CN109266279A - A kind of preparation method of flame-proof weather-resisting type casting glue - Google Patents
A kind of preparation method of flame-proof weather-resisting type casting glue Download PDFInfo
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- CN109266279A CN109266279A CN201811046806.9A CN201811046806A CN109266279A CN 109266279 A CN109266279 A CN 109266279A CN 201811046806 A CN201811046806 A CN 201811046806A CN 109266279 A CN109266279 A CN 109266279A
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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
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
- C09J163/10—Epoxy resins modified by unsaturated compounds
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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
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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
- C09J11/08—Macromolecular additives
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- 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
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/2224—Magnesium hydroxide
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- 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
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2265—Oxides; Hydroxides of metals of iron
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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
- C08L2205/03—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
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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
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
- C08L2205/16—Fibres; Fibrils
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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
- C08L2312/00—Crosslinking
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- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses a kind of preparation methods of flame-proof weather-resisting type casting glue, belong to technical field of adhesive preparation.The present invention is using methylvinyldichlorosilane and dimethylphosphite as raw material, addition reaction occurs under the catalysis of aluminium chloride, with distilled water substitution reaction occurs for the product of generation again, synthesize silyl phosphate, using ginkgo leaf as raw material, dipping by lye, lignin portion in ginkgo leaf decomposes, the decomposed of lignin is separated from each other the cellulose in ginkgo leaf raw material, contain a large amount of iron in ginkgo leaf, the elements such as magnesium, it is reacted with sodium hydroxide and generates iron hydroxide, magnesium hydroxide, the good flame resistance of iron hydroxide and magnesium hydroxide, ginkgo leaf fibre, Black Warrior mineral wool, the water resistance of flax fiber, ageing-resistant performance is excellent, improve the weatherability of casting glue, exclude the air between fiber and glue-line, silyl phosphate is cross-linked to form macromolecular compound, casting glue anti-flammability is promoted, so that flame-proof weather-resisting type casting glue of the present invention has Wide application prospect.
Description
Technical field
The invention discloses a kind of preparation methods of flame-proof weather-resisting type casting glue, belong to technical field of adhesive preparation.
Background technique
Casting glue is also known as electronic pastes, is an extensive address.For the bonding of electronic component, sealing, encapsulating and painting
Cover protection.Casting glue belongs to liquid before uncured, has mobility, glue viscosity is according to the material, performance, production of product
The difference of technique and different from.Casting glue is just able to achieve its use value after being fully cured, waterproof can be played after solidification
Moisture-proof, dust-proof, insulation, thermally conductive, secrecy, anticorrosion, heatproof, shockproof effect.Electron pouring sealant type is very more, from material class
Type divides, at present using at most most common predominantly 3 kinds, i.e. epoxy resin embedding adhesive, organic siliconresin casting glue, polyurethane
Casting glue, and these three material casting glues can segment several hundred kinds of different products.
Encapsulating is exactly that liquid polyurethane compound is poured into the device equipped with electronic component, route with mechanical or manual mode
It is interior, the thermosetting polymer insulating materials haveing excellent performance is solidified under room temperature or heating condition.Its effect is: strengthening electricity
The globality of sub- device improves the resistance to external shock, vibration；It improves and insulate between internal element, route, be conducive to device
Miniaturization, lightweight；It avoids element, route from directly exposing, improves waterproof, the humidity resistance of device.Epoxy pouring sealant application model
It encloses extensively, technical requirements are multifarious, various in style.Being divided to from condition of cure has normal temperature cure and two classes that are heating and curing.From dosage form
Above being divided to has two class of bi-component and one pack system.Multicomponent dosage form, it is rare as commodity due to inconvenient to use.Normal temperature cure ring
Oxygen casting glue is generally bi-component, be not required to after encapsulating heating it is i.e. curable, it is not high to equipment requirement, it is easy to use.It is general multi-purpose
It is used in the encapsulating of Low-voltage Electronic device or the occasion that should not be heating and curing.Be heating and curing bi-component epoxy casting glue, be dosage most
Greatly, the most wide kind of purposes.Single-component epoxy potting compound is used suitable for high voltage electronics automatic assembly line, is recent years abroad hair
The new varieties of exhibition need to be heating and curing.
