CA1038768A - Dentifrice composition - Google Patents
Dentifrice compositionInfo
- Publication number
- CA1038768A CA1038768A CA210,575A CA210575A CA1038768A CA 1038768 A CA1038768 A CA 1038768A CA 210575 A CA210575 A CA 210575A CA 1038768 A CA1038768 A CA 1038768A
- Authority
- CA
- Canada
- Prior art keywords
- dentifrice
- weight
- monofluorophosphate
- synthetic hectorite
- silica xerogel
- 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.)
- Expired
Links
Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q11/00—Preparations for care of the teeth, of the oral cavity or of dentures; Dentifrices, e.g. toothpastes; Mouth rinses
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
- A61K8/20—Halogens; Compounds thereof
- A61K8/21—Fluorides; Derivatives thereof
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
- A61K8/25—Silicon; Compounds thereof
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
- A61K8/26—Aluminium; Compounds thereof
Landscapes
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Birds (AREA)
- Epidemiology (AREA)
- Oral & Maxillofacial Surgery (AREA)
- Cosmetics (AREA)
Abstract
ABSTRACT OF THE DISCLOSURE
The appearance of a visually clear extruded ribbon of dentifrice containing as an abrasive agent silica xerogel and as a thickening and gelling agent a synthetic hectorite can be improved by incorporating in the dentifrice a water soluble monofluorophosphate. The dentifrice as well as being visually clear should be free from visible particles and immobile bubbles of gas. Optionally, the dentifrice can also contain chloroform.
The appearance of a visually clear extruded ribbon of dentifrice containing as an abrasive agent silica xerogel and as a thickening and gelling agent a synthetic hectorite can be improved by incorporating in the dentifrice a water soluble monofluorophosphate. The dentifrice as well as being visually clear should be free from visible particles and immobile bubbles of gas. Optionally, the dentifrice can also contain chloroform.
Description
~ J ~2 76~ - ~
This inve~ltion rela-tes -to a me-thod ol' improving the appeararl.ce of denti-frices an,d to dentifrices so prepared, more particularly to -those contain.ing a silica xerogel as an, abrasive clean.:in,g agent.
Man.y den-til'rioes are visually opaque, for example white9 an.d at-tempts have been made -to improve the appearan,ce of the ex-truded den-t~frice ribbon as used by the consumer in a teeth cleaning operation. One such develop~ent which .~ ;
has proved to be particularly popular is the development of a transparent den-tifrice which is visually clear even -though it contain,s a silica xerogel as an abrasive. ,~
In order to maintain the desired texture and thixo~
tropic behaviour of this type of visually clear dentifrice, '-a silica aerogel or a pyrogenic silica can. be used as a ",~
thickening an.d gelling agen.t. Suclh dentifrices are described ;' ~" ' , : ::
in United States Patent Specification. 3,5389230. ,.
These silica thickenin~g and gellin,g agen.ts however tend to be expen.sive an.d therefore in. the interests of , :- ., .
economy~ al-ternative thickening ~n.d gelling agen.ts have been in.vestigated. One such group of less expen.sive '~ ;
thickening an.d gelling agen.ts is the synthetic he.ctorites ~hich have been shown, to be satisfactory,in that appropriate thicken:ing an.d gellin.g properties can be obtained. However~
den.tifrices Gontaining both a silica xerogel and a . --synthetic hectorite usually deteriorate on storage, partloularly at temperatures above 20C~ so that the surface appearance of the extruded ribbon can appear dull an.d ~, rippled and the ribborl itsel~ can. as~ume a lumpy texture.
We have now discovered that these problems can be overcome by the in,corporation of a monofluorophosphate in dentifrices of this type so that de-teriorative changes
This inve~ltion rela-tes -to a me-thod ol' improving the appeararl.ce of denti-frices an,d to dentifrices so prepared, more particularly to -those contain.ing a silica xerogel as an, abrasive clean.:in,g agent.
Man.y den-til'rioes are visually opaque, for example white9 an.d at-tempts have been made -to improve the appearan,ce of the ex-truded den-t~frice ribbon as used by the consumer in a teeth cleaning operation. One such develop~ent which .~ ;
has proved to be particularly popular is the development of a transparent den-tifrice which is visually clear even -though it contain,s a silica xerogel as an abrasive. ,~
In order to maintain the desired texture and thixo~
tropic behaviour of this type of visually clear dentifrice, '-a silica aerogel or a pyrogenic silica can. be used as a ",~
thickening an.d gelling agen.t. Suclh dentifrices are described ;' ~" ' , : ::
in United States Patent Specification. 3,5389230. ,.
These silica thickenin~g and gellin,g agen.ts however tend to be expen.sive an.d therefore in. the interests of , :- ., .
economy~ al-ternative thickening ~n.d gelling agen.ts have been in.vestigated. One such group of less expen.sive '~ ;
thickening an.d gelling agen.ts is the synthetic he.ctorites ~hich have been shown, to be satisfactory,in that appropriate thicken:ing an.d gellin.g properties can be obtained. However~
den.tifrices Gontaining both a silica xerogel and a . --synthetic hectorite usually deteriorate on storage, partloularly at temperatures above 20C~ so that the surface appearance of the extruded ribbon can appear dull an.d ~, rippled and the ribborl itsel~ can. as~ume a lumpy texture.
