CN107722921A - A kind of silicone adhesive preparation method - Google Patents
A kind of silicone adhesive preparation method Download PDFInfo
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- CN107722921A CN107722921A CN201711216476.9A CN201711216476A CN107722921A CN 107722921 A CN107722921 A CN 107722921A CN 201711216476 A CN201711216476 A CN 201711216476A CN 107722921 A CN107722921 A CN 107722921A
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- CN
- China
- Prior art keywords
- silicone adhesive
- polyoxypropyleneglycol
- quality
- adhesive preparation
- silicon carbide
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Abstract
The invention discloses a kind of silicone adhesive preparation method, it is related to silicone adhesive technical field, is made up of following component：Dialkyl polydimethylsiloxane, gelatinized starch, crosslinking agent, filler, PTMG, epoxy propane butyl ether, nanometer silicon carbide, plasticizer, polyoxypropyleneglycol modified methyl acrylic, silicone adhesive various aspects of performance prepared by the coupling agent present invention is superior, in the present invention, the effect of polyoxypropyleneglycol modified methyl acrylic is plasticising, reduce the modulus of colloid, increase resist displacement ability, the viscosity of base rubber can be improved by polyoxypropyleneglycol modified methyl acrylic and epoxy propane butyl ether interaction, the resistance increase when producing stirring after causing nanometer silicon carbide to add, shearing force is improved, so that nanometer silicon carbide is scattered more uniform, the effective tensile strength and shear strength for improving silicone adhesive.
Description
Technical field
The invention belongs to silicone adhesive technical field, and in particular to a kind of silicone adhesive preparation method.
Background technology
In modern architecture material, ep-type material uses more and more extensive, the national also environmental-protection section bar of encouragement development always
Material realizes sustainable development.Silicone adhesive is widely used in door and window, curtain wall construction engineering and all kinds of building joint fillings as encapsulant
In.Silicone adhesive is silicone portion product, is a kind of similar ointment, once the moisture in ingress of air will be solidified into a kind of heavily fortified point
The material of tough rubber-like solid.De- acetic acid type is broadly divided into, dealcoholized type, deamination type, takes off the third type.Glass cement is that silicone adhesive is commonly called as
Title, because user buys bonding and the sealing in terms of silicone sealant is mainly used for glass, just it is called glass cement.So
And existing silicone adhesive performance is more general, especially tensile strength and shear strength is poor, can not meet the needs of market.
The content of the invention
The purpose of the present invention is to be directed to the problem of existing, there is provided a kind of silicone adhesive preparation method.
The present invention is achieved by the following technical solutions：
A kind of silicone adhesive preparation method, is made up of following component by weight：Dialkyl polydimethylsiloxane 75-80, paste
Change starch 5-8, crosslinking agent 1.2-1.5, filler 10-20, PTMG 2-5, epoxy propane butyl ether 1-4, nanometer
Carborundum 3-6, plasticizer 2-4, polyoxypropyleneglycol modified methyl acrylic 3-8, coupling agent 0.1-0.3.
Further, the gelatinized starch preparation method is：The water of 5 times of its quality is added into cornstarch, stirring is equal
After even, 120 DEG C are heated to, 15min is incubated, is subsequently cooled to 80 DEG C, the maleic acid of its quality 0.15% is added into cornstarch
Acid anhydride, after stirring, 2 hours are incubated, is then dried to constant weight, crushed, grinding, crossed 800 mesh sieves, produce.
Further, the crosslinking agent is dibutyl tin laurate.
Further, the filler is calcium carbonate, and the Carbonate Particle Size is 1250 mesh.
Further, the nanometer silicon carbide granularity is 80nm.
Further, the plasticizer is epoxidized soybean oil.
Further, the polyoxypropyleneglycol modified methyl acrylic preparation method is：
Under nitrogen protection, polyoxypropyleneglycol is added into reaction vessel, after being warming up to 70 DEG C, adds PPOX two
The methacrylate and the tetra-n-butyl titanate catalyst reaction of polyoxypropyleneglycol quality 0.5% that 10 times of alcohol quality
2.5 hours, after being subsequently added into the dihydromethyl propionic acid reaction 40min of polyoxypropyleneglycol quality quality 1.2%, reaction terminated
After be cooled to 20 DEG C, with 3000r/min rotating speeds stir 2 hours, produce.
