CN110464656B - Resin material for dental prosthesis and preparation method thereof - Google Patents

Resin material for dental prosthesis and preparation method thereof Download PDF

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CN110464656B
CN110464656B CN201910807145.5A CN201910807145A CN110464656B CN 110464656 B CN110464656 B CN 110464656B CN 201910807145 A CN201910807145 A CN 201910807145A CN 110464656 B CN110464656 B CN 110464656B
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resin material
antioxidant
dental
antibacterial agent
mixture
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CN110464656A (en
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张耀超
左艳萍
张琳梅
崔晓明
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Xian Medical University
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Xian Medical University
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Abstract

The invention discloses a resin material for dental filling, which comprises the following components in percentage by mass: 20-30% of calcium hydroxy phosphate, 10-15% of polymethyl acrylate, 5-10% of triethyl citrate, 5-10% of diethyl dodecyl phosphonate, 10-15% of calcium alginate, 2-8% of an antibacterial agent, 5-10% of an antioxidant, 1-3% of a stabilizer and 20-25% of double distilled water, wherein the sum of the mass percentages of the components is 100%. The invention also discloses a preparation method of the resin material for dental prosthesis; the resin material for dental prosthesis prepared by the invention has better compressive strength and hardness, does not contain heavy metal, is environment-friendly, and has simple and convenient preparation method and easy popularization.

