CN112107491A - Easily-mixed high-comfort silicone rubber oral impression material and preparation method thereof - Google Patents
Easily-mixed high-comfort silicone rubber oral impression material and preparation method thereof Download PDFInfo
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- CN112107491A CN112107491A CN202011013361.1A CN202011013361A CN112107491A CN 112107491 A CN112107491 A CN 112107491A CN 202011013361 A CN202011013361 A CN 202011013361A CN 112107491 A CN112107491 A CN 112107491A
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/90—Compositions for taking dental impressions
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Abstract
The invention relates to an easily-mixed high-comfort silicone rubber oral cavity impression material which comprises the following components in parts by weight: 15-45 parts of one or more low-volatility dimethyl polysiloxane containing at least two vinyl groups per molecule, 1-5 parts of one or more dimethyl polysiloxane containing at least two or more Si-H groups per molecule, 5-15 parts of fumed silica, 45-75 parts of superfine filler, 0.5-10 parts of softener, 0.05-2 parts of wetting agent and 0.5-3 parts of essence; the catalyst component comprises the following components in parts by weight: 15-45 parts of one or more low-volatility dimethyl polysiloxane containing at least two vinyl groups per molecule, 0.2-5 parts of platinum catalyst, 5-25 parts of fumed silica, 45-70 parts of superfine filler, 0.5-10 parts of softener, 0.05-2 parts of wetting agent and 0.5-3 parts of essence. Compared with the prior art, the invention has the advantages of low viscosity, no stickiness, easy mixing and high comfort level in the entrance.
Description
Technical Field
The invention relates to the technical field of oral impressions, in particular to an easily-mixed high-comfort silicone rubber oral impression material and a preparation method thereof.
Background
Taking and making of the oral impression is the first process in the oral cavity repairing work, and the quality of the oral impression is directly related to the final repairing effect. At present, the commercially available impression materials such as alginates, agar, condensed silicone rubbers, ordinary addition silicone rubbers and polyether rubbers have more or less defects. Alginate impression materials have the defects that the shrinkage is large, and the state of teeth cannot be accurately reflected; the agar impression material has the defects of easy breaking and large brittleness; the condensed silicone rubber has the advantages that small molecules are separated in the curing process, peculiar smell is generated, the volume is slightly shrunk, and the precision in the rubber impression material is lowest; polyether rubbers have high manufacturing cost and high market price, and are not easy to popularize; the common addition type silicone rubber has the defects of difficult mixing, easy hand sticking, slow curing in winter, too fast curing in summer, and poor operability and entrance comfort.
The invention patent CN103655212B discloses a room temperature addition silicone rubber putty type oral cavity impression material applied to a primary impression, which is prepared by blending two components, namely a matrix component and a catalytic component, wherein the matrix component consists of vinyl silicone oil containing more than two vinyl functional groups, hydrogen-containing silicone oil containing more than three Si-H functional groups, a compatibilizer, a reinforcing agent and other auxiliary agents according to a certain proportion. The catalytic component consists of vinyl silicone oil containing more than two vinyl functional groups, a catalyst which is a complex of chloroplatinic acid and the vinyl silicone oil, a compatibilizer, a reinforcing agent and other auxiliary agents according to a certain proportion. The invention has reasonable formula and easy operation, the cured material has elastic recovery of 99.8 percent, the curing time is 3-5min, the Shore hardness is about 65, and the fine duplication is 0.02mm and can be clearly seen, so that the invention can be used for manufacturing accurate dental crowns, dental bridges, false teeth, occlusion records and oral cavity tissue impression taking. But the material of the invention is not soft enough, is not easy to mix and has lower comfort level when entering the mouth; and the use of the general formula in winter and summer can not accurately control the internal curing time under the conditions of both low temperature in winter and high temperature in summer, and the user experience is poor.
The invention patent CN111053698A discloses an oral cavity impression material, which comprises: a catalyst component and a matrix component; the catalyst comprises the following components in parts by weight: 15-40 parts of vinyl silicone oil, 0.5-20 parts of silicone resin, 55-80 parts of reinforcing filler and 0.5-1.5 parts of platinum catalyst; the matrix comprises the following components in parts by weight: 5-25 parts of vinyl silicone oil, 0.5-20 parts of silicone resin, 55-80 parts of reinforcing filler and 5-20 parts of hydrogen-containing silicone oil. The oral cavity impression material is prepared from a catalyst and a matrix, wherein the matrix comprises a base polymer and a cross-linking agent, the catalyst comprises the base polymer and the catalyst, vinyl silicone oil and silicone resin are used as base substances, hydrogen-containing silicone oil is used as the cross-linking agent, and reinforcing fillers are added into the two components, so that the prepared impression material can accurately record occlusion relation and overcomes the defects of low hardness, easy deformation and breakage. But the invention also has the problems of uneasy mixing and low comfort in entrance. Although the material of the invention uses the silicone resin as the reactive filler, the hardness of the material before curing is reduced to a certain extent, but the material is still not soft enough, is not easy to mix and has lower comfort level when entering the mouth; and still use general formula in winter and summer, can't accurately control giving consideration to intraoral curing time under winter low temperature and summer high temperature situation, user experience is relatively poor.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide an easily-mixed high-comfort silicone rubber oral impression material and a preparation method thereof.
