CN1679466A - Liquid of light curing glass ion cement and preparation thereof - Google Patents
Liquid of light curing glass ion cement and preparation thereof Download PDFInfo
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- CN1679466A CN1679466A CN 200510016560 CN200510016560A CN1679466A CN 1679466 A CN1679466 A CN 1679466A CN 200510016560 CN200510016560 CN 200510016560 CN 200510016560 A CN200510016560 A CN 200510016560A CN 1679466 A CN1679466 A CN 1679466A
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Abstract
An optically solidified glass ion cementing solution is proportionally prepared from the copolymer of polyacrylic acid or acrylic acid and itaconic acid or the aqueous solution of acrylic acid-maleic acid copolymer, UDMA, 2-hydroxyethyl methylacrylate (HEMA), bis (2-hydroxy ethyl methylacrylate)-1,2,3,4-butane tetracarboxylate (TCB), optical trigger and cotrigger through sequentially mixing in water bath, stirring, and laying aside at 4-10 deg.C in darkness for 24 hr.
Description
Technical field
The present invention relates to liquor of a kind of light curing glass ion cement and preparation method thereof.
Background technology
The glass-ion cement spit of fland has a wide range of applications in tooth section and biomedical sector, can be used for filling the tooth cavity, makes bedding material, bonding hat and abnormal equipment etc. just.The glass-ion cement spit of fland roughly is divided into: traditional glass ionomer cement and light curing glass ion cement.
The traditional glass ionomer cement is a kind of cement of acid-base reaction, is generally solidified by the glass dust reaction of polycarboxylic acids and acid decomposable to obtain.It can be directly and the tooth bonding, constantly discharges fluorine, therefore has good biocompatibility.But do not have completely crued cement to be subjected to moisture contamination easily, mechanical strength is little, lacks toughness, and therefore brittle fracture takes place easily.
Light curing glass ion cement occurs for the defective that remedies the traditional glass ionomer cement.There are two kinds of curing reactions simultaneously in light curing glass ion cement: acid-base reaction and monomeric photopolymerization reaction.
Light curing glass ion cement except have a traditional glass ionomer cement with the direct bonding and constantly discharging the advantage of fluorine of tooth, also have mechanical strength than better aesthetic property of traditional glass ionomer cement and Geng Gao.
The liquor of light curing glass ion cement is generally by the copolymer in acrylic acid or acrylic acid and itaconic acid; Or the copolymer of acrylic acid and maleic acid; Or the side chain of photopolymerization in grafting on these polymer, photopolymerizable monomer, water, light initiation system are formed.
The glass-ion cement spit of fland that the Chinese Shanghai dental materal factory is produced is the traditional glass ionomer cement.Light curing glass ion cement on the international market mainly is the Fuji II LC of Japanese GC company.The main copolymer by acrylic acid and itaconic acid of liquor part of Fuji II LC, photo-curing monomer HEMA, water, light trigger etc. are formed, and its shortcoming is that compressive strength and flexural strength are not high enough.
Summary of the invention
The preparation method that the purpose of this invention is to provide a kind of liquor of light curing glass ion cement.
Raw material of the present invention is: the copolymer in acrylic acid, acrylic acid and the itaconic acid of (1) percetage by weight 15-25% or the aqueous copolymers solution of acrylic acid and maleic acid;
(2) the amino methyl acid esters double methyl methacrylate (UDMA) of percetage by weight 15-35%;
(3) the 2-ethoxy methyl-prop diluted acid ester (HEMA) of percetage by weight 20-40%;
(4) two (2-ethoxy methyl-prop diluted acid esters)-1,2,3 of percetage by weight 15-35%, 4-butane tetracarboxylic acid esters (TCB);
(5) the light trigger camphorquinone (CQ) of percetage by weight 0.10%-1.0%;
(6) the coinitiator N of percetage by weight 0.10-1.0%, N dimethylamine yl benzoic acid ethyl ester (DMABE).
