SE433037B - PHOTOPOLYMERIZABLE ONE-PHASE COMPOSITION FOR USE IN TREATING DAMAGED TENDERS - Google Patents

Description

7711708-3 «\) an almost solid mass. If you do not succeed in achieving acceptable homogeneity, errors may occur in the repairs.

U.S. Pat. No. 3,759,807 proposes a combination of an organic carbonyl compound and an amine, especially combinations of benzophenone and a tertiary amine, as initiator and acoelerator, respectively. Although the latter compositions are polymerizable, they are not suitable as Filling No. for tooth elongation due to long curing time. complex systems for dental purposes, containing a diglycidyl ether derivative of bisphenol-A, an acrylic binder and filler material] crosslinked with benzoyl peroxide or other suitable catalyst have been proposed in U.S. Patent 3,539,533. These have been found to have a compressive strength of only 18.3 kp / mmz (column 5, line GÄ).

IIiLLi I Is nnviindn kompositionm- For denl-uln íínolalrniil he 'síiluruln val-il two-fn »system, ie. paste / paste, paste / liquid, liquid / liquid or powder / liquid. The two phases are added in certain proportions and mixed. The properties of the final product depend on how well, and how quickly this mixing is performed. During mixing, air can be incorporated into the pulp, and will act as a polymerization inhibitor. The air can thus cause a deterioration of the mechanical properties of the material and cause it to cure more slowly. Unevenness in the mixture further lowers the quality of the repairs. Such inconveniences are eliminated by the present invention.

An object of the present invention is to propose a uniform, vn-Vns kmuposil-íonl Išínnuul För 'm-.ntnlšindzuuzil, which nmdgçor' long Förnrningstid, and which does not require any manual processing in connection with its use.

A further object of the invention is to propose a composition which is suitable for dentistry purposes, and which has a high pressure holding.

The invention also encompasses a novel initiator / accelerator combination which is suitable for use in connection with the photopolymerization of acrylic esters. A further object of the invention is to provide a fast curing composition suitable for dental use. Yet another object of the invention is to propose a dental composition which allows curing at slippery depths, and which is particularly suitable for be used in high salinity of fillers or pigments.

An object of the invention is to propose a dental material which is impermeable to X-rays. and which can be made to harden by the action of actinic radiation.

The invention thus proposes a single-phase composition boom suitable for repairing holes and apricot teeth. and which can be used bum sealants or adhesives, as well as to coat cavities and repair enamel in dental work.

These and other objects can be achieved by using according to the invention a composition, wherein the various components are included with the following parts by weight, Bisphenol A-bis (3 methacrylate-2-hydroxypropyl) ether 10-25, monomeric diluent containing an acrylate 2-5, initial - tor containing an alpha-diketin 0.001 - I, acceleration containing a tertiary amine 0.1 - 2, barium and / or lithium-aluminum alloy and the like.

The advantages of the invention will become apparent from the following description. Photopolymerizable compositions have recently gained increasing use in connection with the repair of teeth. Components used usually contain a monomeric, polymerizable resin containing unsaturated branches, a monomeric diluent for the composition of the resin, a filler, or a combination of fillers, an initiator which emits free radicals and radicals. which reacts with the double bonds in the mouth so that pnlymerisntluner is initiated, and an accelerator sum increases the Photorvnktionshustigheten. The amount of resin used in the preparation of a single-phase paste according to the invention can be obtained by reacting a diglycidyl ester of bisphenol-A with a methacrylic or an acyl acid. 7711708-3 4 ri-I I !! one? n rli cin? npc_v_cr_o_® _c_ Q -occ-cnz + 'mig - c _ coon 5 0 / IL (lm i \ 3 C113? III Ill III (FUB III lr ll (I) ((113 C112 = cc-oc-ccoQ -cQ - Occ- _o_c_c = 011 ,, 1 i ¿1 nn \ ~ H OH CHB H OH H This glycidyl menacrylate derivative of bisphenol-A is known as bisphenol ~ A ~ bís (3 methacrylate-2-hydroxypropyl) ether. binder in photopolymerizations of compoitionez -and hereinafter referred to as ßis-GMA, in short, certain modifications of this resin may also be considered.

