Dental powder/liquid material-containing preparation accommodation bag and dispensing method for same
09931180 ยท 2018-04-03
Assignee
Inventors
Cpc classification
A61K6/30
HUMAN NECESSITIES
C08L33/08
CHEMISTRY; METALLURGY
A61K6/887
HUMAN NECESSITIES
C08L33/08
CHEMISTRY; METALLURGY
A61C13/0024
HUMAN NECESSITIES
A61C5/68
HUMAN NECESSITIES
A61K6/887
HUMAN NECESSITIES
C08L33/10
CHEMISTRY; METALLURGY
A61C5/50
HUMAN NECESSITIES
B65D81/3266
PERFORMING OPERATIONS; TRANSPORTING
A61K6/30
HUMAN NECESSITIES
A61C5/60
HUMAN NECESSITIES
C08L33/10
CHEMISTRY; METALLURGY
A61C19/005
HUMAN NECESSITIES
International classification
B65D25/08
PERFORMING OPERATIONS; TRANSPORTING
A61C5/50
HUMAN NECESSITIES
A61C5/68
HUMAN NECESSITIES
A61C5/60
HUMAN NECESSITIES
B65D81/32
PERFORMING OPERATIONS; TRANSPORTING
Abstract
A dental powder/liquid material-containing preparation accommodation bag, which suppresses entrainment of air in mixing a powder material and a liquid material for dispensing, is provided. A powder material 8 is accommodated in a powder material accommodation chamber 3 of a bag body 2, while a liquid material 9 dissolving the powder material 8 and changing into a pasty form, in cooperation with the powder material 8 is accommodated in a liquid material accommodation chamber 4 partitioned from the powder material accommodation chamber 3 by a weakened section 7. The weakened section 7 is ruptured by applying a pressing force to the bag body 2. As a result, the powder material accommodation chamber 3 and the liquid material accommodation chamber 4 communicate, to feed the liquid material accommodated in the liquid material accommodation chamber 4 into the powder material accommodation chamber 3. Then, the powder material 8 and the liquid material 9 changing into the pasty form are pressed within the powder material accommodation chamber 3 from the surfaces of the bag body 2 for dispensing.
Claims
1. A dental powder/liquid material-containing preparation accommodation bag, comprising: a bag body divided into a plurality of parts to form a plurality of sealed accommodation chambers; and a weakened section, formed between the accommodation chambers, for partitioning the accommodation chambers, the weakened section being formed to be rupturable by a pressing force applied to the bag body, the accommodation chambers being allowed to communicate after rupture of the weakened section, whereby contents accommodated in the accommodation chambers can be gathered within one of the accommodation chambers and can be mixed there, wherein the bag body is configured such that the plurality of accommodation chambers accommodate a powder material containing an organic polymer, and a liquid material dissolving the powder material and changing into a pasty form in cooperation with the powder material being accommodated separately in the accommodation chambers, wherein a volume of air is incorporated into at least one of the accommodation chambers, wherein the volume of the air at room temperature is in a range of 15 to 40% based on a total volume of the accommodation chamber for gathering and mixing the contents accommodated within the accommodation chambers, wherein the powder material and the liquid material changing into the pasty form after rupture of the weakened section can be pressed via surfaces of the bag body, and wherein the dental powder/liquid material is in such a configuration that the powder material contains a powder of a lower alkyl (meth)acrylate polymer, the liquid material contains a monomer, at least one of the powder material and the liquid material contains a polymerization initiator, and a final form of the powder material and the liquid material changing into the pasty form is a cured product.
2. The dental powder/liquid material-containing preparation accommodation bag according to claim 1, wherein an internal volume of the accommodation chamber for gathering and mixing the contents accommodated within the accommodation chambers is 1 to 3 cm.sup.3 relative to 1 g of a pasty substance obtained by blending the powder material and the liquid material.
3. The dental powder/liquid material-containing preparation accommodation bag according to claim 1, wherein a powder contained in the powder material of the dental powder/liquid material has a specific surface area, as measured by a nitrogen adsorption BET method, of 0.01 to 20 m.sup.2/g, and a bulk density, as measured in accordance with JIS K7365, of 0.05 to 1.0 g/cm.sup.3.