The purpose of the invention can be realized by the following technical scheme: an easily-mixed high-comfort silicone rubber oral impression material, which comprises the components of the agent and the catalyst component in equal mass ratio and is characterized in that,
the components of the agent comprise the following components in parts by weight: 15-45 parts of one or more low-volatility dimethyl polysiloxane containing at least two vinyl groups per molecule, 1-5 parts of one or more dimethyl polysiloxane containing at least two or more Si-H groups per molecule, 5-15 parts of fumed silica, 45-75 parts of superfine filler, 0.5-10 parts of softener, 0.05-2 parts of wetting agent and 0.5-3 parts of essence;
the catalyst component comprises the following components in parts by weight: 15-45 parts of one or more low-volatility dimethyl polysiloxane containing at least two vinyl groups per molecule, 0.2-5 parts of platinum catalyst, 5-25 parts of fumed silica, 45-70 parts of superfine filler, 0.5-10 parts of softener, 0.05-2 parts of wetting agent and 0.5-3 parts of essence.
Furthermore, the low-volatility dimethyl polysiloxane containing two vinyl groups has the viscosity of 0.05-10 Pa.s, and comprises vinyl-terminated polydimethylsiloxane, vinyl-terminated polyvinyl polydimethylsiloxane, polyvinyl polyether and vinyl methyl siloxane ring bodies. The CAS number of the vinyl-terminated polydimethylsiloxane mentioned above is 68083-19-2, the CAS number of the vinyl-terminated polyvinyl polydimethylsiloxane is 68083-18-1, the CAS number of the vinylmethylsiloxane ring is 2554-06-5, and commercial products such as the winning series of Polymer VS10000, Polymer RV100, MVC and the like.
Further, the dimethylpolysiloxane containing two or more Si-H groups described herein include trimethylsilyl-terminated hydrogenous polyorganosiloxanes having CAS number 63148-57-2, commercially available products such as the winning Crosslinker 190 series.
The dimethyl polysiloxane containing vinyl and the dimethyl polysiloxane containing Si-H groups are safe macromolecular polymers, and are non-toxic and tasteless; under the catalysis of platinum catalyst, the rapid addition reaction at a lower temperature can be realized, the material can be cured, and no by-product is generated in the curing process.
The platinum catalyst is a winter type catalyst, and comprises a Kanst platinum catalyst diluted with the vinyl silicone oil (i.e., the vinyl-containing dimethylpolysiloxane), the content of platinum atoms is 0.10-1.00%, and the CAS number of the Kanst platinum catalyst is 68478-92-2.
The platinum catalyst is a summer-type catalyst comprising a Kansted platinum catalyst diluted with the vinyl silicone oil (i.e., the vinyl-containing dimethylpolysiloxane) in an amount of 0.10 to 0.80% in terms of platinum atom, and the CAS number of the Kansted platinum catalyst is 68478-92-2.
According to the characteristics of the addition reaction and a large number of practical tests of related materials sold in the market, the fact that the reaction speed containing the addition reaction is obviously influenced due to the difference of the environmental temperature in winter and summer (the temperature of the material is difficult to be consistent with the temperature in a short time) can be found, the formula is universal in winter and summer, in order to take account of the use in winter and summer, the use of the catalyst concentration which is compromised can cause short operation time at high temperature in summer, the hardness of the impression material at the inlet is higher, extra force is needed, even the impression taking fails, and in winter, in order to ensure full curing, the stay time in the mouth can be only prolonged, on one hand, the user experience is influenced, and on the other hand, the impression is inaccurate due to unexpected actions of users possibly occurring in the. The new material adopts different catalyst formulas in winter and summer: that is, the reaction time can be controlled more accurately by using a catalyst formulation with high activity in the case of low temperature in winter and a catalyst formulation with slightly lower activity in the case of high temperature in summer. The method and the device have the advantages that the operation time of operators is ensured to be abundant, and the fast curing in the mouth is realized, so that more comfortable user experience is obtained.