Preparation process: stir, add initiator and coinitiator after percent mixes by weight with HEMA, TCB, UDMA, stirred in water bath at 45-50 ℃, it is fully dissolved, add the copolymer in acrylic acid or acrylic acid and itaconic acid or the aqueous solution of acrylic acid and maleic acid again, the copolymer of the copolymer in polyacrylic acid, acrylic acid and itaconic acid or acrylic acid and the maleic acid 15-25% that is weight percentage; Amino methyl acid esters double methyl methacrylate (UDMA) is 15-35%; 2-ethoxy methyl-prop diluted acid ester (HEMA) is 20-40%, two (2-ethoxy methyl-prop diluted acid ester)-1,2,3,4-butane tetracarboxylic acid esters (TCB) is that 15-35%, camphorquinone (CQ) are 0.10-1.0%, N, N dimethylamine yl benzoic acid ethyl ester (DMABE) is 0.10-1.0%, stirs it is fully dissolved, and then resulting mixed liquor is put into brown bottle, placing more than the 24h at the dark place under 4-10 ℃, get the liquor of light curing glass ion cement.
The liquor of the light curing glass ion cement of the present invention's preparation adopts standard method to estimate its compressive strength and flexural strength, and evaluating method is as follows:
(1) compressive strength
Get an amount of powder and be placed on the tuned plate, get an amount of liquor again, with toolsetting with powder liquid mixing 20s about, debugging is evenly.The material that mixes up packed into immediately to be had down in the mould of the compressive strength of microscope slide diameter 4mm, high 6mm.Another microscope slide is placed on die tip, and steps up gently, excess stock is overflowed with clip.
The center of light source window registration coupon position.Irradiation 40s, then, to sample another side irradiation 40s.Sample is put into 37 ℃ of waters bath with thermostatic control together with mould soak 15min, from mould, take out sample then and be placed in 37 ℃ of distilled water.Test after placing 23h 45min.
During test, sample is placed on the loading platform, carries out loading,, note maximum loading value until sample breakage with the speed of 1mm/min.5 samples of each sample making.
(2) flexural strength
Get an amount of powder and be placed on the tuned plate, get an amount of liquor again, with toolsetting with powder liquid mixing 20s about, debugging is evenly.The material that mixes up packed into immediately to be had down in the mould of the flexural strength of microscope slide 25mm * 2mm * 2mm.Another microscope slide is placed on die tip, and steps up gently, excess stock is overflowed with clip.
The center of light source window registration coupon position.Irradiation 40s, the center of another section of mobile light source window registration coupon, and partly and last time the illumination part was overlapping to some extent need to make each illumination.The irradiation 40s, until the sample various piece all illuminated the enough time.Then, aim at the sample another side and carry out same operation.Sample is put into 37 ℃ of waters bath with thermostatic control together with mould soak 15min, from mould, take out sample then and be placed in 37 ℃ of distilled water.Test after placing 23h45min.
During test, sample is placed on the loading platform, carries out loading,, note maximum loading value until sample breakage with the speed of 0.5mm/min.
The specific embodiment
Embodiment 1:
The proportioning of the liquor of light curing glass ion cement is:
Component weight percentage (%)
TCB????????????????????????????????????????20
UDMA???????????????????????????????????????20
HEMA???????????????????????????????????????39.5
Percetage by weight is 50% polyacrylic acid aqueous solution 19.5
CQ?????????????????????????????????????????0.5
DMEABE?????????????????????????????????????0.5
The preparation of sample and evaluation: in proportion HEMA, TCB, UDMA are mixed the back and stir, add initiator and coinitiator 50 ℃ stirred in water bath, make its dissolving, add the stirring of polyacrylic acid aqueous solution again and make its dissolving, then resulting mixed liquor is put into brown bottle, under 4 ℃, place 24h initiator and coinitiator are fully dissolved, get the liquor of light curing glass ion cement at the dark place.
With the powder of resulting liquor and Fuji II LC, be that 2.7g/1.0g mixes according to the powder/liquid proportional of standard, measure its compressive strength and flexural strength according to standard method then, the results are shown in Table 1.