4. A dental powder/liquid material-containing preparation accommodation bag, comprising: a bag body divided into a plurality of parts to form a plurality of sealed accommodation chambers; and a weakened section, formed between the accommodation chambers, for partitioning the accommodation chambers, the weakened section being formed to be rupturable by a pressing force applied to the bag body, the accommodation chambers being allowed to communicate after rupture of the weakened section, whereby contents accommodated in the accommodation chambers can be gathered within one of the accommodation chambers and can be mixed there, wherein the bag body is configured such that the plurality of accommodation chambers accommodate a powder material containing an organic polymer, and a liquid material dissolving the powder material and changing into a pasty form in cooperation with the powder material being accommodated separately in the accommodation chambers, wherein a volume of air is incorporated into at least one of the accommodation chambers, wherein the volume of the air at room temperature is in a range of 15 to 40% based on a total volume of the accommodation chamber for gathering and mixing the contents accommodated within the accommodation chambers, wherein the powder material and the liquid material changing into the pasty form after rupture of the weakened section can be pressed via surfaces of the bag body, and wherein the dental powder/liquid material is in such a configuration that the powder material contains a powder of a lower alkyl (meth)acrylate polymer, the liquid material contains a liquid plasticizer, and a final form of the powder material and the liquid material changing into the pasty form is an elastic body.
5. The dental powder/liquid material-containing preparation accommodation bag according to claim 4, wherein an internal volume of the accommodation chamber for gathering and mixing the contents accommodated within the accommodation chambers is 1 to 3 cm.sup.3 relative to 1 g of a pasty substance obtained by blending the powder material and the liquid material.
6. The dental powder/liquid material-containing preparation accommodation bag according to claim 4, wherein a powder contained in the powder material of the dental powder/liquid material has a specific surface area, as measured by a nitrogen adsorption BET method, of 0.01 to 20 m.sup.2/g, and a bulk density, as measured in accordance with JIS K7365, of 0.05 to 1.0 g/cm.sup.3.
Description
BRIEF DESCRIPTION OF THE DRAWINGS
(1)
(2)
(3)
(4)
(5)
MODE FOR CARRYING OUT THE INVENTION
(6) A dental powder/liquid material-containing preparation accommodation bag, and a dispensing method therefor, in an embodiment of the present invention will be described with reference to the accompanying drawings.
(7)
(8) The preparation accommodation bag 1 is formed from a bag body 2, and its shape is rectangular in the present embodiment. The bag body 2 is formed by superposing transparent or translucent film sheets. If the bag body 2 is used with prints thereon, it is preferred to provide a transparent or translucent portion in it so that its interior can be observed.
(9) The bag body 2 is divided into a powder material accommodation chamber 3 accommodating a powder material, and a liquid material accommodation chamber 4 accommodating a liquid material, and the accommodation chambers 3 and 4 are adjacent to each other. These accommodation chambers 3, 4 are each preferably quadrilateral, but other shape can be used unless it does not impede mixing. Also, the corners of each chamber can be processed into a round shape in order to increase the efficiency of mixing. The peripheral edge 5 of the bag body 2 is sealed by thermal welding in a predetermined width. Between the powder material accommodation chamber 3 and the liquid material accommodation chamber 4 located adjacently, partition wall 7 for partitioning them is formed. In the present embodiment, the partition wall 7 is formed by thermal welding, but defines a weakened section welded weakly as compared with thermal welding at the peripheral edge 5 of the bag body 2. The weakened section is formed to have such strength that the partition wall 7 is ruptured, for example, upon application of pressing force to the liquid material accommodation chamber 4 when the powder material is accommodated in the powder material accommodation chamber 3, and the liquid material is accommodated in the liquid material accommodation chamber 4. The peripheral edge 5 subjected to thermal welding, on the other hand, has such strength as not to be ruptured against the pressing force.
(10) As the material for the bag body 2, a hard material which cannot deform is excluded, and the material may differ according to the type of the powder material or the liquid material accommodated in the accommodation chamber 3 or 4. Generally, however, various materials having such strength as not to be easily rupturable can be used. For example, synthetic resins such as polyethylene, polypropylene, polyester, polyamide, and ethylene-vinyl acetate, and an aluminum film can be used singly or as a mixture in the form of a sheet. Alternatively, a laminate sheet composed of two or more sheets laminated can be used. The thickness of the sheet is preferably 40 to 200 m.