We have now discovered that these problems can be overcome by the in,corporation of a monofluorophosphate in dentifrices of this type so that de-teriorative changes
- 2 - /''' ' ` ctl ~2 ';
9L~387~
on ~tOI'age~ ~or exampl~ up to s.i,x monl;ils at 50C, do nok occur, the extl~u(led derlt:i:L'r:ico r:i.'hbon remain.i,tlg 'bright and shiny in. appea:rance ~ld o:~' a uni~orm smoo-th texture.
We have also con:eirme~:l by consllmer test,ing that t:hese charac-teristics collec-tivel.y appeal to the user, uhereas , , other denti-frices of thi.s gen.eral type having the undesirable ,'-a-ttributes ~hich develop i~, the absen.ce O-r morlofluoropho5phate ~ ~
are n,ot preferred. I-t was also apparen.t from our con~umer ~"
testing -tha-t -the dentifxice should preferably be free t'ro~ ';~
vlsible particles and other inclusions such as en,-trapped ,`
bubbles of gas.
Accordingly, the invention. provides a ~ethod for improving the appearan.ce of a visually clear extruded '',.
ribbon of denti~rice which is free ero~ visi'ble particles and i~mobile bubbles of gas so as to provide -the extruded ., ~. ' ' ribbon. with a brigh-t, shiny surface appearance, the '', . :~,:. , dentifrice containin:g, as an. abrasive agent, a silica xerogel an,d as a thickening and gellin.g agen-t a syn.thetic :, ' ~ ', hec-torite9 which method i9 characterlsed by inccrporating "~
in. the den-tifrice a water solu'ble mon,o~luorophos-phate.
The silica xerogel employed in the preparation o e .
den,tiirices according to the inven.tion as th0 abrasive ,.
agent pre~erably has an, average particle diameter of Erom 2 to 30 microns, more preferably from 4 to 20 microns.
The sur~ace area oi the silica xerogel i9 usually above 250 ',, ~, particularly i'rom 300 to 1000 m2/g. Particularly suitable , are the silica xerogel,s obtainable :erom t,he Da,vison Chemical ,, v~ orl O e W~l Grace fmd Comparly under the -trade names ;'' SYLOID 63~ S~LOI~ 65 a~d SYLOIV 7~, and those sold by Joseph Cro~ield & Sons under -the -trade names GASIL 200 and r;~SII~ 35.
~no~e~ ~r~Je ~A~
~ J ~2 ~8761~
rhe silica xerogel clesirably forms from 5 to 500/?~
preferably 8 to 30/0 and mos t pre~erably 10 to 25% by weigh-t o~ t;he dentilrice.
Synthe-tic hectorite~ are emplored in. the preparation. :.:
of den-tifrices according to thc inventiou a.s ~:hickening and gelling agents. These are syn-thetic complex clays ;~
having the general formula: :
r Si8Mgs lLi~ ~?~.6~24 ~ ~aO.6 g.! These are sold by Laporte Industries Limited under the trade ~ame LAPONITE; examples are LAPONITE CP, LAPONI~E SP9
9L~387~
on ~tOI'age~ ~or exampl~ up to s.i,x monl;ils at 50C, do nok occur, the extl~u(led derlt:i:L'r:ico r:i.'hbon remain.i,tlg 'bright and shiny in. appea:rance ~ld o:~' a uni~orm smoo-th texture.
We have also con:eirme~:l by consllmer test,ing that t:hese charac-teristics collec-tivel.y appeal to the user, uhereas , , other denti-frices of thi.s gen.eral type having the undesirable ,'-a-ttributes ~hich develop i~, the absen.ce O-r morlofluoropho5phate ~ ~
are n,ot preferred. I-t was also apparen.t from our con~umer ~"
testing -tha-t -the dentifxice should preferably be free t'ro~ ';~
vlsible particles and other inclusions such as en,-trapped ,`
bubbles of gas.
Accordingly, the invention. provides a ~ethod for improving the appearan.ce of a visually clear extruded '',.
ribbon of denti~rice which is free ero~ visi'ble particles and i~mobile bubbles of gas so as to provide -the extruded ., ~. ' ' ribbon. with a brigh-t, shiny surface appearance, the '', . :~,:. , dentifrice containin:g, as an. abrasive agent, a silica xerogel an,d as a thickening and gellin.g agen-t a syn.thetic :, ' ~ ', hec-torite9 which method i9 characterlsed by inccrporating "~
in. the den-tifrice a water solu'ble mon,o~luorophos-phate.
The silica xerogel employed in the preparation o e .
den,tiirices according to the inven.tion as th0 abrasive ,.
agent pre~erably has an, average particle diameter of Erom 2 to 30 microns, more preferably from 4 to 20 microns.
The sur~ace area oi the silica xerogel i9 usually above 250 ',, ~, particularly i'rom 300 to 1000 m2/g. Particularly suitable , are the silica xerogel,s obtainable :erom t,he Da,vison Chemical ,, v~ orl O e W~l Grace fmd Comparly under the -trade names ;'' SYLOID 63~ S~LOI~ 65 a~d SYLOIV 7~, and those sold by Joseph Cro~ield & Sons under -the -trade names GASIL 200 and r;~SII~ 35.
~no~e~ ~r~Je ~A~
~ J ~2 ~8761~
rhe silica xerogel clesirably forms from 5 to 500/?~
preferably 8 to 30/0 and mos t pre~erably 10 to 25% by weigh-t o~ t;he dentilrice.
