
Toothpaste bench consistency test:
consistency at normal temperature: instant consistency 9, 24h consistency 12,7d consistency 15.
15. Day cycle consistency (-25/50 ℃). 3d consistency 21,7d consistency 24, 15d consistency 24.
EXAMPLE 10 CaCO 3 Toothpaste (travel product toothpaste 2)
Raw material formula (% wt): calcium carbonate 62.0 (Siwan Huasheng), sorbitol 8.0 (Lian Yungang Luo Gaite), micro-crosslinked polyquaternium SMPQ-22.7 (SMPQ-22 of Shandou Jitai new material science and technology development Co., ltd., solid content of which is 60%), xanthan gum 0.2 (Nemongzhong Xuang), sodium lauryl sulfate 0.5 (Changzhi Aonike), polyethylene glycol-400.0 (Dow chemical), sodium carboxymethylcellulose 0.7 (Chongqing Lihong), tetrasodium pyrophosphate 0.3 (Tianjin Dacron), saccharin sodium 0.1 (Kaikui), hydroxybenzoate 0.15 (Beijing sangpi), hydroxypropyl 0.05 (Kunshan Shuangyou), essence 0.25, and the balance deionized water. The cost of the raw materials is about 2.0 yuan/KG.
The preparation method of the toothpaste body comprises the following steps:
1. dissolving saccharin sodium and tetrasodium pyrophosphate in deionized water, and pouring into a stirring pot;
2. adding sorbitol and calcium carbonate into a stirring pot, starting stirring, homogenizing for 5 minutes, and uniformly dispersing;
3. dispersing sodium carboxymethyl cellulose, methylparaben and propylparaben in polyethylene glycol-400, pouring into a stirring pot, stirring, homogenizing, and dispersing uniformly;
4. adding micro-crosslinked polyquaternium SMPQ-22, stirring and homogenizing until the mixture is completely dissolved;
5. adding sodium laurylsulfate and essence, stirring, and homogenizing to obtain toothpaste.
Toothpaste bench consistency test:
consistency at normal temperature: instant consistency 9, 24h consistency 12,7d consistency 15.
15. Day cycle consistency (-25/50 ℃). 3d consistency 21,7d consistency 24, 15d consistency over 36.
EXAMPLE 11 transparent toothpaste
Raw material formula (% wt): 6.0% of hydrated silica (MIC type, zhaoqing Jin Sanjiang), 4.1% of hydrated silica (MIA type, zhaoqing Jin Sanjiang), 9.3% of hydrated silica (165 type, zhaoqing Jin Sanjiang), 65.0% of sorbitol (Lianyuangang Luo Gaite), 0.4% of micro-crosslinked poly-quaternary ammonium salt MPQ-22 (MPQ-22 of Shanzhi advanced New Material science development Co., ltd., solid content of 60%), 2.5% of sodium lauryl sulfate, 3.0% of polyethylene glycol-400, 4% of Dow chemical, 0.4% of sodium carboxymethyl cellulose (Chongqing macro), 0.3% of tetra sodium pyrophosphate (Tianjin metallocene), 0.1% of saccharin sodium (Kappy), 0.15% of hydroxy benzyl ester (Beijing sangpi), 0.05% of hydroxy propyl ester (Kunshan double friends), 1.0 of essence and the balance of deionized water. The cost of the raw materials is about 6.4 yuan/KG.
The preparation method of the toothpaste body comprises the following steps:
1. dissolving saccharin sodium and tetrasodium pyrophosphate in deionized water, and pouring into a stirring pot;
2. adding sorbitol and hydrated silica (MIC type, MIA type, 165 type) into stirring pot, stirring, homogenizing for 5 min, and dispersing uniformly;
3. dispersing sodium carboxymethyl cellulose, methylparaben and propylparaben in polyethylene glycol-400, pouring into a stirring pot, stirring, homogenizing, and dispersing uniformly;
4. adding micro-crosslinking poly quaternary ammonium salt MPQ-22, stirring and homogenizing until the micro-crosslinking poly quaternary ammonium salt MPQ-22 is completely dissolved;
5. adding sodium laurylsulfate and essence, stirring, and homogenizing to obtain toothpaste.
Toothpaste bench consistency test:
consistency at normal temperature: an immediate consistency of 12, a 24h consistency of 12, a 7d consistency of 12, a 1 month consistency of 15, a 2 month consistency of 15.