(11) Under the procedures for formation of the preparation accommodation bag 1, two films are superposed, or one sheet is folded, to form a two-layer film. If the film is a continuous sheet, it is cut into a size corresponding to the single bag body 2, and thermally welded on right and left sides 5b, 5c, a lower side 5d, and the partition wall 7. From an upper side 5a of the bag body 2 which is open at this point in time, a desired amount of a powder material 8 is accommodated into the powder material accommodation chamber 3. Similarly, from the upper side 5a, a desired amount of a liquid material 9 is accommodated into the liquid material accommodation chamber 4. In the present embodiment, after a predetermined amount of air is incorporated into the powder material accommodation chamber 3 and/or the liquid material accommodation chamber 4, the upper side 5a of the bag body 2 is thermally welded. Thus, the entire periphery of the bag body 2 is sealed, and the partition wall 7 maintains sealing properties. Hence, the two accommodation chambers 3 and 4 are each formed in a sealed state.
(12) An example of a method for using the dental powder/liquid material-containing preparation accommodation bag 1 will be described.
(13) If its uses are a denture base liner, a dental repair resin, and a dental resin cement, it is preferred for the powder material to contain a powder of a lower alkyl(meth)acrylate polymer, for the liquid material to contain a monomer, and for at least one of the powder material and the liquid material to contain a polymerization initiator. The polymerization initiator is usually mixed with the powder material.
(14) In detail, in the case of the denture base liner and the dental repair resin, a (meth)acrylate polymer, such as a polyethyl methacrylate polymer, a poly(methyl methacrylate-ethyl methacrylate)copolymer, or a polymethyl methacrylate polymer, is used as the powder material. A (meth)acrylate monomer, such as methyl methacrylate, acetoacetoxyethyl methacrylate, or 1,9-nonanediol dimethacrylate, is used as the liquid material. As the polymerization initiator, benzoyl peroxide, dimethyl-p-toluidine, 1-cyclohexyl-5-ethylpyrimidinetrione, dilauryldimethylammonium chloride, or acetylacetone copper or the like is used.
(15) If the use is the dental resin cement, a poly(methyl methacrylate-ethyl methacrylate)copolymer or the like is used as the powder material. A (meth)acrylate monomer, such as methyl methacrylate, hydroxyethyl methacrylate, or urethane dimethyl dimethacrylate, is used as the liquid material. Tetraphenylboron triethanolamine salt, dibutylhydroxytoluene, or sodium p-toluenesulfinate is used as the polymerization initiator.
(16) In the case of the tissue conditioner as the use, it is preferred that the powder material contains a powder of a lower alkyl(meth)acrylate polymer, the liquid material contains a liquid plasticizer, and the final form of the powder material and the liquid material changing into a paste is an elastic body. In detail, a (meth)acrylate polymer, such as a polybutyl methacrylate polymer or a polyethyl methacrylate polymer, is used as the powder material. A liquid plasticizer such as diethyl sebacate or diethyl phthalate is used as the liquid material. The liquid plasticizer may be a polymeric plasticizer such as polybutyl acrylate or polypropyl acrylate.
(17) The powder of a lower alkyl(meth)acrylate polymer, used as the powder material, is excellent in polymerizability, imparts high mechanical strength to a cured product, and is satisfactory in solubility in the monomer. Thus, its specific surface area is preferably in the range of 0.01 to 20 m.sup.2/g, more preferably in the range of 0.05 to 15 m.sup.2/g. The specific surface area is a value measured by the nitrogen adsorption BET method. For the same reasons, the powder of a lower alkyl(meth)acrylate polymer has a bulk density of preferably 0.1 to 1.0 g/cm.sup.3, more preferably 0.15 to 0.8 g/cm.sup.3. The bulk density is a value measured in accordance with JIS K7365.
(18) The powder having a specific surface area and a bulk density in excess of the above upper limit values results in a viscosity rise too quick when the powder material and the liquid material are mixed. Thus, the operator has difficulty in obtaining a sufficient operating time. Moreover, the effect of preventing air intake into the paste tends to lower slightly. The powder having a specific surface area and a bulk density short of the above lower limit values, on the other hand, leads to rough particles, and insufficient solubility in the liquid material, in dental applications.
(19) As shown in
(20) The mixture turns into a highly flowable slurry owing to a dissolution action or the like, and gradually increases in viscosity, becoming pasty, with the progress of dissolution, the progress of a chemical reaction, and so on.
(21) The pressing operation for the mixture does not entrain air from outside the bag into the mixture, unlike kneading or stirring hitherto carried out, but conversely, exhibits the effect of forcing bubbles of air contained in the mixture out of the mixture.
(22) As shown in
(23) Such a dental material is directly applied for treatment to the patient in the dental examination room, or is used for operation, with the patient waiting in a waiting room. Thus, its handling is required to be completed in a short time for prompt treatment. In the present embodiment, dispensing can be started at rupture of the partition wall 7 of the preparation accommodation bag 1. Thus, the conventional labor of charging suitable amounts of the powder material and the liquid material into a blending cup can be saved, and the operating time until obtainment of a suitable viscosity is of the order of 1 minute to 5 minutes.
