CN104905980B - A kind of adhesive for carious tooth Plugging and preparation method thereof - Google Patents

A kind of adhesive for carious tooth Plugging and preparation method thereof Download PDF

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CN104905980B
CN104905980B CN201510260789.9A CN201510260789A CN104905980B CN 104905980 B CN104905980 B CN 104905980B CN 201510260789 A CN201510260789 A CN 201510260789A CN 104905980 B CN104905980 B CN 104905980B
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parts
adhesive
temperature
dibutene
phosphoglycerol
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CN104905980A (en
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李苏杨
李文遐
徐勤霞
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Chen Fenfen
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Chen Fenfen
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Abstract

The invention discloses a kind of adhesive for carious tooth Plugging and preparation method thereof, the adhesive is made up of each component of following mass parts:34 52 parts of epoxy resin, 5 13 parts of sodium hexafluorisilicate, 6 19 parts of phosphoglycerol dimethylacrylate, 12 17 parts of hydroxyethyl cellulose, 15 22 parts of talcum powder, 32 43 parts of glycerine, 38 parts of methacrylic acid, 12 25 parts of dibutene, 6 17 parts of triethanolamine.Adhesives intensity produced by the present invention is high, compressive property is good and is not readily dissolved in saliva.

Description

A kind of adhesive for carious tooth Plugging and preparation method thereof
Technical field
The invention belongs to adhesive field, and in particular to a kind of adhesive and its preparation side for carious tooth Plugging Method.
Background technology
Dental caries are commonly called as decayed tooth, decayed tooth, are bacteriosises, can be with secondary pulpitis and periapical inflammation, or even can cause tooth Groove bone and inflammation of jaws, such as treat not in time, lesion continues to develop, and forms cavity, destroys disappearance completely to corona eventually, and it develops Final result be loss of tooth.Dental caries feature is incidence of disease height, and distribution is wide, is the main common disease in oral cavity, and the mankind are most Itself and tumour and angiocardiopathy are listed as the big keypoint control disease of the mankind three by one of universal disease, the World Health Organization Disease.
The harm of carious tooth have it is following some:(1) inflammation at the positions such as apex radicis dentis is often resulted in, local swelling when serious: As fester and bacterium are absorbed, septicemia or bacteremia can be caused;(2) bad root of the tooth is unable to laboratory rodent chow, aggravates intestines and stomach burden; (3) for the elderly, serious dental caries can badly cause largely or entirely absence of tooth, be unfavorable for the health of the elderly.
The adhesion strength and compression strength of existing carious tooth adhesive are poor, especially hold after Plugging after laboratory rodent chow It is easy to fall off, it is necessary to carry out Retreatment, add the difficulty for the treatment of;Existing carious tooth adhesive is after use easily in mouth simultaneously Dissolving, influences therapeutic effect.
The content of the invention
In order to overcome above the deficiencies in the prior art, the invention provides a kind of adhesive for carious tooth Plugging and Its preparation method, obtained adhesives intensity is high, compressive property is good and is not readily dissolved in saliva.
The technical solution adopted by the present invention is:A kind of adhesive for carious tooth Plugging, by each of following mass parts Component forms:Epoxy resin 34-52 parts, sodium hexafluorisilicate 5-13 parts, phosphoglycerol dimethylacrylate 6-19 parts, ethoxy Cellulose 12-17 parts, talcum powder 15-22 parts, glycerine 32-43 parts, methacrylic acid 3-8 parts, dibutene 12-25 parts, three second Hydramine 6-17 parts.
Preferably, a kind of adhesive for carious tooth Plugging, is made up of each component of following mass parts:Epoxy resin 38-50 parts, sodium hexafluorisilicate 7-11 parts, phosphoglycerol dimethylacrylate 7-15 parts, hydroxyethyl cellulose 13-15 parts, cunning Stone flour 19-21 parts, glycerine 36-40 parts, methacrylic acid 4-7 parts, dibutene 16-22 parts, triethanolamine 8-13 parts.