15. Day cycle consistency (-25/50 ℃). 3d consistency 12,7d consistency 12, 15d consistency 15.
Comparative example 1 (cost comparison)
1. Silica system:
raw material formula (% wt) of MPQ-22 silica toothpaste is: 6.0% of hydrated silica (MIC type, zhaoqing Jin Sanjiang), 4.1% of hydrated silica (MIA type, zhaoqing Jin Sanjiang), 9.3% of hydrated silica (165 type, zhaoqing Jin Sanjiang), 10.0% of sorbitol (Lianyuangang Luo Gaite), 1.3% of micro-crosslinked poly-quaternary ammonium salt MPQ-22 (MPQ-22 of Shanzhi advanced New Material technology development Co., ltd., solid content of 60%), 2.5% of sodium lauryl sulfate, 3.0% of polyethylene glycol-400, 4.9% of Dow chemical, 0.9% of sodium carboxymethyl cellulose (Chongqing macro), 0.3% of tetrasodium pyrophosphate (Tianjin metallocene), 0.1% of saccharin sodium (Kappy), 0.15% of hydroxybenzoate (Beijing sangpi), 0.05% of hydroxypropyl ester (Kunshan double friends), 1.0% of essence and the balance of deionized water. The cost of the raw materials is about 5.0 yuan/KG.
Traditional silica toothpaste raw material formula (% wt): silica hydrate (MIC type, cultellum Jin Sanjiang) 6.0, silica hydrate (MIA type, cultellum Jin Sanjiang) 4.1, silica hydrate (165 type, cultellum Jin Sanjiang) 9.3, sorbitol 50.0 (harbour Luo Gaite), xanthan gum 0.6, sodium lauryl sulfate 2.5 (changii australian), polyethylene glycol-400.0 (dow chemical), sodium carboxymethylcellulose 0.9 (Chongqing macro), tetrasodium pyrophosphate 0.3 (Tianjin metallocene), sodium saccharin 0.1 (Kaolin macro), methylparaben 0.15 (Beijing sangpu), propylparaben 0.05 (kunshan double friends), essence 1.0, the balance deionized water. The cost of the raw materials is about 5.7 yuan/KG.
2. Calcium carbonate system:
raw material formula (% wt) of MPQ-22 calcium carbonate toothpaste comprises: 58.0 of calcium carbonate (Huasheng in West bay), 10.0 of sorbitol (Luo Gaite of Lian Yungang), 0.9 of micro-crosslinked poly-quaternary ammonium salt SMPQ-22 (SMPQ-22 of deep Tai new material science development Co., ltd., solid content of 60 percent), 2.1 of sodium lauryl sulfate (Changzhi Australian), 3.0 of polyethylene glycol-400 (Dow chemical), 0.9 of sodium carboxymethyl cellulose (Chongqing macro), 0.3 of tetrasodium pyrophosphate (Tianjin metallocene), 0.2 of saccharin sodium (Kaikovia), 0.15 of hydroxybenzoate (Beijing Sangpu), 0.05 of hydroxypropyl, 1.0 of essence and the balance of deionized water. The cost of the raw materials is about 2.4 yuan/KG.
Traditional calcium carbonate toothpaste raw material formula (% wt): calcium carbonate 42.0 (Cefzian Huashen), hydrated silica (thickening) 10, sorbitol 25.0 (Liyun Kong Luo Gaite), xanthan gum 0.5, sodium lauryl sulfate 2.1 (Changzhi Australian), polyethylene glycol-400.0 (Dow chemical), sodium carboxymethylcellulose 1.0 (Chongqing Lihong), tetrasodium pyrophosphate 0.3 (Tianjin metallocene), saccharin sodium 0.2 (Kaifeng), methylparaben 0.15 (Beijing Sangpu), propylparaben 0.05 (Kunshan double friends), essence 1.0 and the balance deionized water. The cost of the raw materials is about 3.6 yuan/KG.
Compared with the traditional toothpaste system (whether a silicon dioxide system or a calcium carbonate system), the formula system of the MPQ-22/SMPQ-22 toothpaste containing the micro-crosslinked polyquaternary ammonium salt greatly reduces the dosage of humectant (such as sorbitol) and traditional toothpaste thickener (such as xanthan gum), has higher toothpaste cost controllability and lower production cost, effectively improves the profits of toothpaste enterprises, shows excellent cost advantages, and solves the cost requirements of the toothpaste industry.
