CN104873403A - Orthodontic adhesive and preparation method thereof - Google Patents
Orthodontic adhesive and preparation method thereof Download PDFInfo
- Publication number
- CN104873403A CN104873403A CN201510260788.4A CN201510260788A CN104873403A CN 104873403 A CN104873403 A CN 104873403A CN 201510260788 A CN201510260788 A CN 201510260788A CN 104873403 A CN104873403 A CN 104873403A
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- CN
- China
- Prior art keywords
- parts
- binding agent
- mouth cavity
- coupling agent
- cavity orthodontic
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000003479 dental cement Substances 0.000 title abstract description 8
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 55
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000007822 coupling agent Substances 0.000 claims abstract description 23
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims abstract description 19
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000001768 carboxy methyl cellulose Substances 0.000 claims abstract description 19
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims abstract description 19
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims abstract description 19
- 239000003822 epoxy resin Substances 0.000 claims abstract description 19
- 229910052588 hydroxylapatite Inorganic materials 0.000 claims abstract description 19
- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical compound [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 claims abstract description 19
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 19
- 229920000193 polymethacrylate Polymers 0.000 claims abstract description 19
- 239000011230 binding agent Substances 0.000 claims description 29
- 150000001875 compounds Chemical class 0.000 claims description 28
- 238000006243 chemical reaction Methods 0.000 claims description 14
- 238000004132 cross linking Methods 0.000 claims description 14
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 238000001291 vacuum drying Methods 0.000 claims description 7
- 238000013022 venting Methods 0.000 claims description 7
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 claims description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 3
- BDIZXIOWAPGQTJ-UHFFFAOYSA-N bis(2-ethylhexyl) phosphono phosphate Chemical compound CCCCC(CC)COP(=O)(OP(O)(O)=O)OCC(CC)CCCC BDIZXIOWAPGQTJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000003153 chemical reaction reagent Substances 0.000 claims description 3
- 230000008878 coupling Effects 0.000 claims description 3
- 238000010168 coupling process Methods 0.000 claims description 3
- 238000005859 coupling reaction Methods 0.000 claims description 3
- 229910000077 silane Inorganic materials 0.000 claims description 3
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 claims description 3
- 230000000172 allergic effect Effects 0.000 abstract description 5
- 208000010668 atopic eczema Diseases 0.000 abstract description 5
- 239000000853 adhesive Substances 0.000 abstract description 4
- 230000001070 adhesive effect Effects 0.000 abstract description 4
- 208000024891 symptom Diseases 0.000 abstract description 4
- 238000001723 curing Methods 0.000 description 12
- 238000000016 photochemical curing Methods 0.000 description 4
- 238000012937 correction Methods 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 210000003205 muscle Anatomy 0.000 description 2
- 210000005036 nerve Anatomy 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 230000002159 abnormal effect Effects 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 230000001815 facial effect Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 210000001548 stomatognathic system Anatomy 0.000 description 1
- 238000002560 therapeutic procedure Methods 0.000 description 1
Abstract
The invention discloses an orthodontic adhesive and a preparation method thereof. The adhesive is prepared from the following components in parts by weight: 19-37 parts of epoxy resin, 5-16 parts of polymethacrylate, 3-8 parts of n-butyl acrylate, 12-19 parts of carboxymethylcellulose, 5-15 parts of dibutyl phthalate, 32-43 parts of glycerinum, 3-10 parts of a coupling agent, 12-25 parts of dibutene and 6-21 parts of hydroxyapatite. The prepared adhesive is high in bonding strength and high in stretchability, does not generate an allergic symptom and can be widely applied to clinical treatment.
Description
Technical field
The invention belongs to adhesive field, be specifically related to a kind of mouth cavity orthodontic binding agent and preparation method thereof.