Embodiment 2:
The proportioning of the liquor of light curing glass ion cement is:
Component weight percentage (%)
TCB???????????????????????????????????????????22.5
UDMA??????????????????????????????????????????22.5
HEMA??????????????????????????????????????????34.5
The acrylic acid of percetage by weight 47.5% and itaconic acid copolymer aqueous solution 20
CQ????????????????????????????????????????????0.25
DMABE?????????????????????????????????????????0.25
The preparation of sample and evaluation: earlier HEMA, TCB, UDMA are mixed the back and stir, add initiator and coinitiator 45 ℃ of stirred in water bath, make its dissolving, add the stirring of acrylic acid and itaconic acid copolymer aqueous solution again and make its dissolving, then resulting mixed liquor is put into brown bottle, under 6 ℃, place 48h initiator and coinitiator are fully dissolved, get the liquor of light curing glass ion cement at the dark place.
With the powder of resulting liquor and Fuji II LC, be that 2.7g/1.0g mixes according to the powder/liquid proportional of standard, measure its compressive strength and flexural strength according to standard method then, the results are shown in Table 1.
Embodiment 3:
The proportioning of the liquor of light curing glass ion cement is:
Component weight percentage (%)
TCB?????????????????????????????????????????????25
UDMA????????????????????????????????????????????24.7
HEMA????????????????????????????????????????????25
The acrylic acid of percetage by weight 47.5% and the aqueous copolymers solution of maleic acid 25
CQ??????????????????????????????????????????????0.15
DMABE???????????????????????????????????????????0.15
The preparation of sample and evaluation: earlier HEMA, TCB, UDMA are mixed the back and stir, add initiator and coinitiator 47 ℃ stirred in water bath, make its dissolving, the aqueous copolymers solution that adds acrylic acid and maleic acid again stirs and makes its dissolving, then resulting mixed liquor is put into brown bottle, under 8 ℃, place 36h initiator and coinitiator are fully dissolved, get the liquor of light curing glass ion cement at the dark place.
With the powder of resulting liquor and Fuji II LC, be that 2.7g/1.0g mixes according to the powder/liquid proportional of standard, measure its compressive strength and flexural strength according to standard method then, the results are shown in Table 1.
Embodiment 4:
The proportioning of the liquor of light curing glass ion cement is:
Component weight percentage (%)
TCB???????????????????????????????????????30
UDMA??????????????????????????????????????20
HEMA??????????????????????????????????????29.5
The polyacrylic acid aqueous solution 19 of percetage by weight 50%
CQ????????????????????????????????????????0.75
DMEABE????????????????????????????????????0.75
The preparation of sample and evaluation: earlier HEMA, TCB, UDMA are mixed the back and stir, add initiator and coinitiator 48 ℃ stirred in water bath, make its dissolving, add the stirring of polyacrylic acid aqueous solution again and make its dissolving, then resulting mixed liquor is put into brown bottle, under 8 ℃, place 24h initiator and coinitiator are fully dissolved, get the liquor of light curing glass ion cement at the dark place.
With the powder of resulting liquor and Fuji II LC, be that 2.7g/1.0g mixes according to the powder/liquid proportional of standard, measure its compressive strength and flexural strength according to standard method then, the results are shown in Table 1.
Comparative example:
Powder and the liquid of the Fuji II LC of GC company are mixed with 2.7g/1.0g, measure its compressive strength and flexural strength, the results are shown in Table 1 according to standard method.