(24) Conventionally, the mixture has been mixed using a spatula, so that the entrainment of air bubbles can be somewhat prevented by the operator's skill, etc. In the present embodiment, a dental material with few air bubbles can be always obtained regardless of the skill. Moreover, air taken between the particle gaps or voids of the powder can also be forced out of the paste by the pressing force exerted via the surfaces of the bag body at the time of mixing.
(25) Other characteristics required of dental materials are miscibility, quick viscosity increase, handleability, easy shapability, and prompt curing. In these respects as well, the dental material of the present invention causes no hindrance, and rivals or exceeds conventional dental materials.
EXAMPLES
(26) Next, test examples concerned with the present embodiment will be described, but the present invention is in no way limited by the following test examples.
(27) Using the above-described preparation accommodation bag, a denture base liner and a dental repair resin (Test Example 1), a tissue conditioner (Test Example 2), and a dental resin cement (Test Example 3) were dispensed, and compared with conventional methods.
Test Example 1: Test for Dispensing of Denture Base Liner and Dental Repair Resin
(28) [Materials Used]
(29) (1) The following materials were used as powder materials: Polyethyl methacrylate polymer (PEMA) Particle size 35 m: specific surface area 0.3 m.sup.2/g, bulk density 0.68 g/cm.sup.3 (supplier: Sekisui Plastics Co., Ltd.: EMA35) Particle size 10 m: specific surface area 0.4 m.sup.2/g, bulk density 0.48 g/cm.sup.3 (supplier: Sekisui Plastics Co., Ltd.: EMA10) Poly (methyl methacrylate-ethyl methacrylate)copolymer (P(MMA-EMA)) Particle size 80 m: specific surface area 0.05 m.sup.2/g, bulk density 0.75 g/cm.sup.3 (supplier: Negami Chemical Industrial Co., Ltd.: D100) Particle size 30 m: specific surface area 0.3 m.sup.2/g, bulk density 0.63 g/cm.sup.3 (supplier: Negami Chemical Industrial Co., Ltd.: D200) Polymethyl methacrylate polymer (PMMA) Particle size 20 m: specific surface area 0.2 m.sup.2/g, bulk density 0.51 g/cm.sup.3 (supplier: Negami Chemical Industrial Co., Ltd.: D250ML) Particle size 4 m: specific surface area 0.8 m.sup.2/g, bulk density 0.34 g/cm.sup.3 (supplier: Negami Chemical Industrial Co., Ltd.: D350ML-3A) Particle size 0.2 m: specific surface area 15 m.sup.2/g, bulk density 0.18 g/cm.sup.3 (supplier: Soken Chemical & Engineering Co., Ltd.: MP1451) (2) The following materials were used as liquid materials: Methyl methacrylate (MMA) (supplier: Wako Pure Chemical Industries, Ltd.) Acetoacetoxyethyl methacrylate (AAEM) (supplier: Nippon Synthetic Chemical Industry Co., Ltd.) 1,9-Nonanediol dimethacrylate (ND) (supplier: Shin-Nakamura Chemical Co., Ltd.) (3) The following materials were used as polymerization initiators: Benzoyl peroxide (BPO) (supplier: Wako Pure Chemical Industries, Ltd.) Dimethyl-p-toluidine (DMPT) (supplier: Tokyo Chemical Industry Co., Ltd.) 1-Cyclohexyl-5-ethylpyrimidinetrione (CEPT) Dilauryldimethylammonium chloride (LMAC) (supplier: TAKEMOTO OIL & FAT CO., LTD.) Acetylacetone copper (ACu) (supplier: Wako Pure Chemical Industries, Ltd.)
(30) The methods for preparation of the powder material and the liquid material were as follows:
(31) The powder material in Examples 1 to 9 and Comparative Example 1 was obtained by adding 1 part by weight of EPO, as a polymerization initiator component, to 100 parts by weight of PEMA35. The liquid material in these examples was obtained by adding 20 parts by weight of ND and 0.3 part by weight of DMPT, as a polymerization initiator component, to 80 parts by weight of AAEM.
(32) The powder material in Example 10 was prepared in the same manner as above, except that PEMA35 in Examples 1 to 9 was replaced by PEMA10. The liquid material in this example was prepared in the same manner as above.