Description

Resin material for dental prosthesis and preparation method thereof
Technical Field
The invention belongs to the field of tooth restoration, and particularly relates to a resin material for dental filling and a preparation method of the resin material for dental filling.
Background
Teeth are very important organs of humans. The decayed tooth is also called as a decayed tooth or a decayed tooth, is a bacterial disease, is a decayed lesion of the tooth, and is a decayed hole formed on the surface of the tooth, the decayed hole is larger and larger, so that the tooth can be completely destroyed, and if the decayed tooth is not treated, the tooth crown can be completely destroyed and disappeared, and people cannot chew the decayed tooth.
The method for treating decayed tooth mainly adopts filling material to fill, i.e. firstly, the damaged decayed tooth is removed, and a certain shape is made by using a tool, so that the filling material is filled and the shape of the tooth defect is recovered.
Disclosure of Invention
The invention aims to provide a resin material for dental prosthesis, which has the characteristics of long service life and high hardness.
The invention also provides a preparation method of the resin material for dental filling.
The first technical scheme adopted by the invention is that the resin material for dental filling comprises the following components in percentage by mass: 20-30% of calcium hydroxy phosphate, 10-15% of polymethyl acrylate, 5-10% of triethyl citrate, 5-10% of diethyl dodecyl phosphonate, 10-15% of calcium alginate, 2-8% of an antibacterial agent, 5-10% of an antioxidant, 1-3% of a stabilizer and 20-25% of double distilled water, wherein the sum of the mass percentages of the components is 100%.
The first technical solution adopted by the present invention is further characterized in that,
the antibacterial agent is a mixture of nano silver powder and total matrine powder, and the mass ratio of the total matrine powder to the nano silver powder is 1: 1-3.
The stabilizer is p-methoxyphenol.
The antioxidant is o-methoxyphenol.
The particle size range of the nano silver powder is 50-100 nm.
The particle size of the nano silver powder is 50-60 nm.
The second scheme adopted by the invention is as follows: a preparation method of a resin material for dental filling is implemented according to the following specific steps:
step 1, respectively weighing 20-30% of calcium hydroxy phosphate, 10-15% of polymethyl acrylate, 5-10% of triethyl citrate, 5-10% of diethyl dodecyl phosphonate, 10-15% of calcium alginate, 2-8% of an antibacterial agent, 5-10% of an antioxidant, 1-3% of a stabilizer and 20-25% of double distilled water according to the weight percentage, wherein the sum of the mass percentages of the components is 100%;
step 2, mixing the calcium hydroxy phosphate, the polymethyl acrylate, the triethyl citrate, the diethyl dodecyl phosphonate and the calcium alginate weighed in the step 1, then performing ball milling for 1-2 hours, and performing ultrasonic oscillation for a period of time to obtain a mixture;
and 3, adding the antibacterial agent, the stabilizer and the antioxidant which are weighed in the step 1 into the mixture obtained in the step 2, mixing and stirring uniformly, and obtaining the tooth filling resin material when the mixture is in a uniform paste shape.
The invention adopting the second technical proposal is also characterized in that,
ball milling is carried out in a planetary high-energy ball milling tank, the ball milling speed is 550-650rmp, the ball milling time is 1-2 hours, and the ultrasonic oscillation time is 0.5-1 hour.
The temperature range during mixing is 60-70 ℃, the mixing and stirring speed is 550-650rmp, and the stirring time is 1-2 h.
The antibacterial agent in the step 1 is a mixture of nano silver powder and total matrine powder, the mass ratio of the total matrine powder to the nano silver powder is 1:1-3, the stabilizer is p-methoxyphenol, and the antioxidant is o-methoxyphenol.
The invention has the following beneficial effects: the tooth filling material has the advantages that the mixed powder of the nano silver powder and the total matrine powder is added, so that the tooth filling material has good sterilization effect, the nano silver powder has good sterilization effect, the total matrine is a natural sterilization substance, can be effectively sterilized and acidproof, has a wide sterilization range and high biocompatibility, and the sterilization effect of the tooth filling material prepared by the invention is much better than that of the existing tooth filling material and can exert the sterilization effect for a long time by combining the nano silver powder and the total matrine powder; the resin material for dental prosthesis prepared by the invention has better compressive strength and hardness, is not easy to shrink in volume, does not contain heavy metal, is environment-friendly, and has simple and convenient preparation method and easy popularization.
Detailed Description
The present invention will be described in detail with reference to the following embodiments.
The invention relates to a resin material for dental filling, which comprises the following components in percentage by mass: 20-30% of calcium hydroxy phosphate, 10-15% of polymethyl acrylate, 5-10% of triethyl citrate, 5-10% of diethyl dodecyl phosphonate, 10-15% of calcium alginate, 2-8% of an antibacterial agent, 5-10% of an antioxidant, 1-3% of a stabilizer and 20-25% of double distilled water, wherein the sum of the mass percentages of the components is 100%.
The antibacterial agent is a mixture of nano silver powder and total matrine powder, and the mass ratio of the total matrine powder to the nano silver powder is 1: 1-3.
The stabilizer is p-methoxyphenol.
The antioxidant is o-methoxyphenol.
The particle size range of the nano silver powder is 50-100 nm.
Preferably, the particle size of the nano silver powder is 50 nm.
The invention relates to a preparation method of a resin material for dental filling, which is implemented according to the following specific steps:
step 1, respectively weighing 20-30% of calcium hydroxy phosphate, 10-15% of polymethyl acrylate, 5-10% of triethyl citrate, 5-10% of diethyl dodecyl phosphonate, 10-15% of calcium alginate, 2-8% of an antibacterial agent, 5-10% of an antioxidant, 1-3% of a stabilizer and 20-25% of double distilled water according to the weight percentage, wherein the sum of the mass percentages of the components is 100%.