The specific surface area of the fumed silica is 110 +/-20 m2The grain diameter is 10-40 nm.
The superfine filler comprises one or more of kaolin, silica micropowder, calcium carbonate, talcum powder and calcium phosphate, and the particle size is 400-200 nm.
The fumed silica is a white, loose, amorphous, nontoxic, tasteless, odorless, and pollution-free non-metallic oxide, is an excellent dental filler, has an excellent reinforcing effect on silicone rubber, and can improve hardness. Meanwhile, the price is relatively high; therefore, one or more of kaolin, silica micropowder, calcium carbonate, talcum powder and calcium phosphate with moderate price are selected as the volume filling filler. Finally, the reasonable formula proportion realizes hardness and strength and simultaneously can consider the cost.
The softener comprises refined paraffin oil and polyvinyl polyether, is pure and transparent liquid and has the viscosity of 50-500 mPas.
The wetting agent comprises polyether modified silicone oil, the silicon content of the polyether modified silicone oil is 10-20%, and the surface tension is 15-30 mN/m;
the essence is spearmint essence, mint essence or fruit essence, is universal and is used by the public.
The preparation method of the easily-mixed high-comfort silicone rubber oral cavity impression material comprises the following steps:
(1) weighing 15-45 parts by weight of one or more low-volatility dimethylpolysiloxanes containing at least two vinyl groups per molecule, 1-5 parts by weight of one or more dimethylpolysiloxanes containing at least two or more Si-H groups per molecule, 5-15 parts by weight of fumed silica, 45-75 parts by weight of superfine filler, 0.5-10 parts by weight of softener, 0.05-2 parts by weight of wetting agent and 0.5-3 parts by weight of essence, kneading in a kneader to obtain the component, and then carrying out vacuum degassing for later use;
(2) weighing 15-45 parts by weight of one or more low-volatility dimethylpolysiloxanes containing at least two vinyl groups per molecule, 0.2-5 parts by weight of platinum catalyst, 5-25 parts by weight of fumed silica, 45-70 parts by weight of superfine filler, 0.5-10 parts by weight of softener, 0.05-2 parts by weight of wetting agent and 0.5-3 parts by weight of essence, kneading in a kneader to obtain a catalyst component, and then carrying out vacuum degassing for later use;
(3) weighing the components of the agent and the catalyst in equal mass, and uniformly mixing to obtain the silicone rubber impression material.
Compared with the prior art, the invention has the following advantages:
1. the dimethyl polysiloxane raw material with low volatility is used, so that the safety and environmental protection are realized, gloves are not needed, and the contact is relieved;
2. due to the introduction of the softening agent and the wetting agent, the invention can realize low consistency (25-35) and no stickiness, and can realize rapid mixing by hands;
3. the superfine filler system and the additive organic silicon system realize high precision (20-40 microns), accurately obtain a stamp, have excellent mechanical property and long-term stable size (< 1.0%);
4. the curing time in the mouth can be accurately controlled to ensure the use comfort by different special catalyst designs;
5. the price of the raw materials is moderate, the cost is easy to control, and the rapid popularization is easier.
Detailed Description
The following examples are given for the detailed implementation and specific operation of the present invention, but the scope of the present invention is not limited to the following examples.
Example 1
Weighing 30g of vinyl-terminated polydimethylsiloxane with the viscosity of 10 Pa.s and 10g of vinyl-terminated polyvinyl polydimethylsiloxane with the viscosity of 0.1 Pa.s, weighing 23g of polyvinyl polyether with the viscosity of 0.05 Pa.s, weighing 0.2g of vinyl methyl siloxane ring body, uniformly mixing, adding trimethylsilyl-terminated hydrogen-containing polyorganosiloxane, uniformly mixing and stirring 10g of hydrogen-containing polyorganosiloxane and 0.2g of polyether modified silicone oil; weighing 1.5g of spearmint essence, uniformly mixing again, adding 70g of kaolin with 3000 meshes, 90g of silicon micropowder with 3000 meshes and 12g of fumed silica, kneading in a kneader for 20min to obtain the component mixture, and then carrying out vacuum degassing for later use.
Weighing 52g of vinyl-terminated polydimethylsiloxane with the viscosity of 10 Pa.s and 10g of vinyl-terminated polydimethylsiloxane with the viscosity of 0.1 Pa.s, weighing 10g of polyvinyl polyether with the viscosity of 0.05 Pa.s and 5g of platinum catalyst, and uniformly stirring; 0.2g of polyether modified silicone oil and 1.5g of spearmint essence are weighed and uniformly mixed again, 90g of 3000-mesh kaolin, 70g of 3000-mesh silicon micropowder and 10g of fumed silica are kneaded in a kneader for 20min to obtain a catalyst component mixture, and then vacuum degassing is carried out for later use.