Synthe-tic hectorite~ are emplored in. the preparation. :.:
of den-tifrices according to thc inventiou a.s ~:hickening and gelling agents. These are syn-thetic complex clays ;~
having the general formula: :
r Si8Mgs lLi~ ~?~.6~24 ~ ~aO.6 g.! These are sold by Laporte Industries Limited under the trade ~ame LAPONITE; examples are LAPONITE CP, LAPONI~E SP9
3~ ~ . ,, LAPONITE D a~d LAPONI~E XLG. The u?se o$ some o~ -these materials in denti~rices is described, ~or example in ;
British Patent 17305,353 where their~co~position a~.d nature is ~urther characteri~ed.~
: : Syn:thetic.hectorites of simila~ composition. where ..
fluori~de replaoes some hydroxyl in the above gen.eral ~ -formula, may be used. Examples are I~PONITE B and LAPONITE S
which have the general. formula:
ao r Si8 Ng5 8Lio.520(~l)2F2 ~ 0-5 `
'. ' ',. . .
Varian.ts o~ this ~ormula are dlsclosed in US Pa-ten.t Specification No 3~586,~78.
~he s-yn.thetic hec-torite desirably form3 from O.5 to ~yO~ preferably 1 to 2% by weight of the dentifrice. .~ -q'he water soluble mono~luoropho~phate employed in denti~rice~ accordin.g to the in-vention can be an alkali metal salt which i,s capahle oi providing a source of mono- :~
fluorophosphate ions. Pre~erably, sodium mon.o~luorophosphate i~ used.
C/e~O~tJ ~J~ m~r~
,: , cJ ~
~ 3~7~
Thc mono.flll~rophospha-te should :form :from ~.1 to 2.5%, pre~'erably 0.2 -to 1.~% by wei.~ht o-f the dentifrice.
Derlt:ifrices according -to -the inven.tion. can. also -optionally compr:ise chloro~orm in order -to enhance or .- :.
modify -the flavour oi' the den.tifri.ce. When. used, t'he ~ ~
amount o~ chlorofor~l shou'Ld form from 0.1 to 4%9 preferably ;;. .:
0.5 to 2% by weight o:f -the dentifrice.
The den-tifrice of the in.~ention can. al~o contain .~
various optional ingredient~ ~or instance a 80ap or ' .' syn.thetic de-tergen.-t as foa~ing agen-t; flavouring materials;
bu-f-fers~ sweeteners, such as saccharin.; humec-tants; .'':
preser~atives; an.d colourin.g materlals. '~
The dentifrice can con.tain a humectant and a binder in amounts to give the clentifrice a smooth ;;~
. texture and good flowabilityO Glycerin and sorbitol are pre~erred humectan-ts~ but others, for example ~
~; propyleo.e glycol and polyethylene glycol, especially polyethylene glycol 400, can also be employed. Examples oP suita'ble binders tha-t can be used are gum traga¢anth, ,: , sodium carbo~ymethylcellulose, hydroxyethyl cellulose, '.'' ~.
carragheen an.d its deriva~ives~ s-tarch derivatives and 'locust bean ~um. Polyethylene glycols of high molecular . ~:
weight, for exampl.e polyethylene glycol 1500 or 15409 can. .. ::
optionally be employed to impro~e the water dispersibili-ty, the vi9ual clarity an.d the texture of the fin.ished product.
There can. also 'be included in the dentifr:Lce composition~ of the in:ven.tion. prophylatic or therapeu-tic agents, such a~ germlcides, an.tibio-tics~ astringents and other ~.
fluorine-contalnln.~ compounds. 'rypical examples thereof inc'lude tyrothrycln~ chlorophyllins, hexachlurophene, the flarcos-J.des, astringent salts and water-soluble ionizable fluorine~contaln-lng compounds, nther tharl monoflllorophosphn-te ~uch a~ ~tann.olls l'lwor~de.
" / ~
.. ..
, ,~~` c~ ~2 ~13~761~
Such prophylatic or -t~lerapeutic agents can 'he employed in a 'beneficial amount normal'Ly ran.ging from a'bou-t O.Ol%
to about 2% by weight of -the dent-lfrice.
Humectants can gen.erall~ be emplo.~yed in. an amount from about 5/O to about 70/09 -the bin.ders in an amoun.t -from about ~"
0.5/0 to about 30%9 flavouring agents in an amoun.t ~rom about 0.1% to about 5~0, ~oaming agents in. an amoun-t ~rom about 0.01% to about 6%, buf~ers in an a~ount ~rom about 0.02~ to about 10%~ an.d preservatives in. an amoun-t $rom about 0.01~ to about 2%~ all percentages bein.g 'by weight of . -~, the dentifriceq In, the ~ormulation and preparation o~ denti~rices -~
~ .- . .
accordin.g -to t~e invention, it is necessary -to exclude .
: materials which in the finished product are visible as . :, .
discrete particles and to exclude, for exa~ple by a deaeration :'~
step, en.trapped buhbles o~ air or other gas. This is .' :.-. .:
contrary to the proposal con,templa-ted in British Patent .. . . .