(33) The powder material in Examples 11, 12 and Comparative Example 2 was prepared in the same manner as above, except that PEMA35 in Examples 1 to 9 was replaced by PEMA10 or P (MMA-EMA) The liquid material in these examples was prepared in the same manner as above, except that MMA was used as a substitute.
(34) The powder material in Examples 13 to 16 was obtained by adding 1.5 parts by weight of CEPT and 0.01 part by weight of ACu to 100 parts by weight of the powder component shown in Table 1. The liquid material therein was obtained by adding 0.03 part by weight of LMAC to 100 parts by weight of MMA.
(35) Reference Example 1 concerns a curable material composed of two liquid materials. One of the liquid materials was obtained by adding 1 part by weight of BPO to 100 parts by weight of AAEM. The other liquid material was obtained by adding 40 parts by weight of ND and 0.3 part by weight of DMPT to 60 parts by weight of AAEM.
(36) In connection with the testing methods, the mixing method X shown in Table 1 represents dispensing using the preparation accommodation bag of the present invention, while the mixing method Y represents a method which comprises weighing the powder and the liquid into a blending cup, and blending them in an open state with the use of a spatula, as in customary practice.
(37) The void ratio shown in Table 1 was determined by the percentage of the void volume to the internal volume of the powder material accommodation chamber 3 where the liquid material is fed in and mingled with the powder material.
Void ratio(%)=void volume/internal volume of powder material accommodation chamber100
(38) The void volume was determined by a volume obtained by subtracting the total volume of the charged powder material and liquid material from the internal volume of the powder material accommodation chamber measured beforehand.
Void volume=internal volume of powder material accommodation chamber(volume of powder material+volume of liquid material)
(39) The volume of the powder material was calculated by dividing the weight of the powder material by its bulk density (powder material weight/bulk density), whereas the volume of the liquid material was calculated by dividing the weight of the liquid material by the specific gravity of the liquid (liquid material weight/liquid specific gravity).
(40) The air bubble incorporation in Table 1 was evaluated by observing with a magnifying glass air bubbles confirmed on the surface of a cured product/elastic body measuring 6 mm (diameter)1 mm, voids generated in the presence of fine air bubbles, or blushed regions; and finding the proportion of their area to the total area. In preparing the cured product, the liquid was confirmed to have spread throughout the powder, whichever method of mixing was adopted. Then, the system was blended for a further period of 5 seconds, and a proper amount of the blend was poured into a mold or the like having a hole of the above size. The blend poured in was allowed to stand without pressure contact, cured, and then flattened on the surface using a waterproof abrasive paper (No. 800). An air bubble incorporation rate of less than 10% was evaluated as A, a value of 10% or more, but less than 20% was evaluated as B, a value of 20% or more, but less than 30% was evaluated as C, and a value of 30% or more was evaluated as D. Less air bubble incorporation gained a higher evaluation.
(41) For the flexural strength in Table 1, a mold having a rectangular hole with a width of 4 mm, a thickness of 2 mm, and a length of 40 mm was charged with a curable material, which was cured in the same manner as in the measurement of the unpolymerized amount. The resulting cured product was subjected to a flexural test using a strength tester. Under the following conditions, a crosshead speed of 1 mm/min, and a spanning distance of 15 mm, a 3-point bending test was conducted to find the flexural strength.
(42) The color test (resistance to discoloration) in Table 1 was conducted in the following manner: A cured product measuring 10 mm10 mm2 mm was prepared, stored for 2 hours in water at 37 C., and then measured for (L*), (a*), and (b*) before coloration by means of a color difference meter. Then, the specimen was immersed in a 5 wt. % aqueous solution of coffee, and stored for 24 hours at 40 C. with stirring. After storage, the specimen was washed with water, dried, and then measured again for (L*), (a*), and (b*) by means of the color difference meter. Using the differences (L*) (a*), and (b*) between those parameters before and after the color test, the amount of color (E*) was calculated from the following equation:
Amount of color (E*)={(L*).sup.2+(a*).sup.2+(b*).sup.2}.sup.1/2
(43) The difference (L*) represents a difference in brightness, and the differences (a*) and (b*) represent differences in color chroma. The lower the value of (E*), the smaller change in color differences.
(44) The results of the test are shown in Table 1.