Casting glue is using extremely wide in transformer encapsulating field, and organic silicon potting adhesive is as a kind of common encapsulating
Glue type, wherein using then more extensive, thus use scope is extremely wide in existing transformer.And the quality of casting glue
It will directly affect the performance quality of transformer, and the environment that transformer is commonly used is usually from the environment such as high temperature, thus easily
So that the shortcomings that conventional casting glue is damaged, and there is also poor fires.
Therefore, the flame-proof weather-resisting type casting glue of a kind of good flame resistance and good weatherability is invented to technical field of adhesive preparation
With positive effect.
Summary of the invention
Present invention mainly solves the technical issues of, for casting glue at present on the market flame retardant property is bad, weatherability
The defect of difference, provides a kind of preparation method of flame-proof weather-resisting type casting glue.
In order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is that:
A kind of preparation method of flame-proof weather-resisting type casting glue, it is characterised in that specific preparation step are as follows:
(1) methylvinyldichlorosilane, dimethylphosphite, aluminium chloride are added in reaction kettle, load onto blender, temperature
Meter, nitrogen conduit and condenser and chlorine absorption unit, and nitrogen is passed through until displacing all air, in nitrogen into reaction kettle
Under gas shielded, 60~70 DEG C are heated to, 3~4h is stirred to react, obtains mixture；
(2) flow back 4~5h after said mixture being warming up to 90~100 DEG C, obtains mixed liquor, then mixed liquor is down to room temperature,
Distilled water is added dropwise, until not having gas releasing, reaction was completed, obtains mix products, stands after mix products are stirred, in collection
Layer weak yellow liquid, it is spare；
(3) it weighs ginkgo leaf to be put into tissue pulverizer, 40~50min of crushing obtains ginkgo leaf powder and minces, and ginkgo leaf is crushed
Water bath heating device is moved into after object and sodium hydroxide solution mixing, 60~70 DEG C is heated to, is standing and soaking 40~50min,
Obtain alkali leaching product；
(4) spare weak yellow liquid, above-mentioned alkali leaching product are uniformly mixed, are put into reaction kettle, temperature is set, is stirred to react,
It collects after reaction and obtains reaction product；
(5) 20~30 parts of above-mentioned reaction products, 20~30 parts of Black Warrior stone plain weave fiber cloths, 15~20 parts of flax plain weave fibers are weighed
Cloth, 30~35 parts of epoxy resin, 10~12 parts of peroxide ethyl ketones are uniformly mixed and cold press are added, and pressure, temperature, cold pressing treatment is arranged
After obtain cold pressing treatment product, cold pressing treatment product is put into vulcanizing press after cold pressing, setting temperature be 120~
130 DEG C, pressure is 5.0~6.0MPa, 4~5h of hot-pressing processing, collects treated product, as flame-proof weather-resisting type casting glue.
Methylvinyldichlorosilane described in step (1), dimethylphosphite, aluminium chloride mass ratio be 2 ︰, 2 ︰ 1.
The volume of distilled water described in step (2) is the 15% of mixeding liquid volume, the mixings time of mix products is 30~
40min, time of repose are 2~3h.
It is 2 ︰ 5, the matter of sodium hydroxide solution that ginkgo leaf powder described in step (3), which minces with the mass ratio of sodium hydroxide solution,
Measuring score is 20%.
Spare weak yellow liquid described in step (4), above-mentioned alkali soak the mass ratio that product mixes for 3 ︰ 2, in reaction kettle
Temperature is 150~200 DEG C, and the time being stirred to react is 2~3h.
Pressure in cold press described in step (5) is 2.0~3.0MPa, and temperature is 50~60 DEG C, the cold pressing treatment time
For 1~2h.