And 2, adding the calcium hydroxy phosphate, the polymethyl acrylate, the triethyl citrate, the diethyl dodecyl phosphonate and the calcium alginate weighed in the step 1 into a planetary high-energy ball milling tank, ball milling for 1-2 hours at the speed of 550-650rmp, and then carrying out ultrasonic oscillation for 0.5-1 hour to obtain a mixture.
And 3, adding the antibacterial agent, the stabilizer and the antioxidant weighed in the step 1 into the mixture obtained in the step 2, mixing and stirring uniformly at the temperature of 60-70 ℃, wherein the stirring speed is 550-650rmp, stirring for 1-2 hours, and obtaining the dental filling resin material when the mixture is in a uniform paste shape.
The antibacterial agent is a mixture of nano silver powder and total matrine powder, and the mass ratio of the total matrine powder to the nano silver powder is 1: 1-3.
The stabilizer is p-methoxyphenol.
The antioxidant is o-methoxyphenol.
The invention adopts the mixed powder of the total matrine and the nano silver powder as the antibacterial agent, the biocompatibility of the total matrine is better and safe, and the antibacterial range is widerThe nano silver powder has an antibacterial effect which cannot be compared with a conventional antibacterial agent due to the quantum effect, the small-size effect and the extremely large specific surface area, and is high in safety and lasting in effect. The antibacterial property of the nano silver is far greater than that of the traditional silver bactericide, and the nano silver with smaller particle size has better bactericidal effect. The calcium hydroxy phosphate is selected as tooth filling material because it can pass through the fluoric matter in toothpaste-sodium fluoride (NaF) and calcium hydroxy phosphate [ Ca ]10(PO4)6(OH)2]The calcium fluorophosphate with luster and stronger corrosion resistance can be generated after the reaction.
The chemical equation for the reaction is: ca10(PO4)6(OH)2 + 2NaF= Ca10(PO4)6F2 + 2NaOH
Example 1
The invention relates to a preparation method of resin for dental filling, which is specifically implemented according to the following steps:
step 1, respectively weighing 24% of calcium hydroxy phosphate, 10% of polymethyl acrylate, 10% of triethyl citrate, 5% of diethyl dodecyl phosphonate, 11% of calcium alginate, 3% of nano silver powder, 3% of total matrine powder, 8% of o-methylphenol, 1% of p-methoxyphenol and 25% of double distilled water according to the weight percent, wherein the sum of the mass percentages of the components is 100%.
And 2, adding the calcium hydroxy phosphate, the polymethyl acrylate, the triethyl citrate, the diethyl dodecyl phosphonate, the calcium alginate and the double distilled water weighed in the step 1 into a planetary high-energy ball milling tank, carrying out ball milling for 1h at the speed of 550rmp, and then carrying out ultrasonic oscillation for 0.5h to obtain a mixture.
And 3, adding the nano silver powder, the total matrines, the o-cresol and the p-methoxyphenol weighed in the step 1 into the mixture obtained in the step 2, mixing and stirring uniformly at the temperature of 60 ℃, wherein the stirring speed is 550rmp, and stirring for 1.5 hours to obtain the tooth filling resin material.
Example 2
The invention relates to a preparation method of resin for dental filling, which is specifically implemented according to the following steps:
step 1, weighing 20% of calcium hydroxy phosphate, 15% of polymethyl acrylate, 5% of triethyl citrate, 5% of diethyl dodecyl phosphonate, 15% of calcium alginate, 2% of nano silver powder, 6% of total matrine powder, 10% of o-methylphenol, 2% of p-methoxyphenol and 20% of double distilled water according to the weight percent, wherein the sum of the mass percentages of the components is 100%.
And 2, adding the calcium hydroxy phosphate, the polymethyl acrylate, the triethyl citrate, the diethyl dodecyl phosphonate and the calcium alginate weighed in the step 1 into a planetary high-energy ball milling tank, carrying out ball milling for 1.5h at the speed of 650rmp, and then carrying out ultrasonic oscillation for 1h to obtain a mixture.
And 3, adding the antibacterial agent, the stabilizer and the antioxidant which are weighed in the step 1 into the mixture obtained in the step 2, mixing and stirring uniformly at the temperature of 65 ℃, wherein the stirring speed is 650rmp, and stirring for 2 hours to obtain the tooth filling resin material.
Example 3
The invention relates to a preparation method of resin for dental filling, which is specifically implemented according to the following steps:
step 1, weighing 30% of calcium hydroxy phosphate, 8% of polymethyl acrylate, 7% of triethyl citrate, 10% of diethyl dodecyl phosphonate, 5% of calcium alginate, 1% of nano silver powder, 1% of total matrine powder, 5% of o-methylphenol, 3% of p-methoxyphenol and 30% of double distilled water according to the weight percent, wherein the sum of the mass percentages of the components is 100%.
And 2, adding the calcium hydroxy phosphate, the polymethyl acrylate, the triethyl citrate, the diethyl dodecyl phosphonate and the calcium alginate weighed in the step 1 into a planetary high-energy ball milling tank, carrying out ball milling for 2 hours at the speed of 600rmp, and then carrying out ultrasonic oscillation for 1 hour to obtain a mixture.
And 3, adding the antibacterial agent, the stabilizer and the antioxidant which are weighed in the step 1 into the mixture obtained in the step 2, mixing and stirring uniformly at the temperature of 70 ℃, wherein the stirring speed is 600rmp, and stirring for 1 hour to obtain the tooth filling resin material.
And (3) performance testing:
the products obtained in the embodiments 1 to 3 of the present invention were subjected to performance tests, 20 prepared dental filling materials were randomly selected in each embodiment, rockwell hardness values of the dental filling materials were measured and averaged, and the test results are shown in table 1:
TABLE 1 product Performance test data
Example 1 Example 2 Example 3
Rockwell hardness number 339 345 340
Compressive strength MPa 251 245 242