The present invention has advantages below compared with prior art：Silicone adhesive various aspects of performance prepared by the present invention is superior, this hair
In bright, the effect of polyoxypropyleneglycol modified methyl acrylic is plasticising, reduces the modulus of colloid, increases resist displacement energy
Power, the viscous of base rubber can be improved by polyoxypropyleneglycol modified methyl acrylic and epoxy propane butyl ether interaction
Degree, the resistance increase when producing stirring after causing nanometer silicon carbide to add, shearing force is improved, so that nanometer silicon carbide
Scattered more uniformly effectively to improve the tensile strength and shear strength of silicone adhesive, hardness is significantly improved.PolyTHF
The addition of ether glycol and epoxy propane butyl ether can remove the hydroxyl of nano silicon carbide silicon face, nanometer silicon carbide as reinforcement and
The effect of thixotroping, the further intensity for improving silicone adhesive.What the silicone adhesive prepared by the present invention was prepared with existing production technology
Silicone adhesive is compared and had the advantage that：The outward appearance of product is easier to be controlled, and product appearance disqualification rate substantially reduces, product
Hardening time substantially accelerates, and can greatly reduce the engineering time, improves efficiency of construction.
Embodiment
Embodiment 1
A kind of silicone adhesive preparation method, is made up of following component by weight：Dialkyl polydimethylsiloxane 75, gelatinization are formed sediment
It is powder 5, crosslinking agent 1.2, filler 10, PTMG 2, epoxy propane butyl ether 1, nanometer silicon carbide 3, plasticizer 2, poly-
Propylene oxide glycol modification methacrylate 3, coupling agent 0.1.
Further, the gelatinized starch preparation method is：The water of 5 times of its quality is added into cornstarch, stirring is equal
After even, 120 DEG C are heated to, 15min is incubated, is subsequently cooled to 80 DEG C, the maleic acid of its quality 0.15% is added into cornstarch
Acid anhydride, after stirring, 2 hours are incubated, is then dried to constant weight, crushed, grinding, crossed 800 mesh sieves, produce.
Further, the crosslinking agent is dibutyl tin laurate.
Further, the filler is calcium carbonate, and the Carbonate Particle Size is 1250 mesh.
Further, the nanometer silicon carbide granularity is 80nm.
Further, the plasticizer is epoxidized soybean oil.
Further, the polyoxypropyleneglycol modified methyl acrylic preparation method is：
Under nitrogen protection, polyoxypropyleneglycol is added into reaction vessel, after being warming up to 70 DEG C, adds PPOX two
The methacrylate and the tetra-n-butyl titanate catalyst reaction of polyoxypropyleneglycol quality 0.5% that 10 times of alcohol quality
2.5 hours, after being subsequently added into the dihydromethyl propionic acid reaction 40min of polyoxypropyleneglycol quality quality 1.2%, reaction terminated
After be cooled to 20 DEG C, with 3000r/min rotating speeds stir 2 hours, produce.
Embodiment 2
A kind of silicone adhesive preparation method, is made up of following component by weight：Dialkyl polydimethylsiloxane 80, gelatinization are formed sediment
It is powder 8, crosslinking agent 1.5, filler 20, PTMG 5, epoxy propane butyl ether 4, nanometer silicon carbide 6, plasticizer 4, poly-
Propylene oxide glycol modification methacrylate 8, coupling agent 0.3.
Further, the gelatinized starch preparation method is：The water of 5 times of its quality is added into cornstarch, stirring is equal
After even, 120 DEG C are heated to, 15min is incubated, is subsequently cooled to 80 DEG C, the maleic acid of its quality 0.15% is added into cornstarch
Acid anhydride, after stirring, 2 hours are incubated, is then dried to constant weight, crushed, grinding, crossed 800 mesh sieves, produce.
Further, the crosslinking agent is dibutyl tin laurate.
Further, the filler is calcium carbonate, and the Carbonate Particle Size is 1250 mesh.