Comparative example 2 (comparative skeleton Property)
The traditional toothpaste system does not contain micro-crosslinked polyquaternary ammonium salt MPQ-22, and the raw material ratio of the traditional toothpaste system is (% wt): silica hydrate (MIC type, culprit Jin Sanjiang) 6.0, silica hydrate (MIA type, culprit Jin Sanjiang) 4.1, silica hydrate (165 type, culprit Jin Sanjiang) 9.3, sorbitol 10.0 (harbour Luo Gaite), sodium lauryl sulfate 2.5 (changii australian), polyethylene glycol-400.0 (dow chemical), sodium carboxymethylcellulose 0.9 (Chongqing macro), tetrasodium pyrophosphate 0.3 (Tianjin metallocene), sodium saccharin 0.1 (Kaschin), methylparaben 0.15 (Beijing sangpu), propylparaben 0.05 (Kunshan), essence 1.0, the balance deionized water. The traditional toothpaste system is an integral framework structure formed by the combined action of inorganic matters, thickening agents and a large amount of polyalcohols and the action of hydrogen bonds and interfacial charges, and the three raw materials are indispensable. The amount of sorbitol added to the conventional silica toothpaste of comparative example 1 was reduced from 50.0% to 10.0%, and the toothpaste could not be shaped when extruded without the addition of xanthan gum.
The formula system of the MPQ-22 toothpaste containing the micro-crosslinked polyquaternary ammonium salt comprises the following raw materials in percentage by weight: 6.0% of hydrated silica (MIC type, zhaoqing Jin Sanjiang), 4.1% of hydrated silica (MIA type, zhaoqing Jin Sanjiang), 9.3% of hydrated silica (165 type, zhaoqing Jin Sanjiang), 10.0% of sorbitol (Lianyuangang Luo Gaite), 1.3% of micro-crosslinked poly-quaternary ammonium salt MPQ-22 (MPQ-22 of Shanzhi advanced New Material technology development Co., ltd., solid content of 60%), 2.5% of sodium lauryl sulfate, 3.0% of polyethylene glycol-400, 4.9% of Dow chemical, 0.9% of sodium carboxymethyl cellulose (Chongqing macro), 0.3% of tetrasodium pyrophosphate (Tianjin metallocene), 0.1% of saccharin sodium (Kappy), 0.15% of hydroxybenzoate (Beijing sangpi), 0.05% of hydroxypropyl ester (Kunshan double friends), 1.0% of essence and the balance of deionized water. The micro-crosslinking poly quaternary ammonium salt MPQ-22 is introduced into the traditional toothpaste system, and the novel toothpaste framework structure is jointly constructed by hydrogen bonding, hydrophobic association and interfacial charge, so that the consumption of the humectant sorbitol is greatly reduced, the whole framework structure of the toothpaste is still stiff, cannot collapse, and has excellent long-term stability.
Test example (Performance test of micro-crosslinked Polyquaternium MPQ-22)
Sources of micro-crosslinked polyquaternium MPQ-22: MPQ-22, CAS NO. 53694-17-0, a new material technology development Co., ltd.); SMPQ-22, CAS No. 7732-18-5, a new material technology development Co., ltd. SMPQ-22 is an upgrade of MPQ-22, has stronger association and more excellent stability, and has the same quality index, and the SMPQ-22 is also suitable for and protected by the scheme of the invention. Referring to FIG. 1, the main difference between SMPQ-22 and MPQ-22 is that SMPQ-22 has a higher average molecular weight than MPQ-22.
1. Safety performance test
1. Toxicological safety performance
The testing method comprises the following steps: according to 2015 edition of cosmetic safety technical Specification.
The results of the toxicological safety test on MPQ-22 are shown in Table 1 below:
TABLE 1 acute oral toxicity test results
Conclusion of the test: according to the acute toxicity classification, LD50 is more than 5000mg/kg, which belongs to the actual non-toxic grade.
MPQ-22/SMPQ-22 are all micro-crosslinking functional high molecular polymers, and can not be decomposed in a short time, and can not penetrate cell membranes to be absorbed by human bodies, so that no toxic effect can be generated on the human bodies, and the product has extremely high use safety coefficient.
2. Stimulating safety performance
The testing method comprises the following steps: according to 2015 edition of cosmetic safety technical Specification.
The results of the stimulus safety performance test for MPQ-22 are shown in Table 2 below:
TABLE 2 results of acute ocular irritation test
The mean of individual animal integral refers to the mean integral of each animal over three different observation times (24 h, 48h, and 72 h) in terms of cornea, iris, conjunctival congestion, conjunctival edema (i.e., the sum of the 24h, 48h, and 72h scores of each animal divided by the number of points at observation 3)
Conclusion of the test: acute eye irritation with MPQ-22 is non-irritating.
The acute eye irritation test is carried out on the MPQ-22 to replace the oral mucosa irritation test, so that the MPQ-22 is proved to have excellent safety performance without any irritation. SMPQ-22 has the same structure as MPQ-22 except that the molecular weight distribution is different, and the SMPQ-22 does not bring any irritation, and has very excellent safety performance.