It is furthermore preferred that a kind of adhesive for carious tooth Plugging, is made up of each component of following mass parts:Asphalt mixtures modified by epoxy resin 45 parts of fat, 9 parts of sodium hexafluorisilicate, 13 parts of phosphoglycerol dimethylacrylate, 14 parts of hydroxyethyl cellulose, 20 parts of talcum powder, 37 parts of glycerine, 6 parts of methacrylic acid, 18 parts of dibutene, 11 parts of triethanolamine.
A kind of preparation method of adhesive for carious tooth Plugging, comprises the following steps:
(1) above-mentioned mass parts are pressed, epoxy resin, hydroxyethyl cellulose and talcum powder are added in glycerine, 80-90 DEG C of temperature Lower ultrasonic 5-10min, obtains compound one;
(2) sodium hexafluorisilicate, phosphoglycerol dimethylacrylate, methyl are added into compound one obtained by step (1) Acrylic acid, dibutene and triethanolamine, stirred at a temperature of 130-145 DEG C to being completely dissolved, speed 1000-1200r/ Min, obtain compound two;
(3) compound two obtained by step (2) is placed in vacuum drying oven and vacuumized except solvent processing, vacuum are 0.02-0.8MPa, temperature are 80-120 DEG C, time 100-130min, and curing cross-linking reaction is carried out after deflation and produces the use In the adhesive of dental caries therapeutic.
The temperature of curing cross-linking reaction is 90-150 DEG C in above-mentioned steps (3), reaction time 2-5h.
Beneficial effect:Adhesives intensity produced by the present invention for dental caries therapeutic is between 22.4-25.6N, 72h Compression strength is between 67.5-72.3MPa, and 24h does not produce dissolution phenomena in saliva, is reached by the synergy between component To the performance that adhesion strength is high, compressive property is good and is not readily dissolved in saliva.
Embodiment
Embodiment 1
A kind of adhesive for carious tooth Plugging, it is made up of each component of following mass parts:34 parts of epoxy resin, six 5 parts of prodan, 6 parts of phosphoglycerol dimethylacrylate, 12 parts of hydroxyethyl cellulose, 15 parts of talcum powder, 32 parts of glycerine, first 3 parts of base acrylic acid, 12 parts of dibutene, 6 parts of triethanolamine.
Preparation method:
(1) above-mentioned mass parts are pressed, epoxy resin, hydroxyethyl cellulose and talcum powder are added in glycerine, at a temperature of 80 DEG C Ultrasonic 5min, obtain compound one;
(2) sodium hexafluorisilicate, phosphoglycerol dimethylacrylate, methyl are added into compound one obtained by step (1) Acrylic acid, dibutene and triethanolamine, stir to being completely dissolved, speed 1000r/min, mixed at a temperature of 130 DEG C Close material two;
(3) compound two obtained by step (2) is placed in vacuum drying oven and vacuumized except solvent processing, vacuum are 0.02MPa, temperature are 80 DEG C, time 100min, and curing cross-linking reaction is carried out after deflation, are produced described for dental caries therapeutic The temperature of adhesive, wherein curing cross-linking reaction is 90 DEG C, reaction time 2h.
Embodiment 2
A kind of adhesive for carious tooth Plugging, it is made up of each component of following mass parts:52 parts of epoxy resin, six 13 parts of prodan, 19 parts of phosphoglycerol dimethylacrylate, 17 parts of hydroxyethyl cellulose, 22 parts of talcum powder, 43 parts of glycerine, 8 parts of methacrylic acid, 25 parts of dibutene, 17 parts of triethanolamine.
Preparation method:
(1) above-mentioned mass parts are pressed, epoxy resin, hydroxyethyl cellulose and talcum powder are added in glycerine, at a temperature of 90 DEG C Ultrasonic 10min, obtain compound one;
(2) sodium hexafluorisilicate, phosphoglycerol dimethylacrylate, methyl are added into compound one obtained by step (1) Acrylic acid, dibutene and triethanolamine, stir to being completely dissolved, speed 1200r/min, mixed at a temperature of 145 DEG C Close material two;
(3) compound two obtained by step (2) is placed in vacuum drying oven and vacuumized except solvent processing, vacuum are 0.8MPa, temperature are 120 DEG C, time 130min, and curing cross-linking reaction is carried out after deflation, are produced described for dental caries therapeutic The temperature of adhesive, wherein curing cross-linking reaction is 150 DEG C, reaction time 5h.
Embodiment 3