Table 1, resulting compressive strength of embodiment and comparative example and flexural strength
| Compressive strength (Mpa) | Flexural strength (Mpa) | |
| Embodiment 1 | ????185.6 | ????64.33 |
| Embodiment 2 | ????196.5 | ????70.66 |
| Embodiment 3 | ????210.6 | ????78.82 |
| Embodiment 4 | ????200.4 | ????74.23 |
| Comparative example | ????186.6 | ????28.8 |
Claims (1)
1, a kind of preparation method of liquor of light curing glass ion cement, the raw material of employing is: the copolymer in acrylic acid, acrylic acid and the itaconic acid of (1) percetage by weight 15-25% or the aqueous copolymers solution of acrylic acid and maleic acid;
(2) the amino methyl acid esters double methyl methacrylate of percetage by weight 15-35%;
(3) the 2-ethoxy methyl-prop diluted acid ester of percetage by weight 20-40%;
(4) two (2-ethoxy methyl-prop diluted acid esters)-1,2,3 of percetage by weight 15-35%, 4-butane tetracarboxylic acid esters;
(5) the light trigger camphorquinone of percetage by weight 0.10%-1.0%;
(6) the coinitiator N of percetage by weight 0.10-1.0%, N dimethylamine yl benzoic acid ethyl ester.
Preparation process: with 2-ethoxy methyl-prop diluted acid ester, two (2-ethoxy methyl-prop diluted acid ester)-1,2,3,4-butane tetracarboxylic acid esters, amino methyl acid esters double methyl methacrylate, percent mixes the back stirring, adds initiator and coinitiator by weight, stirred in water bath at 45-50 ℃, it is fully dissolved, add the copolymer in acrylic acid or acrylic acid and itaconic acid or the aqueous solution of acrylic acid and maleic acid again, the copolymer of the copolymer in polyacrylic acid, acrylic acid and itaconic acid or acrylic acid and the maleic acid 15-25% that is weight percentage; Amino methyl acid esters double methyl methacrylate amino methyl acid esters double methyl methacrylate is 15-35%; 2-ethoxy methyl-prop diluted acid ester is 10-40%, two (2-ethoxy methyl-prop diluted acid ester)-1,2,3,4-butane tetracarboxylic acid esters is that 15-35%, camphorquinone are 0.10-1.0%, N, N dimethylamine yl benzoic acid ethyl ester is 0.10-1.0%, stirs, and then resulting mixed liquor is put into brown bottle, placing more than the 24h at the dark place under 4-10 ℃, get the liquor of light curing glass ion cement.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510016560 CN1679466A (en) | 2005-02-01 | 2005-02-01 | Liquid of light curing glass ion cement and preparation thereof |
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| CN 200510016560 CN1679466A (en) | 2005-02-01 | 2005-02-01 | Liquid of light curing glass ion cement and preparation thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102174141A (en) * | 2011-03-21 | 2011-09-07 | 北京化工大学 | Method for preparing glass ionomer cement liquid with low dissolubility and acidity |
| CN108107493A (en) * | 2017-12-15 | 2018-06-01 | 江苏黄金屋光学眼镜股份有限公司 | A kind of ophthalmic len oleophobic layer |
| CN108245433A (en) * | 2017-12-21 | 2018-07-06 | 中国科学院兰州化学物理研究所 | A kind of novel mouth section glass ionomer/fluorinated graphene composite material |
| CN108720954A (en) * | 2017-08-04 | 2018-11-02 | 山东大学 | The department of stomatology glass ionomer modulating device and modulator approach |
-
2005
- 2005-02-01 CN CN 200510016560 patent/CN1679466A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102174141A (en) * | 2011-03-21 | 2011-09-07 | 北京化工大学 | Method for preparing glass ionomer cement liquid with low dissolubility and acidity |
| CN102174141B (en) * | 2011-03-21 | 2013-01-02 | 北京化工大学 | Method for preparing glass ionomer cement liquid with low dissolubility and acidity |
| CN108720954A (en) * | 2017-08-04 | 2018-11-02 | 山东大学 | The department of stomatology glass ionomer modulating device and modulator approach |
| CN108107493A (en) * | 2017-12-15 | 2018-06-01 | 江苏黄金屋光学眼镜股份有限公司 | A kind of ophthalmic len oleophobic layer |
| CN108245433A (en) * | 2017-12-21 | 2018-07-06 | 中国科学院兰州化学物理研究所 | A kind of novel mouth section glass ionomer/fluorinated graphene composite material |
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