Background technology
Correction is exactly straightening of teeth, removes patho-occlusion.Correction mainly studies the Etiologic Mechanism of patho-occlusion, diagnostic analysis and prevention and therapy thereof.Orthodontic treatment adjusts the harmony between the nerve of facial skeleton, tooth and Maxillary region and muscle mainly through various apparatus for correcting, namely between the upper mandibular bone of adjustment, between upper lower teeth, between tooth and jawbone and contact abnormal relation between their nerve and muscle, it finally rescues target is the balance, stable and attractive in appearance reaching stomatognathic system.
Existing orthodontic adhesive mainly contains: use phosphoric acid acid etching to rinse class binding agent, and product can be selected to have non-tune to mix type, photocuring orthodontic adhesive, two paste chemistry fixed line orthodontic adhesive, resin tooth type glass ion etc.
Existing orthodontic adhesive adhesion strength is less, and hot strength is more weak, especially arch wire is fixed on bracket when imposing pulling force, bracket easily comes off, need to carry out secondary bonding, chew simultaneously really up to the mark or cross sticky food time bracket also easily come off, part correction patient have also appeared allergic symptom in addition.
Summary of the invention
In order to overcome above the deficiencies in the prior art, the invention provides a kind of mouth cavity orthodontic binding agent and preparation method thereof, obtained adhesives intensity is high, stretch capability strong and there will not be irritated symptom, can be widely used in clinical treatment.
The technical solution used in the present invention is: a kind of mouth cavity orthodontic binding agent, is made up of each component of following mass parts: epoxy resin 19-37 part, polymethacrylates 5-16 part, n-butyl acrylate 3-8 part, carboxymethyl cellulose 12-19 part, dibutyl phthalate 5-15 part, glycerol 32-43 part, coupling agent 3-10 part, dibutene 12-25 part, hydroxyapatite 6-21 part.
Preferably, a kind of mouth cavity orthodontic binding agent, is made up of each component of following mass parts: epoxy resin 22-32 part, polymethacrylates 9-14 part, n-butyl acrylate 5-7 part, carboxymethyl cellulose 14-18 part, dibutyl phthalate 6-11 part, glycerol 37-41 part, coupling agent 4-8 part, dibutene 14-21 part, hydroxyapatite 11-18 part.
Preferred, a kind of mouth cavity orthodontic binding agent, is made up of each component of following mass parts: epoxy resin 27 parts, polymethacrylates 12 parts, n-butyl acrylate 6 parts, carboxymethyl cellulose 16 parts, dibutyl phthalate 8 parts, glycerol 38 parts, coupling agent 6 parts, dibutene 19 parts, hydroxyapatite 14 parts.
Above-mentioned coupling agent is the one in Silane coupling reagent KH-570, silane coupler KH-560, titanate coupling agent NDZ-401 or titanate coupling agent NDZ-311.
A preparation method for mouth cavity orthodontic binding agent, comprises the following steps:
(1) by above-mentioned mass parts, epoxy resin, polymethacrylates, carboxymethyl cellulose, coupling agent, dibutene and hydroxyapatite are added in glycerol, be stirred at 110-130 DEG C of temperature and dissolve completely, stir speed (S.S.) is 800-1100r/min, obtains compound one;
(2) in step (1) gained compound one, add n-butyl acrylate and dibutyl phthalate, ultrasonic 10-15min at 75-90 DEG C of temperature, obtains compound two;
(3) step (2) gained compound two is placed in vacuum drying oven to carry out evacuation and desolventize process, vacuum is 0.1-0.8MPa, temperature is 80-110 DEG C, and the time is 90-120min, carries out curing cross-linking reaction and namely obtain described mouth cavity orthodontic binding agent after venting.
In above-mentioned steps (3), the temperature of curing cross-linking reaction is 90-130 DEG C, and the response time is 3-6h.
Beneficial effect: the present invention obtain for mouth cavity orthodontic binding agent by the synergism between component, after making photocuring 60s, adhesion strength is between 45.6-50.4N, between 49.5-53.5MPa, there is not allergic phenomena after using in hot strength, can be widely used in clinical treatment.