Specification 19304,090 where immobile bubbles of gas ,'-,,p are deliberately introduced i~to a visually clear den.ti~rice. '. ''-Dentifrices acoordlng to this invention can be made in, several ways. Accordin.g to a preferred method, the ,. ~,~
~ynthetic hectorite is first dispersed with agi-tation or s-tirring in at least a portion. of a humectan-t together ''' wi-th suffi¢ieD,t water to enable an e~fective dispersion 2~ to be obtained. It i.s generally n.ecessary to heat the ':
tJispersion~ for example to a temperature of from 30 to 90C, before coo'l-lng and then passin.g through a colloid mill to ensure that any lump~ of the dispersed hec-torite are bro~en ~.
down.
-"' cJ ~2 ~
~87~
'rhe aera-ted gel so o'btain.ed can, thell.be stirred under vacuum -to remove en.l;rapped air before carefu'L
additi.on of ot.her in.gredien-ts. Fur-ther deaeratian. may ~
'be n.ecessary. Fin.ally, it may 'be necessary to adju~t the "., ' ,.
:, : .
wa-ter level of -t'he compos:ition. to ensure optimum visual ;,; ;' clari-ty. It will be appreciated that some water will '.~
usually be presen.t in some o~ the ingredients used, for ~;.
example in the humec-tant, and that in, some cases i-t may not ' .~. ' be necessary to add water as a separate in.gredient. It car generally be sta-ted that -the total amount of water will .'- .',,~
form from 15 -to 30C/o by weight of the den.tifrice, but the '.''~
actual amount present in a particular denti~rice will ,.
depen.d on. the prec1se n.ature and quantity of sillca xerogel~
-- syn,-thetic hectori-te an,d humectant used~ The appropriate 1~5 amount Or wat~er ca~-thus be determ:i~ed for a par-ticular : den.tifrice by simple experiment. , ;'~;
The invention i~ illustrated by the followin.g Examples. ~ ',-:,m ~; ~ E~ample 1 ,~
A vlsually clear dentifrioe was prepared from the . , -~: 20 ~ollowing i~gr~dien.ts~
' / by weigh-t , ~,, .
Glycerin~: 15.0 ' Sor'bitol ~ ~l.O ~
Silica xerogel (GASIL 200~ 14.0 , ~ :
25 Synthetlc hectorite (LAPONITE CP) 2.0 De-tergent 1.2 , Swee-tener 0.2 Colour (4% aq,ueous) O. 3 Sodium hydroxide 0.15 30 Sodium monofluoropho~phate 0.8 Chloroform 0.8 Fla-vour l.O
Water -to 100 r~A~
~' - .
, ... . .
,~, . . .
cJ ~2 7~8 ~r~le dellti.t`l~i.ce was pr~parecl in, the :f'ollowin.g mann~.3r: ~
* , , (.i) The l~P~NITE Wrl~ di~3persed wil;h a hi,~h speed stirrer :' in a mix-ture o1' gl.yceri~ and svrbi-tol -toge-ther with ~ome wa-ter. ,~
(ii) The susp0n.s:ion so o'bta,ined was heated to a -temperatu:re of 80C -~or 2 hours, and s-tirring was co-n,tin.ued using a low s~hear stirrer. The s~uspensiort was then. cooled.
(iii) The cooled suspen.sion. was passed -through a colloid mill to break up any lumps of the LAPON~TE which had not '', ' .~.
been adequately dispersed.
(iv) The resul-ting aerated gel was deaerated by stirring gently under vacuum and then salts, sweetener a~d colour .. ''~
were added together with the silica xerogel and the mix-ture again deaerated by slow s-ti.rring under vacuu~.
.
: 15 (v) Finally the remaining ingredients in.cluding detergen-t ,. '~
and flavour were added:together ~ith a little water to ~ . .; .
adjust -the refractive index so as to obtain a den,-ti~rice `.
which was visually clear.
(vi) The denti~rice so obtained wa~ finally packed into aluminium tubes, . . . .
, .
'rhis dentifrice was shown.-to be s-table and o~ ;
excellen.-t quality even after s-torage at 50C for six mon.th~
The extruded rib'hon. had a bright, shiny surface appearance, wa.s visually clear and ~ree fron3 visible particles and en,trapped gas 'bubbles an,d the texture was uniform ancl 9~00 th. : :
For ~,omparative pu:rpo~es, a similar c'len-t:if'rice was prepared except that the mono~'Luorophosphate was omit-ted~
the ~Iycerin 'Lcvel being increa~ed to 15.8% by wei~ht 'by way Or compen,~at:ion.. Thi~ den-ti~rice, alth~ gh initially o~ good ~luali-ty, rapidly deteriorated on s-torage a~ter on,e mor)th cl~t ~50C to give a product wh:ich on extrusion ~)roduced a rib'hor1. havi.ng a dul'L, rlppled a~)l)ea-ranc¢ arld a 'ltJrlll)y ~,~xt J r~ J~ K
- `
'' cJ ~1~2 ~876~3 Example 2 ,, -' A visual1.y cleax dentifrice was prepared 'by the mar~er described i.n Example l from the Pollowing . .
~ .
in.gredien,ts: ~ .
~ by weight '; ....... .. .
Sorbitol ~ 56.0 ,, '; ' ,,,.~; Silica xerogel (GASI~ 200) ~ l4.0 ,~ 't' Syntheti.c hec-torite ~APONIrrE CP) 2.0 .~
Detergen-t l.5 , ~:
Swee-t0n.er 0.2 Colour (4% aq,ueous) 0.3 ;~ ' Sodium hydroxide 0.15 Sodium mon,ofluorophosphate 0.8 , .' Flavour 1.0 ',~
l~ Water to lO0 : This denti~rioe had a most pleasing s'hiny, brightappearance when extruded as a ribbon. rrhis characteristic : was still evldent a~ter~storage for 6 months at 50C. The -~
: extruded ribbon was also of smooth, un.i~orm texture a~d .~-.