The monomeric diluent used can be selected from alkyl methacrylate, alkylene dimethacrylate, trimethacrylate, alkyl acrylate, as well as alkylene diacrylate and triacrylate. Some of the suitable monomers are represented by methyl motacrylate, ethyl methacrylate, butyl methacrylate, n-propyl methacrylate, isopropyl methacrylate, 1,3-butylene dimethacrylate, ethylene glycol monomethacrylate, ethylene glycol dimethacrylate, triethyl acrylate, triethyl acrylate, triethyl acrylate, triethyl acrylate.

One or more of these monomers may be used. The monomeric diluents are added together with His-GMA resin soot when dv, in the presence of a photoinitiator and an accelerator, are subjected to nectinic training. The accelerator tower accelerates the reaction.

Another component included in the composition is a polymerization inhibitor of the Bis-MGA resin and the monomeric diluent, which is only present in small amounts. A suitable polymerization inhibitor is hydroquinone (HQ), methyl ether hydroquinone (MEHQ), butylated hydroxytoluene (BUT) and triphenylstyrene. V 7711708-3 '' \ J! Photoinitiators are usually used for photosensitive carhonyl compounds.

The initiators used in connection with the present invention are ul-diketone, and their derivatives of the general formula R-COCO-R 'where R and R' may be the same, or different nliphutic or aromatic (frmyxpvr, ellr-r 'rloruns llz -rivnl. Niígflfz; L-xmnpol ung / ges hšir- nmlnn: tïll, i (. '() (ï (l (šll, š hínuvl.) I CI {, ¿C () C () Cl12 (3} l , $ 2, 'š-pen tzmdi on sön scfocrocöf-IS' benz 1.1 en, oc u 00000 .n non 14,1: udifneroxii hel-mil 5 6 h 6 h 3 (<'¿¿I15 <: <1 < : <> «'6r1ñ) 2o l;, l |' _n> These photoinitiators how pale yellow color.Because they are only present in small quantities, the final product will be practically colorless.

Photo accelerators are chemical compounds that, in the presence of initiators, accelerate the photoreaction. The accelerator tower allows the polymer ion to penetrate into deep half-cylinders. Ancelvrnlorvrnn consists of uminvr (primary. Secondary or lertiary) fi nmi dinminvr.

Examples which may be mentioned are dimethylparatoluidine, N, N '- dimethylbenzylamine.

N-methyldibutylamine, triethylamine, trihexylamine, etc. Examples of suitable diamines are N, N, N ', N' -tetraethylethylenediamine, and N, N, N ', N' -tetramethyl 1,6-hexanediamine.

If no photoinitiator is included in the composition, these eminuxs cannot effect photopolymerization. Although all amines, in combination with the said photoinitiators, cause an increase in the reaction rate, it has been found that the tertiary mines (eg trielylamine, trihexylamine, etc.) are the ones which give the best penetration and deep polymerization ability. Aminur with urumnhiskn groupv | however, are not suitable because they provide wise staining. if they are exposed to the effects of light for a long time.

When known combinations of benzophenone and amine are used in conjunction with Bis-MGA-resin, no photopolymeric ion can be obtained, or only mycoal. låfwgsmrl hširdningi [Jen according to the invention l'íjr «- ln; -; r |: | the unique combination of an alpha-diketone, as photoinitiators and a nmin g 7711798-3 as polymerization accelerator results, when using actinic radiation, a dental filling with high compressive strength.

This photopolymerizable dental composition may contain up to 85% filler material for repair purposes. At least 25% of this is barium-aluminum silicate, which, however, can be used throughout.

The presence of this filler material makes the repair material sufficiently permeable to X-rays. To create contrast with the natural dental material, a minimum of 6.5% barium oxide should be included in the composition. The second filler material may be lithium aluminum silicate. The particle size of these filler materials can range from less than 5 microns to about 10 microns. The filler material must be silane treated so as to obtain a satisfactory bond between the organic filler material and the organic material included in the composition. Suitable silane binders have a general formula RSiX3 R2SiX2 and R3SiX, where X may be a halogen, an alkoxy or hydroxy group, and R may be a vinyl, methacrylate, allyl, methyl alylitaconate, maleate, acrylate, itaconate, maleatacrylate- nnonitrut-, Fnmurut-, alkyl-. nryl, ulkenyl, krotonnt-, ninnumnt- ooh nllrakonut-, surbat ~ or glycldyl ~ group. When the filter treatment is complete, a monomolecular layer of the binder is present on the surfaces of the filler particles, which increases the adhesion between the filler material and the resin mass. Many other suitable filler materials, such as quartz and alumina may also be included.