(45) TABLE-US-00001 TABLE 1 Powder material Liquid Polymerization Particle size Specific surface area material initiator Type (m) (m.sup.2/g) Type Type Ex. 1 PEMA 35 0.3 AAEM/ND BPO/DMPT Ex. 2 Ex. 3 Ex. 4 Ex. 5 Ex. 6 Ex. 7 Ex. 8 Ex. 9 Ex. 10 10 0.4 Ex. 11 P(MMA-EMA) 80 0.05 MMA BPO/DMPT Ex. 12 30 0.3 Ex. 13 CEPT/ACu/LMAC Ex. 14 PMMA 20 0.2 Ex. 15 4 0.8 Ex. 16 0.2 15 Comp. Ex. 1 PEMA 35 0.3 AAEM/ND BPO/DMPT Comp. Ex. 2 P(MMA-EMA) 80 0.05 MMA Ref. Ex. 1 Liquid material (1) AAEM/BPO Liquid material (2) AAEM/ND/DMPT Flexural Void ratio Air bubble strength Color test Mixing method (%) incorporation (MPa) E Ex. 1 X 5 A 77 1.1 Ex. 2 8 A 78 1.2 Ex. 3 10 A 80 1.1 Ex. 4 15 A 81 1.1 Ex. 5 20 A 80 0.9 Ex. 6 30 A 80 0.8 Ex. 7 40 A 81 0.9 Ex. 8 45 B 74 1.6 Ex. 9 60 C 69 2.1 Ex. 10 30 A 80 1.1 Ex. 11 30 A 89 0.6 Ex. 12 A 90 0.6 Ex. 13 A 91 0.5 Ex. 14 A 89 0.8 Ex. 15 A 89 0.7 Ex. 16 B 79 1 Comp. Ex. 1 Y D 55 3.8 Comp. Ex. 2 D 59 3.6 Ref. Ex. 1 A
(46) Reference to Table 1 shows that the proportions of the materials were the same, and the same conditions (excluding the void ratio) were adopted except for the mixing method, in Examples 1 to 9 and Comparative Example 1. It is seen in Table 1, however, that the results in all cases, including air bubble incorporation, were better in Examples 1 to 9 using the preparation accommodation bag of the present invention than in Comparative Example 1.
(47) Similarly, it is seen that the proportions of the materials were the same, and the same conditions were adopted except for the mixing method, in Example 11 and Comparative Example 2, but that the results in all cases were better in Example 11 using the preparation accommodation bag of the present invention than in Comparative Example 2.
(48) From Examples 1 to 9, moreover, it is noted that changes in the void ratio led to differences in the air bubble incorporation, flexural strength, and color effect, thus influencing the quality. Besides, the air bubble incorporation in the range of less than 10% corresponded to the void ratio in the range of 5 to 40%.
(49) The flexural strength was 55 to 59 MPa in the conventional method, and 69 to 91 MPa in the Examples of the present invention. These findings confirmed that the strength of the cured product in the final form was greatly enhanced in the present invention. Moreover, a decline in discoloration (improvement in discoloration resistance) was observed in the present invention.
(50) From Reference Example 1, it was observed that when liquid materials were mixed by the conventional method, incorporation of air bubbles was minimal, unlike the use of a powder-liquid mixture material. This findings showed that when a powder material and a liquid material were mixed, air bubbles were incorporated more easily than when liquid materials were mixed.
Test Example 2: Test for Dispensing of Denture Tissue Conditioner
(51) [Materials Used]
(52) (1) The following materials were used as powder materials: Polybutyl methacrylate polymer (PBMA) Particle size 40 m: specific surface area 0.3 m.sup.2/g (supplier: Negami Chemical Industrial Co., Ltd.: D200B) Polyethyl methacrylate polymer (PEMA) Particle size 35 specific surface area 0.3 m.sup.2/g (supplier: Sekisui Plastics Co., Ltd.: EMA35) (2) The following materials were used as liquid materials: Polybutyl acrylate (PEA): Synthetic product Polypropyl acrylate (PPA): Synthetic product Diethyl sebacate (SE) (supplier: Wako Pure Chemical Industries, Ltd.)
(53) As powder materials and liquid materials in Examples 17 to 28 and Comparative Examples 3 to 5, the powder material and liquid material components shown in Table 2 were used singly as such.
(54) In connection with test samples, X in the mixing method shown in Table 2 represents the one dispensed using the preparation accommodation bag of the present invention, while Y in the mixing method represents that obtained by weighing the powder and the liquid into a blending cup, and blending them in an open state with the use of a spatula, as by a conventional method.
(55) The void ratio and the air bubble incorporation shown in Table 2 were evaluated by the same methods as in the aforementioned Test Example 1.
(56) The results of the test are shown in Table 2.