: 20 free from lumps, as well as being co~pletely clear ~isually ~ -' and free from visible particles an.d o-ther inclusion~.
.
:
oleno~e~ ~r~d~ ~narK
~; "
:~
~ ***
. .
, .
British Patent 17305,353 where their~co~position a~.d nature is ~urther characteri~ed.~
: : Syn:thetic.hectorites of simila~ composition. where ..
fluori~de replaoes some hydroxyl in the above gen.eral ~ -formula, may be used. Examples are I~PONITE B and LAPONITE S
which have the general. formula:
ao r Si8 Ng5 8Lio.520(~l)2F2 ~ 0-5 `
'. ' ',. . .
Varian.ts o~ this ~ormula are dlsclosed in US Pa-ten.t Specification No 3~586,~78.
~he s-yn.thetic hec-torite desirably form3 from O.5 to ~yO~ preferably 1 to 2% by weight of the dentifrice. .~ -q'he water soluble mono~luoropho~phate employed in denti~rice~ accordin.g to the in-vention can be an alkali metal salt which i,s capahle oi providing a source of mono- :~
fluorophosphate ions. Pre~erably, sodium mon.o~luorophosphate i~ used.
C/e~O~tJ ~J~ m~r~
,: , cJ ~
~ 3~7~
Thc mono.flll~rophospha-te should :form :from ~.1 to 2.5%, pre~'erably 0.2 -to 1.~% by wei.~ht o-f the dentifrice.
Derlt:ifrices according -to -the inven.tion. can. also -optionally compr:ise chloro~orm in order -to enhance or .- :.
modify -the flavour oi' the den.tifri.ce. When. used, t'he ~ ~
amount o~ chlorofor~l shou'Ld form from 0.1 to 4%9 preferably ;;. .:
0.5 to 2% by weight o:f -the dentifrice.
The den-tifrice of the in.~ention can. al~o contain .~
various optional ingredient~ ~or instance a 80ap or ' .' syn.thetic de-tergen.-t as foa~ing agen-t; flavouring materials;
bu-f-fers~ sweeteners, such as saccharin.; humec-tants; .'':
preser~atives; an.d colourin.g materlals. '~
The dentifrice can con.tain a humectant and a binder in amounts to give the clentifrice a smooth ;;~
. texture and good flowabilityO Glycerin and sorbitol are pre~erred humectan-ts~ but others, for example ~
~; propyleo.e glycol and polyethylene glycol, especially polyethylene glycol 400, can also be employed. Examples oP suita'ble binders tha-t can be used are gum traga¢anth, ,: , sodium carbo~ymethylcellulose, hydroxyethyl cellulose, '.'' ~.
carragheen an.d its deriva~ives~ s-tarch derivatives and 'locust bean ~um. Polyethylene glycols of high molecular . ~:
weight, for exampl.e polyethylene glycol 1500 or 15409 can. .. ::
optionally be employed to impro~e the water dispersibili-ty, the vi9ual clarity an.d the texture of the fin.ished product.
There can. also 'be included in the dentifr:Lce composition~ of the in:ven.tion. prophylatic or therapeu-tic agents, such a~ germlcides, an.tibio-tics~ astringents and other ~.
fluorine-contalnln.~ compounds. 'rypical examples thereof inc'lude tyrothrycln~ chlorophyllins, hexachlurophene, the flarcos-J.des, astringent salts and water-soluble ionizable fluorine~contaln-lng compounds, nther tharl monoflllorophosphn-te ~uch a~ ~tann.olls l'lwor~de.
" / ~
.. ..
, ,~~` c~ ~2 ~13~761~
Such prophylatic or -t~lerapeutic agents can 'he employed in a 'beneficial amount normal'Ly ran.ging from a'bou-t O.Ol%
to about 2% by weight of -the dent-lfrice.
Humectants can gen.erall~ be emplo.~yed in. an amount from about 5/O to about 70/09 -the bin.ders in an amoun.t -from about ~"
0.5/0 to about 30%9 flavouring agents in an amoun.t ~rom about 0.1% to about 5~0, ~oaming agents in. an amoun-t ~rom about 0.01% to about 6%, buf~ers in an a~ount ~rom about 0.02~ to about 10%~ an.d preservatives in. an amoun-t $rom about 0.01~ to about 2%~ all percentages bein.g 'by weight of . -~, the dentifriceq In, the ~ormulation and preparation o~ denti~rices -~
~ .- . .
accordin.g -to t~e invention, it is necessary -to exclude .
: materials which in the finished product are visible as . :, .
discrete particles and to exclude, for exa~ple by a deaeration :'~
step, en.trapped buhbles o~ air or other gas. This is .' :.-. .:
contrary to the proposal con,templa-ted in British Patent .. . . .
Specification 19304,090 where immobile bubbles of gas ,'-,,p are deliberately introduced i~to a visually clear den.ti~rice. '. ''-Dentifrices acoordlng to this invention can be made in, several ways. Accordin.g to a preferred method, the ,. ~,~
~ynthetic hectorite is first dispersed with agi-tation or s-tirring in at least a portion. of a humectan-t together ''' wi-th suffi¢ieD,t water to enable an e~fective dispersion 2~ to be obtained. It i.s generally n.ecessary to heat the ':
tJispersion~ for example to a temperature of from 30 to 90C, before coo'l-lng and then passin.g through a colloid mill to ensure that any lump~ of the dispersed hec-torite are bro~en ~.
down.