The beneficial effects of the present invention are:
(1) present invention makees using methylvinyldichlorosilane, dimethylphosphite, aluminium chloride as raw material in the catalysis of aluminium chloride
Reacted again with distilled water with lower generation product, be made silyl phosphate, then using ginkgo leaf as raw material, after alkali steeps with it is siliceous
Phosphate hybrid reaction finally will so that silyl phosphate is bonded with the hydroxyls dehydrate on plant fiber and is fixed on fiber
Ginkgo leaf fibre, Black Warrior mineral wool, flax fiber mixing, and by high temperature high pressure process silyl phosphate is cross-linked to form greatly
Molecular compound obtains high flame retardant high-weatherability casting glue, and the present invention is with methylvinyldichlorosilane and phosphorous acid diformazan
Ester is raw material, and addition reaction occurs under the catalysis of aluminium chloride, and with distilled water substitution reaction occurs for the product of generation again, and synthesis contains
Silicon phosphate, the good flame resistance of silyl phosphate, and have the characteristics that efficient, nontoxic, low cigarette, anti-drip, free of contamination, in high temperature
Under the conditions of, silyl phosphate can be bonded with the hydroxyls dehydrate on plant fiber and be fixed on fiber, so that fiber is with fire-retardant
Property；
(2) using ginkgo leaf as raw material, by dipping by lye, so that the lignin portion in ginkgo leaf decomposes, the part of lignin
It decomposes so that the cellulose in ginkgo leaf raw material is separated from each other, this portion of cellulose plays cementation, ginkgo in casting glue
Undecomposed lignin can be used as crosslinking agent in leaf, improve the crosslink density of casting glue.In addition, containing a large amount of in ginkgo leaf
The elements such as iron, magnesium react with sodium hydroxide and generate iron hydroxide, magnesium hydroxide, the good flame resistance of iron hydroxide and magnesium hydroxide,
The anti-flammability of casting glue can be promoted, ginkgo leaf fibre, Black Warrior mineral wool, the water resistance of flax fiber, ageing-resistant performance are excellent,
The mixing of 3 kinds of different fibers is so that the weatherability of mixture is more excellent, to improve the weatherability of casting glue, cold pressing treatment is profound
Both military stone plain weave fiber cloth, flax plain weave fiber cloth and acrylic acid epoxy resin exclude the air between fiber and glue-line, make
Come into full contact with, after by high temperature high pressure process so that silyl phosphate is cross-linked to form macromolecular compound, compound segment increases
Long, molecular mass increases, and casting glue anti-flammability is promoted, so that before flame-proof weather-resisting type casting glue of the present invention has wide application
Scape.
Specific embodiment
Methylvinyldichlorosilane, dimethylphosphite, aluminium chloride that mass ratio is 2 ︰, 2 ︰ 1 are added in reaction kettle,
Blender, thermometer, nitrogen conduit and condenser and chlorine absorption unit are loaded onto, and is passed through nitrogen until displacement into reaction kettle
All air out are heated to 60~70 DEG C, are stirred to react 3~4h, obtain mixture under nitrogen protection；It will be above-mentioned mixed
4~the 5h that flows back after object is warming up to 90~100 DEG C is closed, mixed liquor is obtained, then mixed liquor is down to room temperature, mixeding liquid volume is added dropwise
15% distilled water, until not having gas releasing, reaction was completed, obtains mix products, after mix products are stirred 30~40min
2~3h is stood, upper layer weak yellow liquid is collected, it is spare；It weighs ginkgo leaf to be put into tissue pulverizer, crushes 40~50min and obtain
Mince to ginkgo leaf powder, by the ginkgo leaf powder that mass ratio is 2 ︰ 5 mince with mass fraction be 20% sodium hydroxide solution mix after
Water bath heating device is moved into, 60~70 DEG C is heated to, is standing and soaking 40~50min, obtains alkali leaching product；It is by mass ratio
Spare weak yellow liquid, the above-mentioned alkali leaching product of 3 ︰ 2 is uniformly mixed, and is put into reaction kettle, setting temperature is 150~200 DEG C, is stirred
2~3h of reaction is mixed, collects obtain reaction product after reaction；Weigh 20~30 parts of above-mentioned reaction products, 20~30 parts of Black Warriors
Stone plain weave fiber cloth, 15~20 parts of flax plain weave fiber cloths, 30~35 parts of epoxy resin, 10~12 parts of peroxide ethyl ketones are uniformly mixed
Cold press is added, is that 2.0~3.0MPa is cold-pressed after 1~2h of cold pressing treatment under conditions of temperature is 50~60 DEG C in pressure
Product is handled, cold pressing treatment product is put into vulcanizing press after cold pressing, setting temperature is 120~130 DEG C, and pressure is
5.0~6.0MPa, 4~5h of hot-pressing processing collect treated product, as flame-proof weather-resisting type casting glue.