Further, the nanometer silicon carbide granularity is 80nm.
Further, the plasticizer is epoxidized soybean oil.
Further, the polyoxypropyleneglycol modified methyl acrylic preparation method is：
Under nitrogen protection, polyoxypropyleneglycol is added into reaction vessel, after being warming up to 70 DEG C, adds PPOX two
The methacrylate and the tetra-n-butyl titanate catalyst reaction of polyoxypropyleneglycol quality 0.5% that 10 times of alcohol quality
2.5 hours, after being subsequently added into the dihydromethyl propionic acid reaction 40min of polyoxypropyleneglycol quality quality 1.2%, reaction terminated
After be cooled to 20 DEG C, with 3000r/min rotating speeds stir 2 hours, produce.
Embodiment 3
A kind of silicone adhesive preparation method, is made up of following component by weight：Dialkyl polydimethylsiloxane 78, gelatinization are formed sediment
It is powder 6, crosslinking agent 1.3, filler 15, PTMG 3, epoxy propane butyl ether 2, nanometer silicon carbide 5, plasticizer 3, poly-
Propylene oxide glycol modification methacrylate 6, coupling agent 0.2.
Further, the gelatinized starch preparation method is：The water of 5 times of its quality is added into cornstarch, stirring is equal
After even, 120 DEG C are heated to, 15min is incubated, is subsequently cooled to 80 DEG C, the maleic acid of its quality 0.15% is added into cornstarch
Acid anhydride, after stirring, 2 hours are incubated, is then dried to constant weight, crushed, grinding, crossed 800 mesh sieves, produce.
Further, the crosslinking agent is dibutyl tin laurate.
Further, the filler is calcium carbonate, and the Carbonate Particle Size is 1250 mesh.
Further, the nanometer silicon carbide granularity is 80nm.
Further, the plasticizer is epoxidized soybean oil.
Further, the polyoxypropyleneglycol modified methyl acrylic preparation method is：
Under nitrogen protection, polyoxypropyleneglycol is added into reaction vessel, after being warming up to 70 DEG C, adds PPOX two
The methacrylate and the tetra-n-butyl titanate catalyst reaction of polyoxypropyleneglycol quality 0.5% that 10 times of alcohol quality
2.5 hours, after being subsequently added into the dihydromethyl propionic acid reaction 40min of polyoxypropyleneglycol quality quality 1.2%, reaction terminated
After be cooled to 20 DEG C, with 3000r/min rotating speeds stir 2 hours, produce.
Comparative example 1：Differed only in embodiment 1 and do not add polyoxypropyleneglycol modified methyl acrylic.
Comparative example 2：Differed only in embodiment 1 and polyoxypropyleneglycol modified methyl acrylic is replaced with into methyl
Acrylate.
Experiment：
Embodiment is respectively adopted and carries out performance comparison with silicone adhesive prepared by comparative example method；
Table 1
| Extrudability g/min | Hardness | Tensile strength MPa | Shear strength MPa | |
| Embodiment 1 | 188 | 22A | 2.02 | 1.78 |
| Embodiment 2 | 185 | 22A | 2.05 | 1.75 |
| Embodiment 3 | 186 | 22A | 2.04 | 1.77 |
| Comparative example 1 | 152 | 15 | 1.62 | 1.33 |
| Comparative example 2 | 163 | 17 | 1.70 | 1.41 |
As can be seen from Table 1, the silicone adhesive various aspects of performance that prepared by the inventive method is superior, disclosure satisfy that the demand in market.
Claims (7)
1. a kind of silicone adhesive preparation method, it is characterised in that be made up by weight of following component：Dihydroxy polydimethyl silicon
Oxygen alkane 75-80, gelatinized starch 5-8, crosslinking agent 1.2-1.5, filler 10-20, PTMG 2-5, expoxy propane fourth
Base ether 1-4, nanometer silicon carbide 3-6, plasticizer 2-4, polyoxypropyleneglycol modified methyl acrylic 3-8, coupling agent 0.1-
0.3。
2. a kind of silicone adhesive preparation method as claimed in claim 1, it is characterised in that the gelatinized starch preparation method is：
The water of 5 times of its quality is added into cornstarch, after stirring, 120 DEG C is heated to, is incubated 15min, is subsequently cooled to 80
DEG C, the maleic anhydride of its quality 0.15% is added into cornstarch, after stirring, 2 hours is incubated, is then dried to constant weight,
Crush, grinding, cross 800 mesh sieves, produce.
3. a kind of silicone adhesive preparation method as claimed in claim 1, it is characterised in that the crosslinking agent is the fourth of tin dilaurate two
Ji Xi.
4. a kind of silicone adhesive preparation method as claimed in claim 3, it is characterised in that the filler is calcium carbonate, the carbon
Sour calcium granularity is 1250 mesh.
5. a kind of silicone adhesive preparation method as claimed in claim 1, it is characterised in that the nanometer silicon carbide granularity is
80nm。
6. a kind of silicone adhesive preparation method as claimed in claim 1, it is characterised in that the plasticizer is epoxidized soybean oil.
7. a kind of silicone adhesive preparation method as claimed in claim 1, it is characterised in that the polyoxypropyleneglycol is modified first
Base acrylate preparation method is：
Under nitrogen protection, polyoxypropyleneglycol is added into reaction vessel, after being warming up to 70 DEG C, adds PPOX two
The methacrylate and the tetra-n-butyl titanate catalyst reaction of polyoxypropyleneglycol quality 0.5% that 10 times of alcohol quality
2.5 hours, after being subsequently added into the dihydromethyl propionic acid reaction 40min of polyoxypropyleneglycol quality quality 1.2%, reaction terminated
After be cooled to 20 DEG C, with 3000r/min rotating speeds stir 2 hours, produce.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711216476.9A CN107722921A (en) | 2017-11-28 | 2017-11-28 | A kind of silicone adhesive preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711216476.9A CN107722921A (en) | 2017-11-28 | 2017-11-28 | A kind of silicone adhesive preparation method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107722921A true CN107722921A (en) | 2018-02-23 |
Family
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|---|---|---|---|
| CN201711216476.9A Pending CN107722921A (en) | 2017-11-28 | 2017-11-28 | A kind of silicone adhesive preparation method |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102786909A (en) * | 2012-04-28 | 2012-11-21 | 何忠亮 | Organic silicon light-cured packaging glue used for LED packaging and application |
| CN103232829A (en) * | 2013-04-23 | 2013-08-07 | 广东信翼新材料股份有限公司 | Light-moisture dual-curing adhesive |
| CN103249795A (en) * | 2010-03-31 | 2013-08-14 | 卢敏纳粘合剂公司 | The switchable adhesives |
| CN105368379A (en) * | 2015-12-18 | 2016-03-02 | 广州市白云化工实业有限公司 | Silicone sealant with ultra-high strength and preparation method of silicone sealant |
| CN106085219A (en) * | 2016-06-30 | 2016-11-09 | 北京国电富通科技发展有限责任公司 | A kind of haze type antifouling flush paint and its preparation method and application |
-
2017
- 2017-11-28 CN CN201711216476.9A patent/CN107722921A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103249795A (en) * | 2010-03-31 | 2013-08-14 | 卢敏纳粘合剂公司 | The switchable adhesives |
| CN102786909A (en) * | 2012-04-28 | 2012-11-21 | 何忠亮 | Organic silicon light-cured packaging glue used for LED packaging and application |
| CN103232829A (en) * | 2013-04-23 | 2013-08-07 | 广东信翼新材料股份有限公司 | Light-moisture dual-curing adhesive |
| CN105368379A (en) * | 2015-12-18 | 2016-03-02 | 广州市白云化工实业有限公司 | Silicone sealant with ultra-high strength and preparation method of silicone sealant |
| CN106085219A (en) * | 2016-06-30 | 2016-11-09 | 北京国电富通科技发展有限责任公司 | A kind of haze type antifouling flush paint and its preparation method and application |
Non-Patent Citations (1)
| Title |
|---|
| 百度百科: "聚醚丙烯酸酯", 《百度百科》 * |
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Application publication date: 20180223 |
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