Claims (5)

1. The resin material for dental prosthesis is characterized by comprising the following components in percentage by mass: 20-30% of calcium hydroxy phosphate, 10-15% of polymethyl acrylate, 5-10% of triethyl citrate, 5-10% of diethyl dodecyl phosphonate, 10-15% of calcium alginate, 2-8% of an antibacterial agent, 5-10% of an antioxidant, 1-3% of a stabilizer and 20-25% of double distilled water, wherein the sum of the mass percentages of the components is 100%;
the antibacterial agent is a mixture of nano silver powder and total matrine powder, and the mass ratio of the total matrine powder to the nano silver powder is 1: 1-3;
the particle size range of the nano silver powder is 50-100 nm;
the antioxidant is o-methoxyphenol;
the stabilizer is p-methoxyphenol;
the preparation method of the resin material for dental filling specifically comprises the following steps:
step 1, respectively weighing 20-30% of calcium hydroxy phosphate, 10-15% of polymethyl acrylate, 5-10% of triethyl citrate, 5-10% of diethyl dodecyl phosphonate, 10-15% of calcium alginate, 2-8% of an antibacterial agent, 5-10% of an antioxidant, 1-3% of a stabilizer and 20-25% of double distilled water according to the weight percentage, wherein the sum of the mass percentages of the components is 100%;
step 2, mixing the calcium hydroxy phosphate, the polymethyl acrylate, the triethyl citrate, the diethyl dodecyl phosphonate and the calcium alginate weighed in the step 1, then ball-milling for 1-2 hours, and then carrying out ultrasonic oscillation to obtain a mixture;
and 3, adding the antibacterial agent, the stabilizing agent and the antioxidant which are weighed in the step 1 into the mixture obtained in the step 2, mixing and stirring uniformly, and obtaining the resin material for dental care when the mixture is in a uniform paste shape.
2. The resin material for dental filling as claimed in claim 1, wherein the nano silver powder has a particle size of 50 to 60 nm.
3. A method for preparing a dental resin material according to claim 1, comprising the steps of:
step 1, respectively weighing 20-30% of calcium hydroxy phosphate, 10-15% of polymethyl acrylate, 5-10% of triethyl citrate, 5-10% of diethyl dodecyl phosphonate, 10-15% of calcium alginate, 2-8% of an antibacterial agent, 5-10% of an antioxidant, 1-3% of a stabilizer and 20-25% of double distilled water according to the weight percentage, wherein the sum of the mass percentages of the components is 100%;
step 2, mixing the calcium hydroxy phosphate, the polymethyl acrylate, the triethyl citrate, the diethyl dodecyl phosphonate and the calcium alginate weighed in the step 1, then carrying out ball milling for 1-2 hours, and then carrying out ultrasonic oscillation to obtain a mixture;
and 3, adding the antibacterial agent, the stabilizing agent and the antioxidant which are weighed in the step 1 into the mixture obtained in the step 2, mixing and stirring uniformly, and obtaining the resin material for dental care when the mixture is in a uniform paste shape.
4. The method for preparing a dental resin material as claimed in claim 3, wherein the ball milling in step 1 is performed in a planetary high energy ball milling tank, the ball milling rate is 550-650rmp, the ball milling time is 1-2h, and the ultrasonic oscillation time is 0.5-1 h.
5. The method for preparing dental resin material as claimed in claim 3, wherein the mixing temperature in step 3 is 60-70 ℃, the mixing and stirring rate is 550-650rmp, and the stirring time is 1-2 h.
CN201910807145.5A 2019-08-29 2019-08-29 Resin material for dental prosthesis and preparation method thereof Active CN110464656B (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2006055350A2 (en) * 2004-11-12 2006-05-26 Combe Incorporated Denture liner, denture liner kit and method for making a denture liner
JP2007328325A (en) * 2006-05-10 2007-12-20 Shiyoufuu:Kk Tooth with caries for gnathic teeth model, its manufacturing method and its application
CN101444565A (en) * 2008-12-31 2009-06-03 内蒙古永业生物技术有限责任公司 Method for preparing seed of lightyellow sophora oral bacteriostasis dropping liquid
CN108524292A (en) * 2018-04-25 2018-09-14 佛山科学技术学院 A kind of compound filling tooth material and preparation method thereof
CN109199875A (en) * 2018-09-12 2019-01-15 佛山市佛冠义齿有限公司 A kind of dental filling resin material and preparation method thereof
CN109998930A (en) * 2019-03-26 2019-07-12 南京师范大学 A kind of wear-resisting lower shrinkage dental filling composite material and preparation method

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20040266906A1 (en) * 2001-10-26 2004-12-30 Joachim Klee Hydrolysis stable self-etching,self-priming adhesive

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2006055350A2 (en) * 2004-11-12 2006-05-26 Combe Incorporated Denture liner, denture liner kit and method for making a denture liner
JP2007328325A (en) * 2006-05-10 2007-12-20 Shiyoufuu:Kk Tooth with caries for gnathic teeth model, its manufacturing method and its application
CN101444565A (en) * 2008-12-31 2009-06-03 内蒙古永业生物技术有限责任公司 Method for preparing seed of lightyellow sophora oral bacteriostasis dropping liquid
CN108524292A (en) * 2018-04-25 2018-09-14 佛山科学技术学院 A kind of compound filling tooth material and preparation method thereof
CN109199875A (en) * 2018-09-12 2019-01-15 佛山市佛冠义齿有限公司 A kind of dental filling resin material and preparation method thereof
CN109998930A (en) * 2019-03-26 2019-07-12 南京师范大学 A kind of wear-resisting lower shrinkage dental filling composite material and preparation method

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