A dental material according to the invention can be polymerized by exposing its activator to an energy source which produces a photoreaction. According to the present invention, actinic radiation is used, which can be produced, for example, by ultraviolet radiation from a diagnostic lamp of the type marketed by "Black Light Enstvrn", which is a division of "Spevl.r'or1ir: s Cot'p." lllesthury, Long lslznllll, NY ovh is designated "ñpectrolinv H-IUO". Such an apparatus contains a 100 W high-pressure mercury lamp, which has a radiation wavelength capacity between 3200 and # 200 Å. The pointed bulb used in this lamp is cooled by means of a fan. Such an amount of material, which is consumed during a normal dental filling, ie. 0.2-0.3 g, completely polymerized by irradiation with a lamp of the above type, for a period of 20-30 sec, if the lamp is kept about 10 cm from the filling. The material can be polymerized under these conditions to a depth of 2 mm; 7711708 ~ 3 The ingredients used are in the following proportions Weight sde l al: hurts (including inhibitor) 10 ~ 25 monomeric diluent (incl. Lnhihifor) 2 - S alpha-díkeLon, or derivatives thereof 0.001 - I nmi n O, U 1 - I : filler 70 - 85 The material is prepared as follows.

The resin is mixed with the monomeric diluent, photoinitiator and accelerator. The mixing takes place in a casting vessel during unloading with a rod of TEFLON (registered trademark). When the mixture has become uniform, barium-aluminum silicate is added and mixed well.

Finally, add other filler material in three or four small portions. The whole thing is mixed well and stored for a week before it is tried.

The well-mixed, heavy-duty paste packs a split, cylindrical shape of polyetrafluoroethylene with a single length of 12.5 mm and a diameter of 6 mm, which is open at both ends. Top and bottom Leaked: with tape of MYLAR (registered trademark) and pressudes, hd that you got smooth surfaces. The end portions now covered with MYLAR were exposed for I5 sec each to radiation from a Spektroline B-100 high-pressure mercury lamp placed at a distance of 10 cm. The split mold was then opened, and both sides of the test rod were subjected to nectinic acid / glass; below I ", sec. The total exposure time thus becomes 1 min. After IU minutes of aging, the polymerized product was tested and found to have a strength varying between 19.0 kp / mm 2 and 23.2 kp / mm 2. The strength increases to 28 , 1 kp / mmz if the product is allowed to age for two weeks In case of prolonged aging, the needle strength can be increased up to 31.6 kp / mmz.

E. ll Kempe weight grout Bis-GMA children (incl. MEHQ zoo ppm) 1a methyl methacrylates (incl. MEHQ 100 ppm) 3 h, h'-oxidibenzil 0.2 trihexylamine 0.2 brium ~ aluminum silicate 23 lilium-nluminum silicate 55.6 The landing was made as above described method, after which the solidity of the polymerized product was tested after the material was irradiated with a Spektroline B-100 lamp. After half a minute. Exposure was measured at 17.6 kp / mm 2, after one minute 21.2 kp / mm 2 and after 5 minutes 26.6 kp / mm 2.

Example II Weight percent B15 GMA resin (incl MEHQ 200 ppm) -18 1,3-butylene dimethacrylate (MEHQ 50 ppm) 3 N, N'-dimethoxybenzyl 0.08 N-methyldibutylamine 0.2 barium aluminum silicate 23 lithium aluminosilicate 55.72 The pour strength was tested in the same way as described above, nrh after irradiation for one minute with a Spektroline B-100 lamp a strength of 21.1 kp / mm¿f could be found Example III Weight percent Bis-GMA resin ( incl MEHQ 200 ppm) - 18 triethylene glycol dimethyl acrylate (incl MEHQ 100 ppm) 3 benzyl 0.08 N-methyldibulyline min. U, 2 harium-aluminum silicate 23 lithium-aluminum silicate 55.72 The strength of the polymerized material, after irradiation with a Spektroline B-100 lamp for 1 minute, was found to be 21 kp / mm2.

Example IV In the mixture of Example III, the monomeric diluent was replaced with the same quantity of 2-ethylhexyl acrylate. The strength after 1 minute of irradiation with a Spektroline B-100 lamp was found to be 22.5 kp / mmß. In general, acrylate monomers are more reactive than methacrylate and dimethacrylate monomers.