Methylvinyldichlorosilane, dimethylphosphite, aluminium chloride that mass ratio is 2 ︰, 2 ︰ 1 are added in reaction kettle,
Blender, thermometer, nitrogen conduit and condenser and chlorine absorption unit are loaded onto, and is passed through nitrogen until displacement into reaction kettle
All air out are heated to 60 DEG C, are stirred to react 3h, obtain mixture under nitrogen protection；Said mixture is heated up
Flow back 4h after to 90 DEG C, obtains mixed liquor, then mixed liquor is down to room temperature, the distilled water of mixeding liquid volume 15% is added dropwise, until not having
There is gas releasing, reaction was completed, obtains mix products, stands 2h after mix products are stirred 30min, collects upper layer light yellow liquid
Body, it is spare；It weighs ginkgo leaf to be put into tissue pulverizer, crushing 40min obtains ginkgo leaf powder and minces, and is 2 ︰'s 5 by mass ratio
Water bath heating device is moved into after the sodium hydroxide solution mixing that it is 20% with mass fraction that ginkgo leaf powder, which minces, is heated to 60
DEG C, it is standing and soaking 40min, obtains alkali leaching product；Mass ratio is soaked product for spare weak yellow liquid, the above-mentioned alkali of 3 ︰ 2 to mix
Uniformly, it is put into reaction kettle, setting temperature is 150 DEG C, is stirred to react 2h, collects obtain reaction product after reaction；It weighs
20 parts of above-mentioned reaction products, 20 parts of Black Warrior stone plain weave fiber cloths, 15 parts of flax plain weave fiber cloths, 30 parts of epoxy resin, 10 parts of mistakes
Oxygen ethyl ketone, which is uniformly mixed, is added cold press, is that 2.0MPa is obtained cold under conditions of temperature is 50 DEG C after cold pressing treatment 1h in pressure
Cold pressing treatment product, is put into vulcanizing press by pressure processing product after cold pressing, and setting temperature is 120 DEG C, and pressure is
5.0MPa, hot-pressing processing 4h collect treated product, as flame-proof weather-resisting type casting glue.
Methylvinyldichlorosilane, dimethylphosphite, aluminium chloride that mass ratio is 2 ︰, 2 ︰ 1 are added in reaction kettle,
Blender, thermometer, nitrogen conduit and condenser and chlorine absorption unit are loaded onto, and is passed through nitrogen until displacement into reaction kettle
All air out are heated to 65 DEG C, are stirred to react 3.5h, obtain mixture under nitrogen protection；By said mixture liter
Temperature obtains mixed liquor to the 4.5h that flows back after 95 DEG C, then mixed liquor is down to room temperature, the distilled water of mixeding liquid volume 15% is added dropwise, directly
It is released to no gas, reaction was completed, obtains mix products, stands 2.5h after mix products are stirred 35min, it is light to collect upper layer
Yellow liquid, it is spare；It weighs ginkgo leaf to be put into tissue pulverizer, crushing 45min obtains ginkgo leaf powder and minces, and is by mass ratio
Water bath heating device, heat temperature raising are moved into after the sodium hydroxide solution mixing that it is 20% with mass fraction that the ginkgo leaf powder of 2 ︰ 5, which minces,
To 65 DEG C, it is standing and soaking 45min, obtains alkali leaching product；Mass ratio is soaked into product for spare weak yellow liquid, the above-mentioned alkali of 3 ︰ 2
It is uniformly mixed, is put into reaction kettle, setting temperature is 170 DEG C, is stirred to react 2.5h, and collection is obtained reacting and be produced after reaction
Object；Weigh 25 parts of above-mentioned reaction products, 25 parts of Black Warrior stone plain weave fiber cloths, 17 parts of flax plain weave fiber cloths, 32 parts of epoxy resin,
11 parts of peroxide ethyl ketones, which are uniformly mixed, is added cold press, is 2.5MPa in pressure, under conditions of temperature is 55 DEG C, cold pressing treatment 1.5h
After obtain cold pressing treatment product, cold pressing treatment product is put into vulcanizing press after cold pressing, setting temperature be 125 DEG C,
Pressure is 5.5MPa, hot-pressing processing 4.5h, collect that treated product, as flame-proof weather-resisting type casting glue.