-"' cJ ~2 ~
~87~
'rhe aera-ted gel so o'btain.ed can, thell.be stirred under vacuum -to remove en.l;rapped air before carefu'L
additi.on of ot.her in.gredien-ts. Fur-ther deaeratian. may ~
'be n.ecessary. Fin.ally, it may 'be necessary to adju~t the "., ' ,.
:, : .
wa-ter level of -t'he compos:ition. to ensure optimum visual ;,; ;' clari-ty. It will be appreciated that some water will '.~
usually be presen.t in some o~ the ingredients used, for ~;.
example in the humec-tant, and that in, some cases i-t may not ' .~. ' be necessary to add water as a separate in.gredient. It car generally be sta-ted that -the total amount of water will .'- .',,~
form from 15 -to 30C/o by weight of the den.tifrice, but the '.''~
actual amount present in a particular denti~rice will ,.
depen.d on. the prec1se n.ature and quantity of sillca xerogel~
-- syn,-thetic hectori-te an,d humectant used~ The appropriate 1~5 amount Or wat~er ca~-thus be determ:i~ed for a par-ticular : den.tifrice by simple experiment. , ;'~;
The invention i~ illustrated by the followin.g Examples. ~ ',-:,m ~; ~ E~ample 1 ,~
A vlsually clear dentifrioe was prepared from the . , -~: 20 ~ollowing i~gr~dien.ts~
' / by weigh-t , ~,, .
Glycerin~: 15.0 ' Sor'bitol ~ ~l.O ~
Silica xerogel (GASIL 200~ 14.0 , ~ :
25 Synthetlc hectorite (LAPONITE CP) 2.0 De-tergent 1.2 , Swee-tener 0.2 Colour (4% aq,ueous) O. 3 Sodium hydroxide 0.15 30 Sodium monofluoropho~phate 0.8 Chloroform 0.8 Fla-vour l.O
Water -to 100 r~A~
~' - .
, ... . .
,~, . . .
cJ ~2 7~8 ~r~le dellti.t`l~i.ce was pr~parecl in, the :f'ollowin.g mann~.3r: ~
* , , (.i) The l~P~NITE Wrl~ di~3persed wil;h a hi,~h speed stirrer :' in a mix-ture o1' gl.yceri~ and svrbi-tol -toge-ther with ~ome wa-ter. ,~
(ii) The susp0n.s:ion so o'bta,ined was heated to a -temperatu:re of 80C -~or 2 hours, and s-tirring was co-n,tin.ued using a low s~hear stirrer. The s~uspensiort was then. cooled.
(iii) The cooled suspen.sion. was passed -through a colloid mill to break up any lumps of the LAPON~TE which had not '', ' .~.
been adequately dispersed.
(iv) The resul-ting aerated gel was deaerated by stirring gently under vacuum and then salts, sweetener a~d colour .. ''~
were added together with the silica xerogel and the mix-ture again deaerated by slow s-ti.rring under vacuu~.
.
: 15 (v) Finally the remaining ingredients in.cluding detergen-t ,. '~
and flavour were added:together ~ith a little water to ~ . .; .
adjust -the refractive index so as to obtain a den,-ti~rice `.
which was visually clear.
(vi) The denti~rice so obtained wa~ finally packed into aluminium tubes, . . . .
, .
'rhis dentifrice was shown.-to be s-table and o~ ;
excellen.-t quality even after s-torage at 50C for six mon.th~
The extruded rib'hon. had a bright, shiny surface appearance, wa.s visually clear and ~ree fron3 visible particles and en,trapped gas 'bubbles an,d the texture was uniform ancl 9~00 th. : :
For ~,omparative pu:rpo~es, a similar c'len-t:if'rice was prepared except that the mono~'Luorophosphate was omit-ted~
the ~Iycerin 'Lcvel being increa~ed to 15.8% by wei~ht 'by way Or compen,~at:ion.. Thi~ den-ti~rice, alth~ gh initially o~ good ~luali-ty, rapidly deteriorated on s-torage a~ter on,e mor)th cl~t ~50C to give a product wh:ich on extrusion ~)roduced a rib'hor1. havi.ng a dul'L, rlppled a~)l)ea-ranc¢ arld a 'ltJrlll)y ~,~xt J r~ J~ K
- `
'' cJ ~1~2 ~876~3 Example 2 ,, -' A visual1.y cleax dentifrice was prepared 'by the mar~er described i.n Example l from the Pollowing . .
~ .
in.gredien,ts: ~ .
~ by weight '; ....... .. .
Sorbitol ~ 56.0 ,, '; ' ,,,.~; Silica xerogel (GASI~ 200) ~ l4.0 ,~ 't' Syntheti.c hec-torite ~APONIrrE CP) 2.0 .~
Detergen-t l.5 , ~:
Swee-t0n.er 0.2 Colour (4% aq,ueous) 0.3 ;~ ' Sodium hydroxide 0.15 Sodium mon,ofluorophosphate 0.8 , .' Flavour 1.0 ',~
l~ Water to lO0 : This denti~rioe had a most pleasing s'hiny, brightappearance when extruded as a ribbon. rrhis characteristic : was still evldent a~ter~storage for 6 months at 50C. The -~
: extruded ribbon was also of smooth, un.i~orm texture a~d .~-.