A kind of adhesive for carious tooth Plugging, it is made up of each component of following mass parts:38 parts of epoxy resin, six 7 parts of prodan, 7 parts of phosphoglycerol dimethylacrylate, 13 parts of hydroxyethyl cellulose, 19 parts of talcum powder, 36 parts of glycerine, first 4 parts of base acrylic acid, 16 parts of dibutene, 8 parts of triethanolamine.
Preparation method:
(1) above-mentioned mass parts are pressed, epoxy resin, hydroxyethyl cellulose and talcum powder are added in glycerine, at a temperature of 85 DEG C Ultrasonic 7min, obtain compound one;
(2) sodium hexafluorisilicate, phosphoglycerol dimethylacrylate, methyl are added into compound one obtained by step (1) Acrylic acid, dibutene and triethanolamine, stir to being completely dissolved, speed 1100r/min, mixed at a temperature of 135 DEG C Close material two;
(3) compound two obtained by step (2) is placed in vacuum drying oven and vacuumized except solvent processing, vacuum are 0.4MPa, temperature are 85 DEG C, time 110min, and curing cross-linking reaction is carried out after deflation, are produced described for dental caries therapeutic The temperature of adhesive, wherein curing cross-linking reaction is 120 DEG C, reaction time 3h.
Embodiment 4
A kind of adhesive for carious tooth Plugging, it is made up of each component of following mass parts:50 parts of epoxy resin, six 11 parts of prodan, 15 parts of phosphoglycerol dimethylacrylate, 15 parts of hydroxyethyl cellulose, 21 parts of talcum powder, 40 parts of glycerine, 7 parts of methacrylic acid, 22 parts of dibutene, 13 parts of triethanolamine.
Preparation method:
(1) above-mentioned mass parts are pressed, epoxy resin, hydroxyethyl cellulose and talcum powder are added in glycerine, at a temperature of 85 DEG C Ultrasonic 8min, obtain compound one;
(2) sodium hexafluorisilicate, phosphoglycerol dimethylacrylate, methyl are added into compound one obtained by step (1) Acrylic acid, dibutene and triethanolamine, stir to being completely dissolved, speed 1100r/min, mixed at a temperature of 140 DEG C Close material two;
(3) compound two obtained by step (2) is placed in vacuum drying oven and vacuumized except solvent processing, vacuum are 0.5MPa, temperature are 100 DEG C, time 120min, and curing cross-linking reaction is carried out after deflation, are produced described for dental caries therapeutic The temperature of adhesive, wherein curing cross-linking reaction is 110 DEG C, reaction time 3h.
Embodiment 5
A kind of adhesive for carious tooth Plugging, it is made up of each component of following mass parts:45 parts of epoxy resin, six 9 parts of prodan, 13 parts of phosphoglycerol dimethylacrylate, 14 parts of hydroxyethyl cellulose, 20 parts of talcum powder, 37 parts of glycerine, 6 parts of methacrylic acid, 18 parts of dibutene, 11 parts of triethanolamine.
Preparation method:
(1) above-mentioned mass parts are pressed, epoxy resin, hydroxyethyl cellulose and talcum powder are added in glycerine, at a temperature of 85 DEG C Ultrasonic 7min, obtain compound one;
(2) sodium hexafluorisilicate, phosphoglycerol dimethylacrylate, methyl are added into compound one obtained by step (1) Acrylic acid, dibutene and triethanolamine, stir to being completely dissolved, speed 1100r/min, mixed at a temperature of 140 DEG C Close material two;
(3) compound two obtained by step (2) is placed in vacuum drying oven and vacuumized except solvent processing, vacuum are 0.4MPa, temperature are 95 DEG C, time 110min, and curing cross-linking reaction is carried out after deflation, are produced described for dental caries therapeutic The temperature of adhesive, wherein curing cross-linking reaction is 130 DEG C, reaction time 3h.
Performance test:
Embodiment 1-5 and common carious tooth binder performance test result are as shown in the table:
As can be seen from the above table:Adhesives intensity produced by the present invention for dental caries therapeutic is in 22.4-25.6N Between, 72h compression strength is between 67.5-72.3MPa, and 24h does not produce dissolution phenomena in saliva, and common carious tooth adhesive Adhesion strength is 18.5N, and 72h compression strength is 38.0MPa, and 24h produces partial dissolving phenomena in saliva, it can thus be appreciated that this hair Bright obtained adhesive is by the way that the synergy between component reaches adhesion strength height, compressive property is good and is not easy in saliva The performance of dissolving.