Detailed description of the invention
Embodiment 1
A kind of mouth cavity orthodontic binding agent, is made up of each component of following mass parts: epoxy resin 19 parts, polymethacrylates 5 parts, n-butyl acrylate 3 parts, carboxymethyl cellulose 12 parts, dibutyl phthalate 5 parts, glycerol 32 parts, Silane coupling reagent KH-570 3 parts, dibutene 12 parts, hydroxyapatite 6 parts.
Preparation method:
(1) by above-mentioned mass parts, epoxy resin, polymethacrylates, carboxymethyl cellulose, coupling agent, dibutene and hydroxyapatite are added in glycerol, be stirred at 110 DEG C of temperature and dissolve completely, stir speed (S.S.) is 800r/min, obtains compound one;
(2) in step (1) gained compound one, add n-butyl acrylate and dibutyl phthalate, ultrasonic 10min at 75 DEG C of temperature, obtains compound two;
(3) step (2) gained compound two is placed in vacuum drying oven to carry out evacuation and desolventize process, vacuum is 0.1MPa, temperature is 80 DEG C, time is 90min, carry out curing cross-linking reaction after venting and namely obtain described mouth cavity orthodontic binding agent, wherein the temperature of curing cross-linking reaction is 90 DEG C, and the response time is 3h.
Embodiment 2
A kind of mouth cavity orthodontic binding agent, is made up of each component of following mass parts: epoxy resin 37 parts, polymethacrylates 16 parts, n-butyl acrylate 8 parts, carboxymethyl cellulose 19 parts, dibutyl phthalate 15 parts, glycerol 43 parts, silane coupler KH-560 10 parts, dibutene 25 parts, hydroxyapatite 21 parts.
Preparation method:
(1) by above-mentioned mass parts, epoxy resin, polymethacrylates, carboxymethyl cellulose, coupling agent, dibutene and hydroxyapatite are added in glycerol, be stirred at 130 DEG C of temperature and dissolve completely, stir speed (S.S.) is 1100r/min, obtains compound one;
(2) in step (1) gained compound one, add n-butyl acrylate and dibutyl phthalate, ultrasonic 15min at 90 DEG C of temperature, obtains compound two;
(3) step (2) gained compound two is placed in vacuum drying oven to carry out evacuation and desolventize process, vacuum is 0.8MPa, temperature is 110 DEG C, time is 120min, carry out curing cross-linking reaction after venting and namely obtain described mouth cavity orthodontic binding agent, wherein the temperature of curing cross-linking reaction is 130 DEG C, and the response time is 6h.
Embodiment 3
A kind of mouth cavity orthodontic binding agent, is made up of each component of following mass parts: epoxy resin 22 parts, polymethacrylates 9 parts, n-butyl acrylate 5 parts, carboxymethyl cellulose 14 parts, dibutyl phthalate 6 parts, glycerol 37 parts, titanate coupling agent NDZ-401 4 parts, dibutene 14 parts, hydroxyapatite 11 parts.
Preparation method:
(1) by above-mentioned mass parts, epoxy resin, polymethacrylates, carboxymethyl cellulose, coupling agent, dibutene and hydroxyapatite are added in glycerol, be stirred at 120 DEG C of temperature and dissolve completely, stir speed (S.S.) is 900r/min, obtains compound one;
(2) in step (1) gained compound one, add n-butyl acrylate and dibutyl phthalate, ultrasonic 12min at 80 DEG C of temperature, obtains compound two;
(3) step (2) gained compound two is placed in vacuum drying oven to carry out evacuation and desolventize process, vacuum is 0.3MPa, temperature is 90 DEG C, time is 110min, carry out curing cross-linking reaction after venting and namely obtain described mouth cavity orthodontic binding agent, wherein the temperature of curing cross-linking reaction is 120 DEG C, and the response time is 4h.