: 20 free from lumps, as well as being co~pletely clear ~isually ~ -' and free from visible particles an.d o-ther inclusion~.
.
:
oleno~e~ ~r~d~ ~narK
~; "
:~
~ ***
. .
, .
Claims (13)
1. A visually clear dentifrice substantially free from visible particles and immobile bubbles of gas, the dentifrice having a bright shiny surface appearance when extruded as a ribbon, the dentifrice comprising as an abrasive agent a silica xerogel, as a thickener and gelling agent a synthetic hectorite and as a source of monofluorophosphate ions a water soluble monofluorophosphate and said dentifrice being packed in a container from which it can be extruded as a ribbon.
2. A dentifrice according to claim 1, in which the silica xerogel has an average particle diameter of from 2 to 30 microns and a surface area of greater than 250 m2/g.
3. A dentifrice according to claim 1, in which the silica forms from 5 to 50% by weight of the dentifrice.
4. A dentifrice according to claim 1, in which the synthetic hectorite is a synthetic complex clay having the general formula:
[Si8Mg5.1Li0.6H4.6O24] 0.6-Na+0.6
[Si8Mg5.1Li0.6H4.6O24] 0.6-Na+0.6
5. A dentifrice according to claim 1, in which the synthetic hectorite is a synthetic complex clay having the general formula:
[Si8mg5.8Li0.5(OH)2F2O20] 0.5-Na+0.5
[Si8mg5.8Li0.5(OH)2F2O20] 0.5-Na+0.5
6. A dentifrice according to claim 1,2 or 3, in which the synthetic hectorite forms from 0.5 to 4% by weight of the dentifrice.
7. A dentifrice according to claim 1,2 or 3, in which the monofluorophosphate is sodium monofluorophosphate.
8. A dentifrice according to claim 1,2 or 3, in which the monofluorophosphate forms from 0.1 to 2.5% by weight of the dentifrice.
9. A dentifrice according to claim 1, further comprising chloroform.
10. A dentifrice according to claim 9, in which the chloroform forms from 0.1 to 4% by weight of the dentifrice.
11. A dentifrice according to claim 1,2 or 3, comprising the following ingredients:
from 8 to 30% by weight of a silica xerogel, from 1 to 3% by weight of a synthetic hectorite having the formula:
[Si8Mg5.1Li0.6H4.6O24] 0.6-Na+0.6 from 0.2 to 1.6% by weight of sodium monofluoro-phosphate, and from 5 to 70% by weight of a humectant selected from the group consisting of glycerin and sorbitol and mixtures thereof.
from 8 to 30% by weight of a silica xerogel, from 1 to 3% by weight of a synthetic hectorite having the formula:
[Si8Mg5.1Li0.6H4.6O24] 0.6-Na+0.6 from 0.2 to 1.6% by weight of sodium monofluoro-phosphate, and from 5 to 70% by weight of a humectant selected from the group consisting of glycerin and sorbitol and mixtures thereof.
12. A method for preparing a visually clear dentifrice according to claim 1, which is substantially free from visible particles and immobile bubbles of gas, the dentifrice having a bright, shiny surface appearance when extruded as a ribbon, and containing as an abrasive a silica xerogel and as a thickener and gelling agent a synthetic hectorite, which method comprises incorporating in the dentifrice a water soluble monofluorophosphate.
13. A method according to claim 12 which comprises dispersing the synthetic hectorite in a humectant including water to provide a suspension and deaerating the suspension and dispersing therein the silica xerogel and the water soluble monofluorophosphate.
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| GB4620373A GB1476633A (en) | 1973-10-03 | 1973-10-03 | Dentifrice composition |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA1038768A true CA1038768A (en) | 1978-09-19 |
Family
ID=10440275
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA210,575A Expired CA1038768A (en) | 1973-10-03 | 1974-10-02 | Dentifrice composition |
Country Status (16)
| Country | Link |
|---|---|
| AT (1) | ATA788774A (en) |
| AU (1) | AU499049B2 (en) |
| BE (1) | BE820652A (en) |
| CA (1) | CA1038768A (en) |
| CH (1) | CH610202A5 (en) |
| DE (1) | DE2446618A1 (en) |
| DK (1) | DK137825B (en) |
| FI (1) | FI58588C (en) |
| FR (1) | FR2246261B1 (en) |
| GB (1) | GB1476633A (en) |
| IE (1) | IE39681B1 (en) |
| IT (1) | IT1020922B (en) |
| NL (1) | NL7412992A (en) |
| PH (1) | PH11091A (en) |
| SE (1) | SE413738B (en) |
| ZA (1) | ZA746240B (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2109682B (en) * | 1981-11-19 | 1985-09-11 | Colgate Palmolive Co | Stable dentifrice |
| GB2109683B (en) * | 1981-11-19 | 1985-09-11 | Colgate Palmolive Co | Stable dentifrice |