(57) TABLE-US-00002 TABLE 2 Powder material Par- Specific Air ticle surface Liquid Void bubble size area material Mixing ratio incorpo- Type (m) (m.sup.2/g) Type method (%) ration Ex. 17 PBMA 40 0.3 PBA X 5 A Ex. 18 8 A Ex. 19 10 A Ex. 20 15 A Ex. 21 20 A Ex. 22 30 A Ex. 23 40 A Ex. 24 45 B Ex. 25 60 C Ex. 26 PPA 30 A Ex. 27 SE A Ex. 28 PEMA 35 0.3 SE A Comp. PBMA 40 0.3 PBA Y D Ex. 3 Comp. PPA D Ex. 4 Comp. SE D Ex. 5
(58) Reference to Table 2 shows that the same conditions (excluding the void ratio) were adopted except for the mixing method, in Examples 17 to 25 and Comparative Example 3. It is seen in Table 2, however, that Examples 17 to 25 using the preparation accommodation bag of the present invention were better than Comparative Example 3 in terms of less incorporation of air bubbles. Besides, the air bubble incorporation in the range of less than 10% corresponded to the void ratio in the range of 5 to 40%.
Test Example 3: Test for Dispensing of Dental Resin Cement
(59) [Materials Used]
(60) (1) The following materials were used as powder materials: Poly(methyl methacrylate-ethyl methacrylate)copolymer (P(MMA-EMA)) Particle size 30 m: specific surface area 0.3 m.sup.2/g (supplier: Negami Chemical Industrial Co., Ltd.: D200) Pulverized polymethyl methacrylate polymer (PMMA1) Particle size 20 m (synthetic product of Tokuyama Dental Corp.: For the method of synthesis, see Japanese Patent No. 5110923) Sulfonate-containing acidic resin (SP-01) (synthetic product of Tokuyama Dental Corp.: For the method of synthesis, see Japanese Patent No. 5110923) Fluoroaluminosilicate glass filler (FASG) (supplier: Tokuyama Dental Corp.: basicity-abated product: For the method of abating treatment, see Japanese Patent No. 3669563) -Methacryloxypropyltrimethoxysilane-treated spherical silica-zirconia filler (G1) Particle size 0.52 m (synthetic product of Tokuyama Dental Corp.) (2) The following materials were used as liquid materials: Methyl methacrylate (MMA) (supplier: Wako Pure Chemical Industries, Ltd.) Hydroxyethyl methacrylate (HEMA) (supplier: Wako Pure Chemical Industries, Ltd.) Urethanedimethyl dimethacrylate (UDMA) (supplier: KYOEISHA CHEMICAL CO., LTD.) (3) The following materials were used as polymerization initiators/inhibitors: Tetraphenylboron triethanolamine salt (PhBTEOA) (supplier: Wako Pure Chemical Industries, Ltd.) Dibutylhydroxytoluene (BHT) (supplier: Tokyo Chemical Industry Co., Ltd.) Sodium p-toluenesulfinate (pTsNa) (4) The following materials were used as pretreatment materials: Mixture of 2-methacryloyloxyethyl dihydrogen phosphate and bis(2-methacryloyloxyethyl)hydrogen phosphate (PM) Bis(maltolato)oxovanadium (IV) (BMOV) (supplier: Sigma-Aldrich Corporation) Urethanedimethyl dimethacrylate (UDMA) (supplier: KYOEISHA CHEMICAL CO., LTD.) Acetone (supplier: Wako Pure Chemical Industries, Ltd.) Isopropanol (IPA) (supplier: Wako Pure Chemical Industries, Ltd.)
(61) The methods for preparation of the powder materials and the liquid materials were as follows:
(62) The powder material in Example 29 and Comparative Example 6 was obtained by adding 5 parts by weight of SP-01 to a resin powder mixture (for the powder material) composed of 60 parts by weight of PMMA-EMA1 and 40 parts by weight of PMMA1. The liquid material in these examples was obtained by adding 4 parts by weight of PhBTEOA to a polymerizable monomer mixture (for the liquid material) composed of a mixture of 80 parts by weight of MMA, 10 parts by weight of HEMA, 10 parts by weight of UDMA, and 0.1 part by weight of BHT.
(63) The powder material in Example 30 and Comparative Example 7 was obtained by mixing 100 parts by weight of FASG, 10 parts by weight of G1, 0.5 part by weight of BPO, and 1 part by weight of pTSNa. The liquid material in these examples was obtained by mixing 100 parts by weight of PM, 250 parts by weight of HEMA, 150 parts by weight of UDMA, and 0.5 part by weight of DMPT.