Embodiment 4
A kind of mouth cavity orthodontic binding agent, is made up of each component of following mass parts: epoxy resin 32 parts, polymethacrylates 14 parts, n-butyl acrylate 7 parts, carboxymethyl cellulose 18 parts, dibutyl phthalate 11 parts, glycerol 41 parts, titanate coupling agent NDZ-401 8 parts, dibutene 21 parts, hydroxyapatite 18 parts.
Preparation method:
(1) by above-mentioned mass parts, epoxy resin, polymethacrylates, carboxymethyl cellulose, coupling agent, dibutene and hydroxyapatite are added in glycerol, be stirred at 120 DEG C of temperature and dissolve completely, stir speed (S.S.) is 1000r/min, obtains compound one;
(2) in step (1) gained compound one, add n-butyl acrylate and dibutyl phthalate, ultrasonic 14min at 85 DEG C of temperature, obtains compound two;
(3) step (2) gained compound two is placed in vacuum drying oven to carry out evacuation and desolventize process, vacuum is 0.7MPa, temperature is 95 DEG C, time is 110min, carry out curing cross-linking reaction after venting and namely obtain described mouth cavity orthodontic binding agent, wherein the temperature of curing cross-linking reaction is 120 DEG C, and the response time is 5h.
Embodiment 5
A kind of mouth cavity orthodontic binding agent, is made up of each component of following mass parts: epoxy resin 27 parts, polymethacrylates 12 parts, n-butyl acrylate 6 parts, carboxymethyl cellulose 16 parts, dibutyl phthalate 8 parts, glycerol 38 parts, titanate coupling agent NDZ-311 6 parts, dibutene 19 parts, hydroxyapatite 14 parts.
Preparation method:
(1) by above-mentioned mass parts, epoxy resin, polymethacrylates, carboxymethyl cellulose, coupling agent, dibutene and hydroxyapatite are added in glycerol, be stirred at 120 DEG C of temperature and dissolve completely, stir speed (S.S.) is 1000r/min, obtains compound one;
(2) in step (1) gained compound one, add n-butyl acrylate and dibutyl phthalate, ultrasonic 14min at 85 DEG C of temperature, obtains compound two;
(3) step (2) gained compound two is placed in vacuum drying oven to carry out evacuation and desolventize process, vacuum is 0.7MPa, temperature is 95 DEG C, time is 110min, carry out curing cross-linking reaction after venting and namely obtain described mouth cavity orthodontic binding agent, wherein the temperature of curing cross-linking reaction is 120 DEG C, and the response time is 5h.
Performance test:
Embodiment 1-5 and as shown in the table to common orthodontic adhesive the performance test results:
As can be seen from the above table: the present invention obtain for adhesion strength after mouth cavity orthodontic binding agent photocuring 60s between 45.6-50.4N, hot strength is between 49.5-53.5MPa, allergic phenomena is there is not after using, and adhesion strength is 24.8N after common orthodontic adhesive photocuring 60s, hot strength is 38.1MPa, and there is allergic phenomena, it can thus be appreciated that the binding agent that the present invention obtains enhances adhesion strength and hot strength by the synergism between component, there will not be irritated symptom simultaneously, can clinical treatment be widely used in.
Claims (6)
1. a mouth cavity orthodontic binding agent, it is characterized in that, be made up of the component of following mass parts: epoxy resin 19-37 part, polymethacrylates 5-16 part, n-butyl acrylate 3-8 part, carboxymethyl cellulose 12-19 part, dibutyl phthalate 5-15 part, glycerol 32-43 part, coupling agent 3-10 part, dibutene 12-25 part, hydroxyapatite 6-21 part.
2. a kind of mouth cavity orthodontic binding agent according to claim 1, it is characterized in that, be made up of the component of following mass parts: epoxy resin 22-32 part, polymethacrylates 9-14 part, n-butyl acrylate 5-7 part, carboxymethyl cellulose 14-18 part, dibutyl phthalate 6-11 part, glycerol 37-41 part, coupling agent 4-8 part, dibutene 14-21 part, hydroxyapatite 11-18 part.