2. Stability test
1. Mechanism of action of micro-crosslinked polyquaternium MPQ-22/SMPQ-22
The action mechanism of the micro-crosslinking poly quaternary ammonium salt MPQ-22/SMPQ-22 comprises covalent bond blocking, charge blocking and association blocking:
(1) Covalent bond blocking: the micro-crosslinked polyquaternary ammonium salt MPQ-22/SMPQ-22 has a space three-dimensional network structure, and the micro-crosslinked network main chain structure (covalent bond) can suspend solid raw materials (such as abradant, traditional Chinese medicine powder and the like) in the system and simultaneously obstruct the possibility of agglomeration of powder raw materials. The micro-crosslinking poly quaternary ammonium salt MPQ-22/SMPQ-22 main chain can form stable hydrogen bond with carboxymethyl cellulose (CMC) and polyalcohol to form the framework structure of the toothpaste system together.
(2) Charge blocking: the specific surface area of the commonly used solid raw materials (abrasive agent, chinese herbal medicine powder and the like) is large, and the surface of the solid raw materials has a large amount of negative charges due to the action of static electricity. The main chain of the micro-crosslinked polyquaternary ammonium salt MPQ-22/SMPQ-22 has positive charges and negative charges at the same time, wherein the groups with positive charges can be automatically loaded and adsorbed on the surface of the solid raw material, so that the suspending capability of the solid raw material is enhanced.
(3) Association barrier: the micro-crosslinking poly quaternary ammonium salt MPQ-22/SMPQ-22 has long side chain hydrophobic groups, and a large number of hydrophobic groups are aggregated by Van der Waals force to generate association to form association areas. The associated areas are relatively soft, enhancing the flexibility of the toothpaste system. Even under extreme conditions such as high temperature (50 ℃), low temperature (5 ℃) and freezing (-25 ℃), the flexibility of the toothpaste system can be maintained, and the stability of the toothpaste is greatly improved.
The covalent bond separation, the charge separation and the association separation are combined to ensure that the micro-crosslinked polyquaternium MPQ-22/SMPQ-22 has excellent skeleton property and stability, and can improve the stability of a toothpaste system.
2. Toothpaste formula stability testing method
Based on the research on the cosmetic stability test method, a stability test method was formulated.
The requirements are: in the test process, the appearance of the material body is not unstable, such as coarsening, water diversion, shelling, water seepage at a pipe orifice and the like, and the material body is restored to the room temperature and is basically consistent with the appearance of the material body placed at the room temperature; the shearing of the sample after the stability test is basically consistent with the appearance of the sample material at normal temperature.
3. The stability test was passed on all the toothpaste pastes prepared in examples 1-11 above, and it was confirmed that MPQ-22/SMPQ-22 could improve the stability of the toothpaste product.
4. Salt tolerance stability
4-1. In the new MPQ-22 silica toothpaste system, 7.0% sodium chloride, 4.0% sodium bicarbonate and 0.2% sodium fluoride are added respectively to test the salt tolerance of the paste.
The basic raw material formula (% wt) of the novel MPQ-22 silica toothpaste system comprises the following components: 19.4 parts of hydrated silica, 10.0 parts of sorbitol, 1.3 parts of micro-crosslinked poly quaternary ammonium salt MPQ-22 (MPQ-22 of advanced new material science and technology development Co., ltd., solid content of which is 60%), 2.5 parts of sodium lauryl sulfate, 3.0 parts of polyethylene glycol-400, 0.9 parts of sodium carboxymethyl cellulose, 0.3 parts of tetrasodium pyrophosphate, 0.1 part of saccharin sodium, 0.15 parts of methylparaben, 0.05 parts of propylparaben, 1.0 part of essence and the balance of deionized water.
Based on the basic raw material formula, 7.0% sodium chloride, 4.0% sodium bicarbonate and 0.2% sodium fluoride are added respectively to obtain a novel MPQ-22 silica toothpaste system containing salt.
The three novel MPQ-22 silica toothpaste systems containing salt are subjected to high-low temperature cycle test for 15 days, the appearance of the toothpaste is fine and smooth and glossy, and the appearance of the toothpaste is basically consistent with that of the toothpaste placed at normal temperature, so that the novel MPQ-22 silica toothpaste system has excellent salt tolerance.
4-2. In the novel SMPQ-22 silica toothpaste system, 7.0% sodium chloride, 4.0% sodium bicarbonate, and 0.2% sodium fluoride were added, respectively, to test the salt tolerance of the paste.