Example V Bis_GMA resin (incl. MEHQ 200 ppm) 13 methyl methacrylate (incl. MEHQ 100 ppm) 3 benzophenone 0, ü triethylamine 0, H barium-aluminum silicate 23 lithium-aluminum silicate 55.2 7711708-3 No curing could be observed despite the mixture «S för bvstrålníng fran en ápvkßrn fi ng H-IUU lampa under h minus.

Example VI In the mixture of Example V, benzyl was used instead of benzene. The mixture was packed in a 12.5 mm mold in the same manner as Lidi fi nre and subjected to horse rolling from a Spektrulinv H-IUU lamp for a total of 1 min. The strength of the polymerizing f) material was found to be 23.2 kp / mm '.

Example VII In the mixture according to Example V used% (kH5COCOCOC6H5 instead of benzophenone. After irradiation for 1 minute from a Spektroline B-IUU f) lamp, a pour strength of only 5.2 kp / mm "could be found.

Example VIII Weight sample n1s_GMA narc (incl MEHQ 200 ppm) 1H methyl methacrylate (incl MEHQ 100 ppm) 3 Ü, H'-oxidibenzyl 0.05 Leuraethylethylenediamine 0.00 barium-aluminum silicate 33 Lithium-aluminum silicate Example 55.86 The strength of the polymerized material, after irradiation with a Spektroline B-100 lamp below: 2 In min. was found to be 21.1 kp / mm.

Example IX Weighted product of β-GMA-narfs (incl. MEHQ zoo ppm) ns methyl methacrylate (incl. MEHQ 100 ppm) 3 μl, H '-oxydibenzyl 0.2 di-isopropylamine 0.2 barlum-Aluminum silicate 21 lithium-aluminum silicate 33.6 case a secondary amine was used. After mixing, the pulp was packed in a form of the above kind, and those covered with MYLAR tape were both coated for 15 seconds with a Speklroline H-IUO lamp.

When the mold was opened, the piece was broken in two, which indicates that the ruactin 7711708-3 TO was slow. In a second case, the covered ends were irradiated for ¶7sec each, after which the mold was opened. The specimen could be taken out completely, and irradiated for a further 30 seconds on each side.

The total exposure time was thus 2 min. The pressure gauge 0 of this test piece was found to be 18.3 kp / mmß.

Example X Example 11 was repeated with a primary amine, n-butylamino. The strength strength after 2 minutes of irradiation from a Spektroline B-100 lamp was found to be only 11.2 kp / mm¿, indicating that a tertiary amine is the most suitable additive.

Example XI In this case a slightly different resin was used. Gylcidyl ether of bisphenol-A is reacted with glacial acrylic acid, and the product bisphenol-A-bis (Beacrylate-2-hydroxypronyl) ether is used in preparing the composition Weight percent bisphenol-A-bis (3-acrylate-2-hydroxypropyl ether (incl. MEHQ 100 ppm) 1,6_nexanediyl1acrylate (incl. HQ 200 ppm) benzyl trihexylamine barium ~ aluminum silicate lithium aluminum silicate ... x Ulïå LWLJOOXAJOC '\ 1 NC N UD The mixture was treated in the same manner as described above. After irradiation for a total time of 1 minute from a Spektroline B-100 lamp, a compressive strength of 22.2 kp / mmg could be ascertained.

Example XII WIRELESS PRINCIPLE β1-GMA resin (incl. MEHQ 200 ppm) 23.9 1.6_hexanediyl diacrylate (incl. Zoo ppm) 3.9 benzyl _ 0.1 trihexylamine 0.26 silicon 72.3h min from a Spektrolíne B-100 lamp, was found to be 19.0 kp / mmg. 7711708-3 The most suitable composition for repairing teeth is Weight Proconi Bis ~ GMA Hurts (incl. MEHQ 300 ppm) 1H 1.6 hexanediol diacrylate (incl. MEHQ 100 ppm) 2.6 benzyl 0.03 trihexylamine 0.2 sodium aluminum silicate 21 lithium-aluminum silicate 5K, 82 Two kilograms of the above mixture were made using a mechanical mixer, and samples were made on the same hob as described in the oven. The bolymevised material was found. after a total irradiation time of 1 min from a Spektrokhneß-IUO lamp,, 2 be 2¿, 5 kp / mm.