Claims (4)

1. a kind of adhesive for carious tooth Plugging, it is characterised in that be made up of the component of following mass parts:Epoxy resin 34-52 parts, sodium hexafluorisilicate 5-13 parts, phosphoglycerol dimethylacrylate 6-19 parts, hydroxyethyl cellulose 12-17 parts, cunning Stone flour 15-22 parts, glycerine 32-43 parts, methacrylic acid 3-8 parts, dibutene 12-25 parts, triethanolamine 6-17 parts;Preparation side Method:(1)By above-mentioned mass parts, epoxy resin, hydroxyethyl cellulose and talcum powder are added in glycerine, surpassed at a temperature of 80-90 DEG C Sound 5-10min, obtain compound one;(2)To step(1)Sodium hexafluorisilicate, phosphoglycerol diformazan are added in gained compound one Base acrylate, methacrylic acid, dibutene and triethanolamine, stirred at a temperature of 130-145 DEG C to being completely dissolved, speed For 1000-1200r/min, compound two is obtained;(3)By step(2)Gained compound two, which is placed in vacuum drying oven, take out very Sky is handled except solvent, vacuum 0.02-0.8MPa, and temperature is 80-120 DEG C, time 100-130min, is consolidated after deflation Change cross-linking reaction and produce the adhesive for being used for dental caries therapeutic.
2. a kind of adhesive for carious tooth Plugging according to claim 1, it is characterised in that by following mass parts Component be made:Epoxy resin 38-50 parts, sodium hexafluorisilicate 7-11 parts, phosphoglycerol dimethylacrylate 7-15 parts, hydroxyl second Base cellulose 13-15 parts, talcum powder 19-21 parts, glycerine 36-40 parts, methacrylic acid 4-7 parts, dibutene 16-22 parts, three Monoethanolamine 8-13 parts.
3. a kind of adhesive for carious tooth Plugging according to claim 1, it is characterised in that by following mass parts Component be made:45 parts of epoxy resin, 9 parts of sodium hexafluorisilicate, 13 parts of phosphoglycerol dimethylacrylate, hydroxyethyl cellulose 14 parts, 20 parts of talcum powder, 37 parts of glycerine, 6 parts of methacrylic acid, 18 parts of dibutene, 11 parts of triethanolamine.
A kind of 4. adhesive for carious tooth Plugging according to claim 1, it is characterised in that the step(3) The temperature of middle curing cross-linking reaction is 90-150 DEG C, reaction time 2-5h.
CN201510260789.9A 2015-05-21 2015-05-21 A kind of adhesive for carious tooth Plugging and preparation method thereof Active CN104905980B (en)

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* Cited by examiner, † Cited by third party
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CN105640784A (en) * 2016-03-08 2016-06-08 苏州市贝克生物科技有限公司 Photo-curing adhesive for oral cavities and method for preparing photo-curing adhesive
CN111437201A (en) * 2020-03-18 2020-07-24 东华大学 Photocurable dentin binder for dental restoration and preparation method thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SU688193A1 (en) * 1977-11-25 1979-09-30 Харьковский Завод Медицинских Пластмасс И Стоматологических Материалов Tooth filling composition
CN1239415A (en) * 1996-11-29 1999-12-22 科尔公司 Single dose dental adhesive delivery system and method and adhesive therefor

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SU688193A1 (en) * 1977-11-25 1979-09-30 Харьковский Завод Медицинских Пластмасс И Стоматологических Материалов Tooth filling composition
CN1239415A (en) * 1996-11-29 1999-12-22 科尔公司 Single dose dental adhesive delivery system and method and adhesive therefor

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
互穿网络法增韧环氧树脂胶粘剂的研究;韦亚兵等;《中国胶粘剂》;20021231;第11卷(第1期);第6-8页 *

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