The basic raw material formula (% wt) of the novel SMPQ-22 silica toothpaste system comprises: 19.4 parts of hydrated silica, 40.0 parts of sorbitol, 1.0 part of micro-crosslinked poly quaternary ammonium salt SMPQ-22 (the solid content of the micro-crosslinked poly quaternary ammonium salt SMPQ-22 is 60% of the advanced technology development of new materials, co., ltd.), 0.2 parts of xanthan gum, 2.5 parts of sodium lauryl sulfate, 3.0 parts of polyethylene glycol-400, 0.6 parts of sodium carboxymethyl cellulose, 0.3 parts of tetrasodium pyrophosphate, 0.1 part of saccharin sodium, 0.15 parts of methylparaben, 0.05 parts of propylparaben, 1.0 part of essence and the balance of deionized water.
Based on the basic raw material formula, 7.0% sodium chloride, 4.0% sodium bicarbonate and 0.2% sodium fluoride are added respectively to obtain the novel salty SMPQ-22 silica toothpaste system.
The three novel salty SMPQ-22 silica toothpaste systems are subjected to 15-day high-low temperature cycle test, the appearance of the toothpaste is fine and smooth and glossy, and the toothpaste is basically consistent with the toothpaste placed at normal temperature, so that the novel SMPQ-22 silica toothpaste system has excellent salt tolerance.
5. Stability against active substances
5-1. In the novel MPQ-22 silica toothpaste system, 1% of cortex Ilicis Rotundae extract and 0.2% of cortex Magnolia officinalis extract are respectively added, and the tolerance of the toothpaste system to active substances is tested.
The basic raw material formula (% wt) of the novel MPQ-22 silica toothpaste system comprises the following components: 19.4 parts of hydrated silica, 10.0 parts of sorbitol, 1.3 parts of micro-crosslinked poly quaternary ammonium salt MPQ-22 (MPQ-22 of advanced new material science and technology development Co., ltd., solid content of which is 60%), 2.5 parts of sodium lauryl sulfate, 3.0 parts of polyethylene glycol-400, 0.9 parts of sodium carboxymethyl cellulose, 0.3 parts of tetrasodium pyrophosphate, 0.1 part of saccharin sodium, 0.15 parts of methylparaben, 0.05 parts of propylparaben, 1.0 part of essence and the balance of deionized water. On the basis of the basic raw material formula, 1% of holly bark extract and 0.2% of magnolia bark extract are added respectively to obtain a toothpaste system containing the holly bark extract or the magnolia bark extract.
5-2, respectively adding 1% of cortex rotundae officinalis extract and 0.2% of cortex magnoliae officinalis extract into a novel MPQ-22 calcium carbonate toothpaste system, and testing the tolerance of the toothpaste system to active substances.
The basic raw material formula (% wt) of the novel MPQ-22 calcium carbonate toothpaste system comprises the following components: 58.0 parts of calcium carbonate, 10.0 parts of sorbitol, 1.3 parts of micro-crosslinked poly-quaternary ammonium salt MPQ-22 (MPQ-22 of new material technology development Co., ltd., shandou Jitai, solid content of 60%), 2.1 parts of sodium lauryl sulfate, 3.0 parts of polyethylene glycol-400, 0.9 parts of sodium carboxymethyl cellulose, 0.3 parts of tetrasodium pyrophosphate, 0.1 parts of saccharin sodium, 0.05 parts of propyl hydroxybenzoate, 1.0 parts of essence and the balance of deionized water. On the basis of the basic raw material formula, 1% of holly bark extract and 0.2% of magnolia bark extract are added respectively to obtain a toothpaste system containing the holly bark extract or the magnolia bark extract.
5-3. To the novel SMPQ-22 silica toothpaste system, 1% of the cortex Ilicis Rotundae extract and 0.2% of the Magnolia officinalis extract were added respectively, and the tolerance of the toothpaste system to active substances was tested.
The basic raw material formula (% wt) of the novel SMPQ-22 silica toothpaste system comprises: 19.4 parts of hydrated silica, 40.0 parts of sorbitol, 1.0 part of micro-crosslinked poly quaternary ammonium salt SMPQ-22 (the solid content of the micro-crosslinked poly quaternary ammonium salt SMPQ-22 is 60% of the advanced technology development of new materials, co., ltd.), 0.2 parts of xanthan gum, 2.5 parts of sodium lauryl sulfate, 3.0 parts of polyethylene glycol-400, 0.6 parts of sodium carboxymethyl cellulose, 0.3 parts of tetrasodium pyrophosphate, 0.1 part of saccharin sodium, 0.15 parts of methylparaben, 0.05 parts of propylparaben, 1.0 part of essence and the balance of deionized water. On the basis of the basic raw material formula, 1% of holly bark extract and 0.2% of magnolia bark extract are added respectively to obtain a toothpaste system containing the holly bark extract or the magnolia bark extract.
5-4. To the novel SMPQ-22 calcium carbonate toothpaste system, 1% of cortex Ilicis Rotundae extract and 0.2% of cortex Magnolia officinalis extract were added respectively, and the tolerance of the toothpaste system to active substances was tested.