According to the following steps of 1: 1 weighing (measuring) the same amount of the present component and the catalyst component, and uniformly mixing to prepare the silicone rubber impression material.
Example 2
Weighing 50g of vinyl-terminated polydimethylsiloxane with the viscosity of 20 Pa.s and 15g of vinyl-terminated polydimethylsiloxane with the viscosity of 0.1 Pa.s, weighing 9g of polyvinyl polyether with the viscosity of 0.03 Pa.s, weighing 0.3g of vinyl methyl siloxane ring body, uniformly mixing, adding trimethylsilyl-terminated hydrogen-containing polysiloxane, uniformly mixing and stirring 6.5g and 0.7g of polyether modified silicone oil; weighing 2.5g of mint essence, uniformly mixing again, adding 50g of 5000-mesh light calcium carbonate, 65g of 3500-mesh talcum powder and 22g of fumed silica, kneading in a kneader for 20min to obtain a mixture of the components, and then carrying out vacuum degassing for later use.
Weighing 48g of vinyl-terminated polydimethylsiloxane with the viscosity of 20 Pa.s and 17g of vinyl-terminated polydimethylsiloxane with the viscosity of 0.1 Pa.s, weighing 10g of polyvinyl polyether with the viscosity of 0.03 Pa.s and 3.5g of platinum catalyst, and uniformly stirring; 0.2g of polyether modified silicone oil and 2.5g of mint essence are weighed and mixed uniformly again, 50g of 5000-mesh light calcium carbonate, 65g of 3500-mesh talcum powder and 20g of fumed silica are kneaded in a kneader for 20min to obtain a catalyst component mixture, and then vacuum degassing is carried out for later use.
According to the following steps of 1: 1 weighing (measuring) the same amount of the present component and the catalyst component, and uniformly mixing to prepare the silicone rubber impression material.
Example 3
Weighing 70g of vinyl-terminated polydimethylsiloxane with the viscosity of 10 Pa.s and 20g of vinyl-terminated polydimethylsiloxane with the viscosity of 0.08 Pa.s, weighing 2.5g of refined paraffin oil with the viscosity of 0.01 Pa.s, weighing 0.6g of divinyl tetramethylsiloxane ring, uniformly mixing, adding trimethylsilyl-terminated hydrogen-containing polysiloxane, uniformly mixing and stirring 3.7g and 0.2g of polyether modified silicone oil; weighing 1.0g of fruit essence, uniformly mixing again, adding 55g of 5000-mesh silicon micropowder, 45g of 5000-mesh calcium phosphate and 15g of fumed silica, kneading in a kneader for 20min to obtain a component mixture, and then degassing in vacuum for later use.
Weighing 65g of vinyl-terminated polydimethylsiloxane with the viscosity of 10 Pa.s and 22g of vinyl-terminated polydimethylsiloxane with the viscosity of 0.1 Pa.s, weighing 3.0g of refined paraffin oil with the viscosity of 0.01 Pa.s and 2.5g of platinum catalyst, and uniformly stirring; 0.3g of polyether modified silicone oil and 1.5g of fruit essence are weighed and uniformly mixed again, 55g of 5000-mesh silicon powder, 45g of 5000-mesh calcium phosphate and 5g of fumed silica are kneaded in a kneader for 20min to obtain a catalyst component mixture, and then vacuum degassing is carried out for later use.
According to the following steps of 1: 1 weighing (measuring) the same amount of the present component and the catalyst component, and uniformly mixing to prepare the silicone rubber impression material.