(64) The pretreatment material used in Example 29 and Comparative Example 6 was obtained by adding 0.2 part by weight of BMW to 20 parts by weight of PM, 30 parts by weight of water, 5 parts by weight of UDMA, 35 parts by weight of acetone, and 10 parts by weight of IPA.
(65) In connection with test samples, X in the mixing method shown in Table 3 represents the one dispensed using the preparation accommodation bag of the present invention, while Y in the mixing method represents that obtained by weighing the powder and the liquid into a blending cup, and blending them in an open state with the use of a spatula, as in customary practice.
(66) The void ratio and the air bubble incorporation shown in Table 3 were evaluated by the same methods as in the aforementioned Test Example 1.
(67) The adhesive force in Table 3 was investigated in the following manner: A bovine front tooth was extracted within 24 hours after slaughter and, with water being poured thereover, it was sanded down with a #800 emery paper to expose the enamel or dentinal plane so as to be parallel to the labial surface. Then, compressed air was blown against this plane for about 10 seconds to dry it. Then, a double-coated tape having a hole of 3 mm in diameter was secured to the plane to form a simulated cavity. Within the simulated cavity, a dental primer was coated on the tooth surface, and allowed to stand for 20 seconds. Then, compressed air was blown against it for about 5 seconds. Then, the dental adhesive of the Example or the Comparative Example was charged into the simulated cavity, whereafter a stainless attachment with a diameter of 8 mm was pressure-contacted therewith to prepare an adhesion test piece. The adhesion test piece was immersed in water at 37 C. for 24 hours, and then the strength of its adhesion to the tooth was measured at a crosshead speed of 1 mm/min with the use of a tensile tester (Autograph, produced by Shimadzu Corporation).
(68) The results of the test are shown in Table 3.
(69) TABLE-US-00003 TABLE 3 Powder material Specific Void Adhesive Particle surface Liquid material Mixing ratio Air bubble force Type size (m) area Type method (%) incorporation (MPa) Ex. 29 P(MMA-EMA) 30 0.3 MMA/HEMA/UDMA X 30 A 29.3 Ex. 30 FASG HEMA/UDMA 30 A 18.1 Comp. Ex. 6 P(MMA-EMA) 40 0.3 MMA/HEMA/UDMA Y D 22.0 Comp. Ex. 7 FASG HEMA/UDMA D 11.3
(70) Reference to Table 3 shows that the particle size was different between Examples 29, 30 and Comparative Examples 6, 7, but Examples 29, 30 using the preparation accommodation bag of the present invention were better than Comparative Examples 6, 7 in terms of less incorporation of air bubbles. Besides, the adhesive force was 22.0 MPa in Comparative Example 6 and 29.3 MPa in Example 29, while it was 11.3 MPa in Comparative Example 7 and 18.1 MPa in Example 30. These findings show the product dispensed using the preparation accommodation bag had greater adhesive force.
(71) The results of Tests 1 to 3 show the following:
(72) In connection with the denture base liner, the dental repair resin, the tissue conditioner, and the dental resin cement, the mixing method X showed marked decreases in the amount of air bubbles incorporated as compared with the mixing method Y.
(73) The flexural strength was clearly higher in the Examples than in the Comparative Examples, as seen from Table 1. A primary factor in enhancing the adhesive strength is considered to be an increase in the rate of internal polymerization ascribed to a decrease in air bubble incorporation due to absence of contact with outside air, and a decrease in the amount of entrained air.
(74) The present invention has been described in detail above based on the embodiment with reference to the accompanying drawings. However, the present invention is in no way limited to the foregoing embodiment, but other changes or modifications can be made without departing from the scope of the invention.
(75) In the above embodiment, for example, the bag body 2 is divided into the powder material accommodation chamber 3 and the liquid material accommodation chamber 4. However, the bag body 2 may be divided into three or more accommodation chambers, and the contents of these accommodation chambers may be mixed together.
(76) In the above-described embodiment, the preparation accommodation bag is shaped like a sheet with a small thickness, but a bag of a three-dimensional structure can be used for practice of the present invention.
EXPLANATION OF LETTERS OR NUMERALS
(77) 1 Preparation accommodation bag
(78) 2 Bag body
(79) 3 Powder accommodation chamber
(80) 4 Liquid accommodation chamber
(81) 5 Peripheral edge
(82) 7 Weakened section
(83) 8 Powder material
(84) 9 Liquid material