The basic raw material formula (% wt) of the novel SMPQ-22 calcium carbonate toothpaste system comprises the following components: 58.0 parts of calcium carbonate, 25.0 parts of sorbitol, 1.3 parts of micro-crosslinked poly quaternary ammonium salt SMPQ-22 (the solid content of the micro-crosslinked poly quaternary ammonium salt SMPQ-22 is 60% of Shandong Jitai new material science and development Co., ltd.), 0.2 parts of xanthan gum, 2.1 parts of sodium lauryl sulfate, 3.0 parts of polyethylene glycol-400, 0.6 parts of sodium carboxymethylcellulose, 0.3 parts of tetrasodium pyrophosphate, 0.1 part of saccharin sodium, 0.05 parts of propyl hydroxybenzoate, 1.0 part of essence and the balance of deionized water. On the basis of the basic raw material formula, 1% of holly bark extract and 0.2% of magnolia bark extract are added respectively to obtain a toothpaste system containing the holly bark extract or the magnolia bark extract.
Through tests, the MPQ-22/SMPQ-22 silicon dioxide toothpaste system and the MPQ-22/SMPQ-22 calcium carbonate toothpaste system paste containing active ingredients such as the cortex holly bark extract and the magnolia bark extract can not have unstable phenomena such as water diversion, oil diversion, shelling, coarseness and the like. The novel MPQ-22/SMPQ-22 silica toothpaste system and the novel MPQ-22/SMPQ-22 calcium carbonate toothpaste system have strong tolerance performance to various active substances.
6. Stability of refractory Chinese medicine powder
6-1, adding different types of traditional Chinese medicine powder into a novel MPQ-22 silica system respectively, testing the stability of toothpaste, and verifying the tolerance of the novel MPQ-22 silica toothpaste system to different traditional Chinese medicine powder.
The basic raw material formula (% wt) of the novel MPQ-22 silica toothpaste system comprises the following components: 19.4 parts of hydrated silica, 10.0 parts of sorbitol, 1.0 part of micro-crosslinked poly quaternary ammonium salt MPQ-22 (MPQ-22 of advanced materials science and technology development Co., ltd., solid content of which is 60%), 2.5 parts of sodium lauryl sulfate, 3.0 parts of polyethylene glycol-400, 0.9 parts of sodium carboxymethyl cellulose, 0.3 parts of tetrasodium pyrophosphate, 0.1 part of saccharin sodium, 0.15 parts of methylparaben, 0.05 parts of propylparaben, 1.0 part of essence and the balance of deionized water. Based on the basic raw material formula, 1 wt% of traditional Chinese medicine powder is added.
6-2, respectively adding different types of traditional Chinese medicine powder into the novel MPQ-22 calcium carbonate toothpaste system, testing the stability of the toothpaste, and verifying the tolerance of the novel MPQ-22 calcium carbonate toothpaste system to different traditional Chinese medicine powder.
The basic raw material formula (% wt) of the novel MPQ-22 calcium carbonate toothpaste system comprises the following components: 58.0 parts of calcium carbonate, 10.0 parts of sorbitol, 1.3 parts of micro-crosslinked poly-quaternary ammonium salt MPQ-22 (MPQ-22 of new material technology development Co., ltd., shandou Jitai, solid content of 60%), 2.1 parts of sodium lauryl sulfate, 3.0 parts of polyethylene glycol-400, 0.9 parts of sodium carboxymethyl cellulose, 0.3 parts of tetrasodium pyrophosphate, 0.2 parts of saccharin sodium, 0.05 parts of propyl hydroxybenzoate, 1.0 part of essence and the balance of deionized water. Based on the basic raw material formula, 1 wt% of traditional Chinese medicine powder is added.
6-3, respectively adding different types of traditional Chinese medicine powder into the novel SMPQ-22 silica system, testing the stability of the toothpaste, and verifying the tolerance of the novel SMPQ-22 silica toothpaste system to different traditional Chinese medicine powder.
The basic raw material formula (% wt) of the novel SMPQ-22 silica toothpaste system comprises: 19.4 parts of hydrated silica, 40.0 parts of sorbitol, 1.0 part of micro-crosslinked poly quaternary ammonium salt SMPQ-22 (the solid content of the micro-crosslinked poly quaternary ammonium salt SMPQ-22 is 60% of the advanced technology development of new materials, co., ltd.), 0.2 parts of xanthan gum, 2.5 parts of sodium lauryl sulfate, 3.0 parts of polyethylene glycol-400, 0.6 parts of sodium carboxymethyl cellulose, 0.3 parts of tetrasodium pyrophosphate, 0.1 part of saccharin sodium, 0.15 parts of methylparaben, 0.05 parts of propylparaben, 1.0 part of essence and the balance of deionized water. Based on the basic raw material formula, 1 wt% of traditional Chinese medicine powder is added.