The properties of the impression materials obtained in the above examples are shown in the following table
The properties of the impression materials obtained in the above examples after curing are shown in the following table
Example 1 | Example 2 | Example 3 | |
Hardness (Shao's A) | 67 | 65 | 61 |
Dimensional stability% | 0.9 | 1.0 | 0.7 |
Details of replication (μm) | 25 | 20 | 27 |
Breaking strength MPa | 2.17 | 2.23 | 2.36 |
Elongation at break% | 99.5 | 97.4 | 89.8 |
Example 4
The formulation of the easy-mix high comfort silicone rubber oral impression material of this example is shown in the following table:
example 5
The formulation of the easy-mix high comfort silicone rubber oral impression material of this example is shown in the following table:
the properties of the impression materials obtained in the above examples after curing are shown in the following table
Example 4 | Example 5 | |
Hardness (Shao's A) | 65 | 66 |
Dimensional stability% | 0.9 | 0.8 |
Details of replication (μm) | 26 | 23 |
Breaking strength MPa | 2.27 | 2.33 |
Elongation at break% | 93.5 | 88.1 |
。
Claims (10)
1. The silicone rubber oral impression material is easy to mix and high in comfort level, and comprises the following components in parts by weight: 15-45 parts of one or more low-volatility dimethyl polysiloxane containing at least two vinyl groups per molecule, 1-5 parts of one or more dimethyl polysiloxane containing at least two or more Si-H groups per molecule, 5-15 parts of fumed silica, 45-75 parts of superfine filler, 0.5-10 parts of softener, 0.05-2 parts of wetting agent and 0.5-3 parts of essence;
the catalyst component comprises the following components in parts by weight: 15-45 parts of one or more low-volatility dimethyl polysiloxane containing at least two vinyl groups per molecule, 0.2-5 parts of platinum catalyst, 5-25 parts of fumed silica, 45-70 parts of superfine filler, 0.5-10 parts of softener, 0.05-2 parts of wetting agent and 0.5-3 parts of essence.
2. The easy-mixing high-comfort silicone rubber oral impression material as claimed in claim 1, wherein the low volatility dimethylpolysiloxane containing two vinyl groups has a viscosity of 0.05-10 Pa-s, and comprises vinyl terminated polydimethylsiloxane, vinyl terminated polyvinylpolydimethylsiloxane, polyvinyl polyether, vinylmethylsiloxane ring.
3. The ready-mix, high comfort silicone rubber oral impression material of claim 1, wherein the dimethylpolysiloxane containing two or more Si-H groups comprises trimethylsilyl-terminated hydrogenous polyorganosiloxane.
4. The ready-mix high comfort silicone rubber oral impression material of claim 1, wherein the platinum catalyst is a winter-type catalyst comprising a vinyl silicone oil-diluted kastt platinum catalyst in an amount of 0.01 to 1.00% by weight as calculated as platinum atoms.
5. The ready-mix high comfort silicone rubber oral impression material of claim 1, wherein the platinum catalyst is a summer type catalyst comprising a vinyl silicone oil diluted kastt platinum catalyst in an amount of 0.01 to 0.80% by weight of platinum atoms.
6. The easy-mixing high-comfort silicone rubber oral impression material as claimed in claim 1, wherein the fumed silica has a specific surface area of 110 ± 20m2The grain diameter is 10-40 nm.
7. The miscible high-comfort silicone rubber oral impression material as defined in claim 1, wherein the ultrafine filler comprises one or more of kaolin, silica micropowder, calcium carbonate, talc and calcium phosphate, and has a particle size of 400-200 nm.
8. The easy-mixing high-comfort silicone rubber oral impression material as claimed in claim 1, wherein the softener comprises refined paraffin oil and polyvinyl polyether, and is a pure transparent liquid with a viscosity of 50-500 mPas.
9. The ready-mix high comfort silicone rubber oral impression material of claim 1, wherein the humectant comprises a polyether modified silicone oil having a silicon content of 10-20% and a surface tension of 15-30 mn/m;
the essence is spearmint essence, mint essence or fruit essence.
10. A method for preparing the easy-mixing high-comfort silicone rubber oral impression material according to any one of claims 1 to 9, comprising the steps of:
(1) weighing 15-45 parts by weight of one or more low-volatility dimethylpolysiloxanes containing at least two vinyl groups per molecule, 1-5 parts by weight of one or more dimethylpolysiloxanes containing at least two or more Si-H groups per molecule, 5-15 parts by weight of fumed silica, 45-75 parts by weight of superfine filler, 0.5-10 parts by weight of softener, 0.05-2 parts by weight of wetting agent and 0.5-3 parts by weight of essence, kneading in a kneader to obtain the component, and then carrying out vacuum degassing for later use;
(2) weighing 15-45 parts by weight of one or more low-volatility dimethylpolysiloxanes containing at least two vinyl groups per molecule, 0.2-5 parts by weight of platinum catalyst, 5-25 parts by weight of fumed silica, 45-70 parts by weight of superfine filler, 0.5-10 parts by weight of softener, 0.05-2 parts by weight of wetting agent and 0.5-3 parts by weight of essence, kneading in a kneader to obtain a catalyst component, and then carrying out vacuum degassing for later use;
(3) weighing the components of the agent and the catalyst in equal mass, and uniformly mixing to obtain the silicone rubber impression material.
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