Parts of the mixture were stored in the dark for more than three years at room temperature and samples were then taken. Hardening and half-strength properties were found unchanged, which confirms the material 'Jdngn Jagringslivslängd. lsïlïorsom tzmdlšrikzarml can: lnviínzla the tillhundalüíllrnzn pasta as it is, without additives or processing, he can perform londlugniugnr which are essentially completely free of entrapped air blues. This eliminates a number of mechanical defects and improves the surface structure so that a very smooth and hard surface is obtained. With a smooth wool, you run less risk of discoloration and bacterial infestation, and get a surface that is comfortable for the tongue.

Radiation with wavelengths between 2970 Ä and 3200 Ä can reeulteru in sunburn and carinogenesis. This emula hand can cause harmful photo reactions. The polymerization reaction repeated fi after the radiation was completely filtered up to] 3200 Ä, but no change in strength could be detected.

By inserting different optical filters between the lamp and the material, it could be stated that the most effective polymerisulionvu inlrffudv in radiation mollnn HUOO Ä and HSOU Å, ie. in the> ynli fi u area.

The curing tests were repeated with a tungsten halogen lamp, which is a source of visible light, and of a type manufactured by: General 7711708-3 Electric Co. The light was focused on the material using a 15 cm long bundle of fibers. It could then be stated that the material cured better after irradiation with a tungsten halogen lamp than with a mercury lamp.

In addition to pure repair purposes, the proposed base composition (as a single-phase paste, unlike conventional in-phase systems) can be used to fill pits and cracks, as a binder, to cover cavities or to restore enamel coating. Such work is usually called coating work.

All compositions for such purposes contain a photopolymerizable aromatic resin, e.g. Bie-GMA, a monomeric diluent, e.g. methacrylate, dimethacrylate, acrylate or diacrylate, a photoinitiator and an aocelerator. These compositions differ from the first ones in that they do not contain filler material. or only small amount of such. These compositions are polymerized in the mouth by actinic irradiation. Coating compositions generally contain 70 to 80 weight percent Bis-GMA resin, 30 to 20 weight percent methyl methacrylate with 100 ppm MEHQ inhibitor, 0.01 to 1 weight percent initiator and 0.01 to 1 weight percent accelerator.

The best recipe contains Bis-GMA resin (with 200 ppm MEHQ inhibitor) 75 parts methyl methacrylate (with 100 ppm MEHQ inhibitor) 23 parts benzyl 0.5 parts trihexylamine 0.5 parts hn | 'sihlur | blznnlnírnï, x | tan | Li llszxts zxv 1'í | l Fill again p; | ~ op. ~ U 'uvh spriekoxg as a heavenly part To klii in l | ¿1lir, f- heats and to make enamel. Although other methyl acrylates, acrylics, dimethyl acrylates, diacrylates or triacrylates can be used as monomeric diluents in the above composition, it has been found that methyl mutacrylate provides the best properties of a thin film. The amount of methyl methacrylate can be varied for the purpose of changing the viscosity of the mixture. A composition as above for coating work has a storage time of one year if it is stored airtight in a dark container. 7711708-3 Above, the compositions that have been found to be the best have been stated, but some modifications in the formulas are possible. An increase in the amount of diluent reduces the viscosity. An increase in the amount of filler increases the strength, but makes the paste thicker. The pour strength increases even if you increase the amount of benzyl. However, too much benzyl must be avoided, as it causes a yellowing of the paste and may result in polymerization if the material is temporarily exposed to light. The proposed combination of initiator and accelerator can be used to photopolymerize a plurality of monomeric resins.

The proposed dental material thus enables the dentist to use visible light to polymerize the material.

This avoids the risks associated with the use of ultraviolet light (Journal of the American Dental Association, Vol. 02).

April 1976). Although the description above contains certain selected proportions and approaches in connection with preferred applications, other suitable materials and approaches may be considered. activate, increase or modify the new composition and the result of its use. Such modifications and ramifications of the basic idea of the invention will be apparent to those skilled in the art which read the foregoing description, and are set forth in the appended claims.