6-4, respectively adding different types of traditional Chinese medicine powder into the novel SMPQ-22 calcium carbonate toothpaste system, testing the stability of the toothpaste, and verifying the tolerance of the novel SMPQ-22 calcium carbonate toothpaste system to different traditional Chinese medicine powder.
The basic raw material formula (% wt) of the novel SMPQ-22 calcium carbonate toothpaste system comprises the following components: 58.0 parts of calcium carbonate, 25.0 parts of sorbitol, 1.3 parts of micro-crosslinked poly quaternary ammonium salt SMPQ-22 (the solid content of the micro-crosslinked poly quaternary ammonium salt SMPQ-22 is 60% of Shandong Jitai new material science and development Co., ltd.), 0.2 parts of xanthan gum, 2.1 parts of sodium lauryl sulfate, 3.0 parts of polyethylene glycol-400, 0.6 parts of sodium carboxymethylcellulose, 0.3 parts of tetrasodium pyrophosphate, 0.1 part of saccharin sodium, 0.05 parts of propyl hydroxybenzoate, 1.0 part of essence and the balance of deionized water. Based on the basic raw material formula, 1 wt% of traditional Chinese medicine powder is added.
Through tests, the novel MPQ-22/SMPQ-22 silica toothpaste system containing various traditional Chinese medicine powders and the novel MPQ-22/SMPQ-22 calcium carbonate toothpaste system are very stable, and the phenomena of unstable water division, oil division, shelling, coarseness and the like do not occur, so that the MPQ-22/SMPQ-22 has excellent stabilizing effect on the toothpaste system containing the traditional Chinese medicine powders.
Third, adhesion test
Commercially available silica toothpaste and calcium carbonate toothpaste, silica toothpaste of examples 1-5, 11, and calcium carbonate toothpaste of examples 6-10 were simultaneously placed in a refrigerator at 4 ℃ for cold storage of 24 h, and the toothpaste was extruded onto a toothbrush to observe the adhesion of the toothpaste on the toothbrush.
Test results: commercial silica and calcium carbonate toothpastes have poor adhesion in low temperature environments; the toothpastes of examples 1-11 all exhibited excellent adhesion under low temperature environments.
The scheme of the invention is not limited to the listed MPQ-22/SMPQ-22 implementation scheme, and the subsequent upgrading products based on the MPQ-22/SMPQ-22 also have the same effect when applied to a toothpaste system, and belong to the protection scope of the invention.
Claims (4)
1. The application of the high molecular polymer in improving the stability of toothpaste products is characterized in that:
the high polymer is prepared by acrylic acid and dimethyl diallyl ammonium chloride through aqueous solution polymerization or suspension polymerization, and has a molecular weight of 500-2000 ten thousand;
the application method of the high molecular polymer comprises the following steps: (1) The high molecular polymer is directly added into a toothpaste system; or (2) diluting the high molecular polymer with water to prepare a dilute solution preparation, and adding the dilute solution preparation into a toothpaste system; or (3) mixing the high molecular polymer with water and a water-soluble humectant to obtain a thickening component, and adding the thickening component into a toothpaste system; or (4) adding the high molecular polymer, an aqueous solution of the high molecular polymer, or a thickening component obtained by mixing the high molecular polymer with water and a water-soluble humectant as a consistency adjusting component to the produced toothpaste body to adjust the consistency of the toothpaste body.
2. The use of the high molecular polymer according to claim 1 for improving the stability of toothpaste products, characterized in that: the water is deionized water.
3. The use of the high molecular polymer according to claim 1 for improving the stability of toothpaste products, characterized in that: the addition amount of the high molecular polymer in the toothpaste system is 0.05-5.0 wt%.