3. a kind of mouth cavity orthodontic binding agent according to claim 1, it is characterized in that, be made up of the component of following mass parts: epoxy resin 27 parts, polymethacrylates 12 parts, n-butyl acrylate 6 parts, carboxymethyl cellulose 16 parts, dibutyl phthalate 8 parts, glycerol 38 parts, coupling agent 6 parts, dibutene 19 parts, hydroxyapatite 14 parts.
4. a kind of mouth cavity orthodontic binding agent according to claim 1, is characterized in that, described coupling agent is the one in Silane coupling reagent KH-570, silane coupler KH-560, titanate coupling agent NDZ-401 or titanate coupling agent NDZ-311.
5. the preparation method of a kind of mouth cavity orthodontic binding agent of Claims 1-4 described in any one, is characterized in that: comprise the following steps:
(1) by above-mentioned mass parts, epoxy resin, polymethacrylates, carboxymethyl cellulose, coupling agent, dibutene and hydroxyapatite are added in glycerol, be stirred at 110-130 DEG C of temperature and dissolve completely, stir speed (S.S.) is 800-1100r/min, obtains compound one;
(2) in step (1) gained compound one, add n-butyl acrylate and dibutyl phthalate, ultrasonic 10-15min at 75-90 DEG C of temperature, obtains compound two;
(3) step (2) gained compound two is placed in vacuum drying oven to carry out evacuation and desolventize process, vacuum is 0.1-0.8MPa, temperature is 80-110 DEG C, and the time is 90-120min, carries out curing cross-linking reaction and namely obtain described mouth cavity orthodontic binding agent after venting.
6. the preparation method of a kind of mouth cavity orthodontic binding agent according to claim 5, is characterized in that: in described step (3), the temperature of curing cross-linking reaction is 90-130 DEG C, and the response time is 3-6h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510260788.4A CN104873403B (en) | 2015-05-21 | 2015-05-21 | A kind of mouth cavity orthodontic adhesive and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510260788.4A CN104873403B (en) | 2015-05-21 | 2015-05-21 | A kind of mouth cavity orthodontic adhesive and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104873403A true CN104873403A (en) | 2015-09-02 |
| CN104873403B CN104873403B (en) | 2018-04-27 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510260788.4A Active CN104873403B (en) | 2015-05-21 | 2015-05-21 | A kind of mouth cavity orthodontic adhesive and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN108403443A (en) * | 2018-02-27 | 2018-08-17 | 苏州凌科特新材料有限公司 | A kind of dental cement and preparation method thereof |
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| WO2009029734A2 (en) * | 2007-08-28 | 2009-03-05 | Pioneer Surgical Technology, Inc. | Cement products and methods of making and using the same |
| CN104434542A (en) * | 2014-11-27 | 2015-03-25 | 苏州市贝克生物科技有限公司 | Medical antibacterial adhesive and preparation method thereof |
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2015
- 2015-05-21 CN CN201510260788.4A patent/CN104873403B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009029734A2 (en) * | 2007-08-28 | 2009-03-05 | Pioneer Surgical Technology, Inc. | Cement products and methods of making and using the same |
| CN104434542A (en) * | 2014-11-27 | 2015-03-25 | 苏州市贝克生物科技有限公司 | Medical antibacterial adhesive and preparation method thereof |
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| 张玲等: "环氧树脂胶粘剂的丙烯酸丁酯增韧研究", 《高校化学工程学报》 * |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN108403443A (en) * | 2018-02-27 | 2018-08-17 | 苏州凌科特新材料有限公司 | A kind of dental cement and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104873403B (en) | 2018-04-27 |
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Effective date of registration: 20240229 Address after: 537000, No. 593 Education Middle Road, Yulin City, Guangxi Zhuang Autonomous Region Patentee after: Guangxi Lantian Dental Hospital Group Co.,Ltd. Country or region after: China Address before: 318000 Donghui village, Haimen street, Jiaojiang District, Taizhou, Zhejiang 88 Patentee before: Wang Mengmeng Country or region before: China |
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