Cationically curable dental materials
View Patent ↗The invention relates to a polymerizable dental material containing: (a) 3 to 80 wt. % of one or more cationically curable monomers; (b) 3 to 90 wt. % of one or more radio-opaque fillers; (c) 0.01 to 25 wt. % of initiators, retarders and/or accelerators, and; (d) 0 to 25 wt. % of auxiliary agents, whereby the cited percentages each refer to the total weight of the material. Filler (b) is produced by means of a melting method and is selected so that it has a refractive index of n D =1.49–1.54, so that the viscosity of the polymerizable dental material, after a period of at least 9 months during which it was stored at a temperature ranging from 20 to 25° C., has a value of +/−50 % of the initial value measured 24 hours after the polymerizable dental material was produced, and so that the polymerizable dental material has a reactivity of the type that, once polymerization is initiated, the amount of the maximum heat flux generated by the dental material equals at least 0.8 mW/mg, and this maximum heat flux is attained within a period of no longer than 60s.
1. A process for the preparation of a polymerizable dental material, the process comprising:
(a) preparing a filler from individual components by a melting process at a temperature of at least 1550° C.;
(b) grinding the filler obtained in (a) to a particle size of 0.1–15μm;
(c) surface-treating the filler obtained in (b); and
(d) incorporating the surface-treated filler in a matrix comprising:
(i) cationically curable monomers; and
(ii) initiators, retarders, accelerators, auxiliary agents, or combinations thereof; wherein the filler is an X-ray opaque filler comprising at least 65 weight % of SiO 2 , and wherein the surface-treated filler has a refractive index of n D =1.49–1.54.
2. The process of claim 1 , wherein the melting process is carried out at a temperature of at least 1600° C.
3. The process of claim 1 , wherein the melting process is carried out in an inductively heated furnace at 1550–3000° C. over 5 to 60 minutes, or in a plasma melting unit at 2000–3000° C.
4. The process of claim 1 , wherein the polymerizable dental material comprises:
(a) 3 to 80 weight % of one or more cationically curable monomers;
(b) 3 to 90 weight % of the surface-treated filler;
(c) 0.01 to 25 weight % of initiators, retarders and/or accelerators; and
(d) 0 to 25 weight % of auxiliary agents;
wherein the percentages are in each case with reference to the total weight of the material;
wherein the filler (b) exhibits a refractive index of n D =1.49–1.54;
wherein the polymerizable dental material, at a storage temperature of 20 to 25° C. for at least 9 months, has a viscosity of +/−50% of the starting value, which is measured 24 hours after preparation of the polymerizable dental material; and
wherein the polymerizable dental material has a reactivity such that, after the start of polymerization, the material generates a maximum heat flux of at least 0.8 mW/mg within at most 60 seconds.
5. The process of claim 1 , wherein the polymerizable dental material is a dental bonding material.
6. The process of claim 1 , wherein the polymerizable dental material is a dental fixing material.
7. The process of claim 1 , wherein the surface-treated filler has an X-ray opacity corresponding to an aluminum X-ray equivalent of at least 100%.
8. The process of claim 1 , wherein the surface-treated filler has a refractive index of n D =1.50–1.53.
9. The process of claim 1 , wherein the surface-treated filler has an average particle size of 0.1–15 μm and a specific surface of 1–35 m 2 /g.
10. The process of claim 9 , wherein the surface-treated filler has an average particle size of 1–4 μm and a specific surface of 3–9 m 2 /g.
11. The process of claim 1 , wherein the surface-treated filler comprises a total of at most 35 weight % of one or more of the oxides of the elements from the 5 th period, 6 th period, or both; a total of at most 3 weight % of one or more of the oxides from the first main group; and a total of at most 3 weight % of the oxides B 2 O 3 , Al 2 O 3 , and P 2 O 5 .
12. The process of claim 1 , wherein the surface treated filler comprises a total of at most 35 weight % of one or more of the oxides chosen from the group consisting of Y 2 O 3 , lanthanide oxides, ZrO 2 , HfO 2 , Nb 2 O 5 , Ta 2 O 5 , In 2 O 3 , SnO 2 , and WO 3 ; a total of at most 3 weight % of one or more of the oxides from the first main group; and a total of at most 3 weight % of the oxides B 2 O 3 , Al 2 O 3 , and P 2 O 5 .
13. The process of claim 1 , wherein the polymerizable dental material comprises:
(a) 3 to 80 weight % of one or more cationically curable monomers;
(b) 3 to 90 weight % of one or more X-ray-opaque fillers;
(c) 0.01 to 25 weight % of initiators, retarders, accelerators, or combinations thereof; and
(d) 0 to 25 weight % of auxiliary agents;
wherein the percentages are in each case with reference to the total weight of the material.
14. The process of claim 1 , wherein the polymerizable dental material, at a storage temperature of 20 to 25° C. for at least 9 months, has a viscosity of +/−50% of the starting value, which is measured 24 hours after preparation of the polymerizable dental material.
15. The process of claim 1 , wherein the polymerizable dental material has a reactivity such that, after the start of polymerization, the material generates a maximum heat flux of at least 0.8 mW/mg within at most 60 seconds.
16. The process of claim 4 , wherein the melting process is carried out at a temperature of at least 1600° C.
17. The process of claim 4 , wherein the melting process is carried out in an inductively heated furnace at 1550–3000° C. over 5 to 60 minutes, or in a plasma melting unit at 2000–3000° C.