4. Use of a high molecular polymer according to claim 3 for improving the stability of toothpaste products, characterized in that: the addition amount of the high molecular polymer in the toothpaste system is 0.4-2.0 wt%.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202310683789.4A CN116407465A (en) | 2023-06-10 | 2023-06-10 | Application of high molecular polymer in improving stability of toothpaste product |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202310683789.4A CN116407465A (en) | 2023-06-10 | 2023-06-10 | Application of high molecular polymer in improving stability of toothpaste product |
Publications (1)
Publication Number | Publication Date |
---|---|
CN116407465A true CN116407465A (en) | 2023-07-11 |
Family
ID=87054703
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202310683789.4A Pending CN116407465A (en) | 2023-06-10 | 2023-06-10 | Application of high molecular polymer in improving stability of toothpaste product |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN116407465A (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN116898741A (en) * | 2023-08-18 | 2023-10-20 | 广州品硬生物科技有限公司 | Gum restoration toothpaste containing lysozyme and probiotics and preparation method thereof |
Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103012674A (en) * | 2012-12-11 | 2013-04-03 | 汕头市大千高新科技研究中心有限公司 | Polymeric quaternary ammonium salt with suspension function and application thereof |
CN103705404A (en) * | 2013-12-31 | 2014-04-09 | 汕头市大千高新科技研究中心有限公司 | Emulsion bath foam containing natural oil and preparation method thereof |
CN106511140A (en) * | 2016-01-04 | 2017-03-22 | 无限极(中国)有限公司 | Body wash and preparation method thereof |
WO2019014868A1 (en) * | 2017-07-19 | 2019-01-24 | Henkel (China) Investment Co., Ltd. | Hair conditioning composition having snow-melting effect |
CN111635489A (en) * | 2020-06-15 | 2020-09-08 | 中国石油化工股份有限公司 | Multifunctional supermolecule thickening agent and preparation method thereof |
CN115068369A (en) * | 2022-07-21 | 2022-09-20 | 北京吾星球科技有限公司 | Cation matrix slow-release system and preparation method and application thereof |
-
2023
- 2023-06-10 CN CN202310683789.4A patent/CN116407465A/en active Pending
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103012674A (en) * | 2012-12-11 | 2013-04-03 | 汕头市大千高新科技研究中心有限公司 | Polymeric quaternary ammonium salt with suspension function and application thereof |
CN103705404A (en) * | 2013-12-31 | 2014-04-09 | 汕头市大千高新科技研究中心有限公司 | Emulsion bath foam containing natural oil and preparation method thereof |
CN106511140A (en) * | 2016-01-04 | 2017-03-22 | 无限极(中国)有限公司 | Body wash and preparation method thereof |
WO2019014868A1 (en) * | 2017-07-19 | 2019-01-24 | Henkel (China) Investment Co., Ltd. | Hair conditioning composition having snow-melting effect |
CN111635489A (en) * | 2020-06-15 | 2020-09-08 | 中国石油化工股份有限公司 | Multifunctional supermolecule thickening agent and preparation method thereof |
CN115068369A (en) * | 2022-07-21 | 2022-09-20 | 北京吾星球科技有限公司 | Cation matrix slow-release system and preparation method and application thereof |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN116898741A (en) * | 2023-08-18 | 2023-10-20 | 广州品硬生物科技有限公司 | Gum restoration toothpaste containing lysozyme and probiotics and preparation method thereof |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN102204877B (en) | Oral care composition | |
BRPI0608963B1 (en) | low irritation composition and manufacturing methods | |
JPH0272112A (en) | Toothpaste composition having stripes | |
CN116407465A (en) | Application of high molecular polymer in improving stability of toothpaste product | |
JP2610614B2 (en) | Mild skin cleansing soap containing hydrated cationic polymer | |
AU2010357689B2 (en) | Cleansing composition with decyl and coco glucosides | |
EP2651387A2 (en) | Methyl ethyl hydroxyethyl cellulose for personal care applications | |
CN105902409B (en) | One kind is mild and has thixotropic toothpaste | |
US20080071077A1 (en) | Cosmetic formulations comprising carboxymethyl cellulose | |
JP2012149028A (en) | Hair treatment agent composition | |
CN113633561A (en) | UV-screening cosmetic composition in the form of aqueous dispersion containing heterogeneous organic thickener | |
EP2480194A1 (en) | Carrageenan mixtures useful as cosmetic ingredients and hair styling gels comprising them | |
CN113827508A (en) | Thickening agent, gargling toothpaste and preparation method thereof | |
EP2651519B1 (en) | Oral compositions and method for producing thereof | |
KR100786492B1 (en) | Thixotropic gel type cosmetic composition | |
CN107638341A (en) | A kind of amino acid cleansing cream and preparation method thereof | |
US20150265518A1 (en) | Processes for Preparing Toothpaste | |
US20240009098A1 (en) | Solid composition comprising a combination of anionic surfactants of sulfonate and carboxylate types | |
CN114028273A (en) | Tooth cleaning composition | |
SG190699A1 (en) | Oral compositions and method for producing thereof | |
JP2000327541A (en) | Shampoo composition for hair | |
CN113616553B (en) | Mild and moisture-stable soap-based cleansing cream and preparation method thereof | |
JP2014237618A (en) | Toothpaste composition and production method of toothpaste composition | |
JPS623122B2 (en) | ||
SG190213A1 (en) | Oral compositions and method for producing thereof |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination |