CN110128999A - A kind of fire-retardant bonded adhesives of one-component additional organosilicon and preparation method thereof - Google Patents
A kind of fire-retardant bonded adhesives of one-component additional organosilicon and preparation method thereof Download PDFInfo
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- CN110128999A CN110128999A CN201910406263.5A CN201910406263A CN110128999A CN 110128999 A CN110128999 A CN 110128999A CN 201910406263 A CN201910406263 A CN 201910406263A CN 110128999 A CN110128999 A CN 110128999A
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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
- 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
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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
- 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
- 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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- 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
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- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The present invention relates to flame-retardant adhesive glue, more particularly to a kind of fire-retardant bonded adhesives of one-component additional organosilicon and preparation method thereof, which includes: containing hydrogen silicone oil, vinyl silicone oil, siloxanes, reinforcing agent, fire retardant polysilazane, pH adjusting agent, inhibitor and platinum catalyst.Siloxanes is replaced with reinforcing agent and is repeatedly added in silicone oil, after being sufficiently mixed in planet machine, part fire retardant is added, pH adjusting agent is added, so that siloxanes is hydrolyzed and is crosslinked with reinforcing agent, fire retardant, it is surface modified, fire retardant is added in batches then, after sufficiently reacting with fire retardant, reinforcing agent, is washed to neutrality, moisture removal is removed under vacuum conditions, remaining silicone oil is added, obtains mixed prepolymer, is eventually adding containing hydrogen silicone oil, inhibitor, platinum catalyst and obtains finished product.Product of the present invention excellent flame retardancy, adhesion strength is high, high-efficiency environment friendly.
Description
Technical field
The present invention relates to flame-retardant adhesive glue, and in particular to a kind of fire-retardant bonded adhesives of one-component additional organosilicon and its preparation
Method.
Background technique
Addition-type silicon rubber is that one kind is non-toxic and tasteless, has excellent resistance to low temperature, weatherability, chemical-resistant resistance, electricity absolutely
The performances such as edge are widely used in the fields such as space flight and aviation, electronic apparatus, automobile, building, but its flame retardant property is not able to satisfy still
Application demand.As China's economy continues to develop, the requirement to organosilicon adhesive glue is continuously improved, especially to organosilicon adhesive glue
Flame retardant property.Currently, organosilicon adhesive glue it is fire-retardant mainly using outer doping improve, be broadly divided into reactive flame retardant and
Filled-type fire retardant.Reactive flame retardant can preferably be combined with silica gel, but flame retardant effect is general, higher cost, such as phosphorus system
It is compound etc. to close object, compound nitrogen series and the two, but it is easy to make catalyst poisoning, solidification is caused to be obstructed；Filled-type fire retardant at
This is low, and addition is convenient, but additive amount is big, is easy to cause organosilicon bonding adhesive force decline, as aluminium hydroxide, magnesium hydroxide,
Montmorillonite etc..
Summary of the invention
The purpose of the present invention is overcoming drawbacks described above, a kind of fire-retardant bonded adhesives of one-component additional organosilicon and its system are provided
Preparation Method.
To solve the above-mentioned problems, use polysilazane for fire retardant, polysilazane itself has good heating conduction
And heat resistance, heat can be conducted rapidly and heat is inhibited to assemble, to reach fire-retardant purpose, but polysilazane is easy to from bonding
It is precipitated in glue, influences adhesive glue performance.The present invention is by by vinyl silicone oil, vinylsiloxane, white carbon black and polysilazane
After being sufficiently mixed, vinylsiloxane is hydrolyzed under alkaline condition, to white carbon black and polysilazane in vinyl silicone oil system
Middle progress surface is modified, is well-dispersed in it in vinyl silicone oil, improves polysilazane and white carbon black in adhesive glue
Dispersibility.The adhesive property of adhesive glue can be improved in the silicone hydroxyl not being condensed after vinylsiloxane hydrolysis simultaneously, further improves
The cementitiousness of organosilicon adhesive glue.
Technical solution of the present invention: a kind of fire-retardant bonded adhesives of one-component additional organosilicon, by weight, component includes:
30-35 parts of containing hydrogen silicone oil, 1900-2200 parts of vinyl silicone oil, 2-4.5 parts of siloxanes, 280-310 parts of reinforcing agent, fire retardant is poly-
24-30 parts of silazane, 12-15 parts of pH adjusting agent, 1.5-2.0 parts of inhibitor, 10-15 parts of platinum catalyst.
As the polysilazane of fire retardant, heat resisting temperature is up to 750 DEG C or so, after hydroxyl silazane dehydrating condensation
Form polysilazane.
Further, the siloxanes is vinyltriethoxysilane or vinyltrimethoxysilane.
Further, the reinforcing agent is fume colloidal silica.
Further, the pH adjusting agent is alkaline matter, using ammonium hydroxide.
Further, the inhibitor is alkynol compound, using ethynylcyclohexanol, methyl butynol or 3,7,
11- trimethyl dodecyne -3- alcohol.
Further, the vinyl silicone oil viscosity is 9000-10000mPaS, contents of ethylene 0.34-0.38%；
Containing hydrogen silicone oil, viscosity 200-300mPaS, hydrogen content 0.7-0.8%.
Further, the platinum content 3000ppm of the platinum catalyst.
The present invention also provides a kind of preparation methods of mentioned-above fire-retardant bonded adhesives of one-component additional organosilicon, including
Following steps:
A, 1000-1200 parts of vinyl silicone oils and 1-2 parts of siloxanes stir 2-3min in planet machine；
B, 100-110 parts of fume colloidal silicas are added in planet machine, stir 60-70min；
C, 1-1.5 parts of siloxanes are added in planet machine, stir 2-3min；
D, 90-100 parts of fume colloidal silicas are added in planet machine, stir 90-100min；
E, 0.5-1 parts of siloxanes are added in planet machine, stir 2-3min
F, 100-110 parts of fume colloidal silicas are added in planet machine, stir 120-130min；
G, 8-10 parts of polysilazanes are added in planet machine, stir 20-30min；
H, after ensuring that polysilazane is sufficiently mixed, 12-15 parts of ammonium hydroxide are added, stir 20-30min；
I, 8-10 parts of polysilazanes are added, 20-30min is stirred；
J, 8-10 parts of polysilazanes are added after being heated to 85 DEG C, stir 20-30min；
K, for continuous heating to 105 DEG C, 0.1MPa is evacuated to 145 DEG C；
L, it washes four times, it is cooling after 145 DEG C of vacuum keep 90-100min；
M, 900-1000 parts of vinyl silicone oils are added；30-35 parts of containing hydrogen silicone oil are finally sequentially added, inhibitor 1.5-2.0
Part, it stirs evenly, 10-15 parts of platinum catalysts stir evenly, and can be obtained the fire-retardant bonded adhesives of one-component additional organosilicon.
The present invention compared with prior art the utility model has the advantages that
1, one pack system additional organosilicon flame-retardant adhesive glue of the invention, preparation process is simple, and adhesion strength is better than market
Conventional flame retardant adhesive glue, and flame retardant property can meet electronics industry flame retardant rating requirement, be a kind of excellent flame retardancy, bonding is strong
Degree is high, the one pack system additional organosilicon flame-retardant adhesive glue of high-efficiency environment friendly.
2, the present invention uses polysilazane to reach fire-retardant purpose for fire retardant, while solving polysilazane and being easy to from bonding
The problem of being precipitated in glue improves adhesive glue performance.
Specific embodiment
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, those skilled in the art
Member can various modifications may be made or change, such equivalent forms equally fall within the application the appended claims and limited to the present invention
Range.
In organic silicon flame-retardant adhesive glue preparation process of the present invention, siloxanes is replaced with reinforcing agent silicone oil is repeatedly added first
In, after being sufficiently mixed in planet machine, part fire retardant is first added, pH adjusting agent is then added, so that siloxanes hydrolysis is simultaneously
With reinforcing agent, fire retardant be crosslinked, be surface modified, then continue for remaining fire retardant to be added in batches, sufficiently with fire retardant,
It after reinforcing agent reaction, is washed with water to neutrality, and remove moisture removal under vacuum conditions, remaining silicone oil is added, obtain organosilicon resistance
Fire adhesive glue mixed prepolymer.It finally sequentially adds after containing hydrogen silicone oil, inhibitor, platinum catalyst are sufficiently mixed and obtains one pack system
Additional organosilicon flame-retardant adhesive glue.Specific implementation step is as follows:
A, 1000-1200 parts of vinyl silicone oils and 1-2 parts of vinyltrimethoxysilanes stir 2- in planet machine
3min；
B, 100-110 parts of fume colloidal silicas are added in planet machine, stir 60-70min；
C, 1-1.5 parts of vinyltrimethoxysilanes are added in planet machine, stir 2-3min；
D, 90-100 parts of fume colloidal silicas are added in planet machine, stir 90-100min；
E, 0.5-1 parts of vinyltrimethoxysilanes are added in planet machine, stir 2-3min
F, 100-110 parts of fume colloidal silicas are added in planet machine, stir 120-130min；
G, 8-10 parts of polysilazanes are added in planet machine, stir 20-30min；
H, after ensuring that polysilazane is sufficiently mixed, 12-15 parts of ammonium hydroxide are added, stir 20-30min；
I, 8-10 parts of polysilazanes are added, 20-30min is stirred；
J, 8-10 parts of polysilazanes are added after being heated to 85 DEG C, stir 20-30min；
K, for continuous heating to 105 DEG C, 0.1MPa is evacuated to 145 DEG C；
L, it washes four times, it is cooling after 145 DEG C of vacuum keep 90-100min；
M, 900-1000 parts of vinyl silicone oils are added；30-35 parts of containing hydrogen silicone oil are finally sequentially added, inhibitor 1.5-2.0
Part, it stirs evenly, 10-15 parts of platinum catalysts stir evenly, and can be obtained the fire-retardant bonded adhesives of one-component additional organosilicon.
According to above-mentioned preparation method, 8 groups of embodiments are set, and the one-component additional organosilicon obtained to each group is fire-retardant viscous
Connect the test that glue carries out viscosity, oxygen index (OI), fire-retardant rank, shear strength, hardness and tensile strength.
It is divided according to the fire-retardant rank of UL94HB, judges fire-retardant rank.Test setting and test result is as follows table.
As seen from the above table, the minimum 86543cps of viscosity, oxygen index (OI) minimum 28.5%, fire-retardant rank reaches
UL94V0, the minimum 2.3MPa of shear strength (aluminium), hardness minimum 31, the minimum 3.9MPa of tensile strength.Market routinely produces
Product fire-retardant rank is UL94V1, and oxygen index (OI) is 27% or so, hardness 31, tensile strength 3MPa, shear strength 1.6MPa, with market
Conventional products are compared, and the performance of product of the present invention is superior to market conventional flame retardant adhesive glue.
Claims (8)
1. a kind of fire-retardant bonded adhesives of one-component additional organosilicon, which is characterized in that by weight, component includes: containing hydrogen silicone oil
30-35 parts, 1900-2200 parts of vinyl silicone oil, 2-4.5 parts of siloxanes, 280-310 parts of reinforcing agent, fire retardant polysilazane 24-
30 parts, 12-15 parts of pH adjusting agent, 1.5-2.0 parts of inhibitor, 10-15 parts of platinum catalyst.
2. the fire-retardant bonded adhesives of one-component additional organosilicon according to claim 1, which is characterized in that the siloxanes is
Vinyltriethoxysilane or vinyltrimethoxysilane.
3. the fire-retardant bonded adhesives of one-component additional organosilicon according to claim 1, which is characterized in that the reinforcing agent is
Fume colloidal silica.
4. the fire-retardant bonded adhesives of one-component additional organosilicon according to claim 1, which is characterized in that the pH value is adjusted
Agent uses ammonium hydroxide.
5. the fire-retardant bonded adhesives of one-component additional organosilicon according to claim 1, which is characterized in that the inhibitor is adopted
With ethynylcyclohexanol, methyl butynol or 3,7,11- trimethyl dodecyne -3- alcohol.
6. the fire-retardant bonded adhesives of one-component additional organosilicon according to claim 1, which is characterized in that the vinyl silicon
Oil viscosity is 9000-10000mPaS, contents of ethylene 0.34-0.38%；Containing hydrogen silicone oil, viscosity 200-300mPaS,
Hydrogen content is 0.7-0.8%.
7. the fire-retardant bonded adhesives of one-component additional organosilicon according to claim 1, which is characterized in that the platinum catalysis
The platinum content 3000ppm of agent.
8. a kind of preparation method of the described in any item fire-retardant bonded adhesives of one-component additional organosilicon of claim 1-7, special
Sign is, comprising the following steps:
A, 1000-1200 parts of vinyl silicone oils and 1-2 parts of siloxanes stir 2-3min in planet machine；
B, 100-110 parts of fume colloidal silicas are added in planet machine, stir 60-70min；
C, 1-1.5 parts of siloxanes are added in planet machine, stir 2-3min；
D, 90-100 parts of fume colloidal silicas are added in planet machine, stir 90-100min；
E, 0.5-1 parts of siloxanes are added in planet machine, stir 2-3min
F, 100-110 parts of fume colloidal silicas are added in planet machine, stir 120-130min；
G, 8-10 parts of polysilazanes are added in planet machine, stir 20-30min；
H, after ensuring that polysilazane is sufficiently mixed, 12-15 parts of ammonium hydroxide are added, stir 20-30min；
I, 8-10 parts of polysilazanes are added, 20-30min is stirred；
J, 8-10 parts of polysilazanes are added after being heated to 85 DEG C, stir 20-30min；
K, for continuous heating to 105 DEG C, 0.1MPa is evacuated to 145 DEG C；
L, it washes four times, it is cooling after 145 DEG C of vacuum keep 90-100min；
M, 900-1000 parts of vinyl silicone oils are added；30-35 parts of containing hydrogen silicone oil are finally sequentially added, 1.5-2.0 parts of inhibitor, is stirred
It mixes uniformly, 10-15 parts of platinum catalysts stir evenly, and can be obtained the fire-retardant bonded adhesives of one-component additional organosilicon.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910406263.5A CN110128999A (en) | 2019-05-15 | 2019-05-15 | A kind of fire-retardant bonded adhesives of one-component additional organosilicon and preparation method thereof |
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| CN201910406263.5A CN110128999A (en) | 2019-05-15 | 2019-05-15 | A kind of fire-retardant bonded adhesives of one-component additional organosilicon and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113122180A (en) * | 2021-04-20 | 2021-07-16 | 浙江清优材料科技有限公司 | Fireproof ceramic organosilicon foaming sealant and preparation method thereof |
| CN113801626A (en) * | 2021-09-24 | 2021-12-17 | 广州集泰化工股份有限公司 | Single-component addition type adhesive and preparation method thereof |
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|---|---|---|---|---|
| CN1297962A (en) * | 1999-11-25 | 2001-06-06 | 中国科学院化学研究所 | Antioxidant polysiloxane composition |
| CN105153760A (en) * | 2015-08-26 | 2015-12-16 | 中国科学院化学研究所 | Filler modified by polysilazane at room temperature and preparation method and application of filler |
-
2019
- 2019-05-15 CN CN201910406263.5A patent/CN110128999A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1297962A (en) * | 1999-11-25 | 2001-06-06 | 中国科学院化学研究所 | Antioxidant polysiloxane composition |
| CN105153760A (en) * | 2015-08-26 | 2015-12-16 | 中国科学院化学研究所 | Filler modified by polysilazane at room temperature and preparation method and application of filler |
Non-Patent Citations (3)
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| P•科隆博: "《先驱体陶瓷 从纳米结构到应用》", 29 February 2016, 国防工业出版社 * |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113122180A (en) * | 2021-04-20 | 2021-07-16 | 浙江清优材料科技有限公司 | Fireproof ceramic organosilicon foaming sealant and preparation method thereof |
| CN113801626A (en) * | 2021-09-24 | 2021-12-17 | 广州集泰化工股份有限公司 | Single-component addition type adhesive and preparation method thereof |
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| CB03 | Change of inventor or designer information |
Inventor after: Hong Xingyuan Inventor after: Wu Changlin Inventor after: Pang Qingtao Inventor after: Li Jinbo Inventor before: Hong Xingyuan Inventor before: Li Wu Inventor before: Chang Lin Inventor before: Pang Qingtao Inventor before: Li Jinbo |
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