Claims (11)

7711708-3 19 GATENT REQUIREMENTS 1. 1. A single-phase composition suitable for the treatment of tooth damage, characterized in that the various components therein contain the following parts by weight, Bisphenol A-bis (3 methacrylate-2-hydroxypropyl) ether 10 - 25 monomeric diluent containing an acrylate 2 - 5 initiator containing an alpha-diketone 0.001 ~ 1 accelerator containing a tertiary amine 0.1 - 2 barium and / or lithium aluminum silicate 0 - 85. 2. A composition according to claim 1, characterized in that it contains, a Bisphenol A-bis (3 methacrylate-2-hydroxypropyl) Weight 6 ether (inhibited by 200 ppm MEHQ) 18 methyl methacrylate (inhibited by 100 ppm MEHQ) 3 4,4'-oxidibenzil 0.2 trihexylamine 0.2 barium aluminum silicate 23 lithium aluminum silicate 55.6. 3. A composition according to claim 1, characterized in that it contains, Bisphenol A-bis (3 methacrylate-2-hydroxypropyl)% by weight or (inhibited by 200 ppm MEHQ) 18 1,3-butylene dimethacrylate (inhibited with 50 ppm MEHQ) 3 4,4'-dimethoxybenzyl 0.08 N-methyldibutylamine 0.2 barium aluminum silicate 23 lithium aluminum silicate 55.72. 7711708-3 45 4. A composition according to claim 1, characterized in that it contains, Bisphenol A-bis (3 methacrylate-2-hydroxypropyl) Weight% ether (inhibited by 200 ppm MEHQ) 18 triethylene glycol dimethacrylate (inhibited by 100 ppm MEHQ ) 3 benzyl 0.08 N-methyldibutylamine 0.2 barium aluminum silicate 23 lithium aluminum silicate 7 55.72. 5. A composition according to claim 1, characterized in that it contains, Bisphenol A-bis (3 methacrylate-2-hydroxypropyl) Weight% ether (inhibited by 200 ppm MEHQ) 18 methyl methacrylate (inhibited by 100 ppm MEHQ) 3 benzophenone 0.4 triethylamine 0.4 barium aluminum silicate 23 lithium aluminum silicate 55.2. 6. A composition according to claim 5, characterized in that the benzophenone is replaced by diphenyltriketone (C6H5COCOCOC6H5). 7. A composition according to claim 1, characterized in that it contains, Bisphenol A-bis (3 methacrylate-2-hydroxypropyl) Weight% ether (inhibited by 200 ppm MEHQ) 18 methyl methacrylate (inhibited by 100 ppm MEHQ) 3 4,4'-Cxidibenzil 0.05 tetraethylethylenediamine 0.09 barium aluminum silicate 23 lithium aluminum silicate 55.86. ? 7117ns-sl 16 8. A composition according to claim 1, characterized in that it contains, Bisphenol A-bis (3 methacrylate-2-hydroxypropyl) Weight% ether (inhibited by 200 ppm MEHQ) 18 ethyl methacrylate (inhibited by 100 ppm MEHQ) 3 .4,4'-oxidibenzil 0.2 diisopropylamine 0.2 barium aluminum silicate 23 lithium aluminum silicate U 55.6 9. A composition according to claim 1, characterized in that it contains, Bisphenol A-bis (3 methacrylate-2-hydroxypropyl) Weight% ether (inhibited by 100 ppm MEHQ) "18 1,6-hexanediol diacrylate (inhibited by 200 ppm MEHQ) ~ 3 benzyl 0o, os trihexylamine 0.2 barium phaluminum silicate 23 lithium aluminum silicate 55.72. 10. A composition according to claim 1, characterized in that it contains, Bisphenol A-bis (3 methacrylate-2-hydroxypropyl) Weight% ether (inhibited with 200 ppm MEHQ) 23.9 1,6-hexanediol diacrylate (inhibited with 200 ppm MEHQ) 3.9 benzyl 0.1 trihexylamine 0.26 barium and / or lithium aluminum silicate 72.34. 11. ll. Composition according to Claim 1, characterized in that it contains, Bisphenol A-bis (3 methacrylate-2-hydroxypropyl)% by weight of ether (inhibited by 200 ppm MEHQ) 18 1.6 hexanediol diacrylate (inhibited by 100 ppm MEHQ) 2.8 benzyl 0.08 trihexylamine _- 0.2 barium aluminum silicate - 23 lithium aluminum silicate 55.82.