| ES2544241T3 (en) * | 2005-03-21 | 2015-08-28 | Glaxo Group Limited | Alkyl sulfate and orthophosphate free dentifrice composition comprising a source of fluoride and a silica dental abrasive |
| DE102008006683A1 (en) * | 2008-01-30 | 2009-08-06 | Evonik Degussa Gmbh | silica dispersion |
| CA2926403C (en) | 2013-10-28 | 2018-01-02 | The Procter & Gamble Company | Late stage addition of rheology modifier |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3538230A (en) * | 1966-12-05 | 1970-11-03 | Lever Brothers Ltd | Oral compositions containing silica xerogels as cleaning and polishing agents |
| GB1305353A (en) * | 1970-11-27 | 1973-01-31 | ||
| GB1304090A (en) * | 1970-11-27 | 1973-01-24 | ||
| GB1400154A (en) * | 1971-10-22 | 1975-07-16 | Unilever Ltd | Toothpaste |
| BE790859A (en) * | 1971-11-02 | 1973-04-30 | Pfizer | CARBOXAMIDOBENZOIC ACIDS AS HYPOLIPEMIC AGENTS |
-
1973
- 1973-10-03 GB GB4620373A patent/GB1476633A/en not_active Expired
-
1974
- 1974-09-26 DK DK507574AA patent/DK137825B/en not_active IP Right Cessation
- 1974-09-27 PH PH16339A patent/PH11091A/en unknown
- 1974-09-30 DE DE19742446618 patent/DE2446618A1/en not_active Ceased
- 1974-10-01 AU AU73834/74A patent/AU499049B2/en not_active Expired
- 1974-10-01 ZA ZA00746240A patent/ZA746240B/en unknown
- 1974-10-01 AT AT788774A patent/ATA788774A/en not_active Application Discontinuation
- 1974-10-01 FR FR7433027A patent/FR2246261B1/fr not_active Expired
- 1974-10-01 IE IE2035/74A patent/IE39681B1/en unknown
- 1974-10-02 IT IT69951/74A patent/IT1020922B/en active
- 1974-10-02 FI FI2878/74A patent/FI58588C/en active
- 1974-10-02 SE SE7412424A patent/SE413738B/en not_active IP Right Cessation
- 1974-10-02 NL NL7412992A patent/NL7412992A/en not_active Application Discontinuation
- 1974-10-02 CA CA210,575A patent/CA1038768A/en not_active Expired
- 1974-10-02 BE BE149171A patent/BE820652A/en not_active IP Right Cessation
- 1974-10-03 CH CH1331974A patent/CH610202A5/en not_active IP Right Cessation
Also Published As
| Publication number | Publication date |
|---|---|
| AU499049B2 (en) | 1979-04-05 |
| PH11091A (en) | 1977-10-25 |
| DK507574A (en) | 1975-06-09 |
| IT1020922B (en) | 1977-12-30 |
| ATA788774A (en) | 1979-05-15 |
| BE820652A (en) | 1975-04-02 |
| DK137825C (en) | 1978-10-23 |
| IE39681L (en) | 1975-04-03 |
| FR2246261B1 (en) | 1979-07-20 |
| CH610202A5 (en) | 1979-04-12 |
| SE7412424L (en) | 1975-04-04 |
| DK137825B (en) | 1978-05-16 |
| FR2246261A1 (en) | 1975-05-02 |
| DE2446618A1 (en) | 1975-04-10 |
| NL7412992A (en) | 1975-04-07 |
| FI58588B (en) | 1980-11-28 |
| FI287874A (en) | 1975-04-04 |
| ZA746240B (en) | 1976-06-30 |
| AU7383474A (en) | 1976-04-08 |
| IE39681B1 (en) | 1978-12-06 |
| SE413738B (en) | 1980-06-23 |
| FI58588C (en) | 1981-03-10 |
| GB1476633A (en) | 1977-06-16 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US3927201A (en) | Dentifrices | |
| US4263276A (en) | Dentifrices | |
| US3927202A (en) | Dentifrices | |
| US3925543A (en) | Antibacterial oral compositions containing preservative-antioxidants | |
| US4618488A (en) | Toothpaste composition | |
| EP0664694B1 (en) | Oral hygiene composition | |
| US3862307A (en) | Dentifrices containing a cationic therapeutic agent and improved silica abrasive | |
| US4456585A (en) | Visually clear pigment-colored dentifrice composition | |
| US4098878A (en) | Toothpaste containing milled alpha-alumina trihydrate | |
| US3887701A (en) | Antibacterial oral compositions containing preservative-antioxidants | |
| US4003971A (en) | Production of particles for incorporation in dentifrices | |
| EP2600938B1 (en) | Oral care compositions | |
| US20070154412A1 (en) | Dentifrices comprising biogenic silica materials | |
| CA1038768A (en) | Dentifrice composition | |
| US20080159967A1 (en) | Dentifrices comprising biogenic silica materials and at least one calcium phosphate | |
| EP0938287B1 (en) | Toothpaste compositions containing fluidized polymer suspensions of carboxymethyl cellulose | |
| WO2011001781A1 (en) | Water-in-oil emulsion-type cosmetic preparation | |
| US4036949A (en) | Clear dentifrice | |
| JPH0246005B2 (en) | ||
| CA1329369C (en) | Dentifrice having decreased abrasivity | |
| US4007259A (en) | Dental cream | |
| US20060008423A1 (en) | Dentifrice compositions and abrasive systems | |
| US20070154413A1 (en) | Dentifrices comprising biogenic silica materials | |
| US6896876B1 (en) | High cleaning silica gel dental abrasive, dentifrices prepared therefrom, and a method for preparing the dental abrasive | |
| FR2583981A1 (en) | TRANSPARENT TOOTHPASTE |