Methylvinyldichlorosilane, dimethylphosphite, aluminium chloride that mass ratio is 2 ︰, 2 ︰ 1 are added in reaction kettle,
Blender, thermometer, nitrogen conduit and condenser and chlorine absorption unit are loaded onto, and is passed through nitrogen until displacement into reaction kettle
All air out are heated to 70 DEG C, are stirred to react 4h, obtain mixture under nitrogen protection；Said mixture is heated up
Flow back 5h after to 100 DEG C, obtains mixed liquor, then mixed liquor is down to room temperature, the distilled water of mixeding liquid volume 15% is added dropwise, until
There is no gas releasing, reaction was completed, obtains mix products, stands 3h after mix products are stirred 40min, it is faint yellow to collect upper layer
Liquid, it is spare；It weighs ginkgo leaf to be put into tissue pulverizer, crushing 50min obtains ginkgo leaf powder and minces, and is 2 ︰ 5 by mass ratio
Ginkgo leaf powder mince with mass fraction be 20% sodium hydroxide solution mixing after move into water bath heating device, be heated to
70 DEG C, it is standing and soaking 50min, obtains alkali leaching product；Mass ratio is soaked product for spare weak yellow liquid, the above-mentioned alkali of 3 ︰ 2 to mix
It closes uniformly, is put into reaction kettle, setting temperature is 200 DEG C, is stirred to react 3h, collects obtain reaction product after reaction；Claim
Take 30 parts of above-mentioned reaction products, 30 parts of Black Warrior stone plain weave fiber cloths, 20 parts of flax plain weave fiber cloths, 35 parts of epoxy resin, 12 parts
Peroxide ethyl ketone, which is uniformly mixed, is added cold press, is that 3.0MPa is obtained after cold pressing treatment 2h under conditions of temperature is 60 DEG C in pressure
Cold pressing treatment product is put into vulcanizing press by cold pressing treatment product after cold pressing, and setting temperature is 130 DEG C, and pressure is
6.0MPa, hot-pressing processing 5h collect treated product, as flame-proof weather-resisting type casting glue.
The flame-proof weather-resisting type casting glue that comparative example is produced with Shenzhen company is as a comparison case to produced by the present invention fire-retardant
Flame-proof weather-resisting type casting glue in weather-proof casting glue and comparative example carries out performance detection, and testing result is as shown in table 1:
Test method:
Heat distortion temperature test is detected by GB1634-79 standard；
Weatherability test process are as follows: each casting glue is received into ultraviolet light irradiation, irradiation used ultraviolet-uisible spectrophotometer after 6 hours
Test yellowness index；
Yellowness index test method is tested by the saying of xanthochromia series Δ Yi, is divided by yellowness index:
0 grade: without discoloration, Δ Yi≤1.5；
1 grade: very light discolouration, 1.6 < Δ Yi≤3.0；
2 grades: light discolouration, 3.1 < Δ Yi≤6.0；
3 grades: obvious discoloration, 6.1 < Δ Yi≤9.0；
4 grades: larger discoloration, 9.1 < Δ Yi≤12.0；
5 grades: serious discoloration, 12.0 < Δ Yi.
By flame retardant rating by HB, the standard that V-2, V-1 are incremented by step by step to V-0 is detected for flame retardant rating test；
Oxygen index (OI) test carries out performance detection using oxygen index measurer.
1 casting glue performance measurement result of table
| Test item | Example 1 | Example 2 | Example 3 | Comparative example |
| Heat distortion temperature (0.45MPa/ DEG C) | 88 | 89 | 90 | 60 |
| Yellowness index (Δ Yi) | 0.8 | 0.7 | 0.6 | 6.8 |
| Flame retardant rating (grade) | 1 | 0 | 0 | 2 |
| Oxygen index (OI) | 33 | 33 | 34 | 22 |
According to above-mentioned detection data flame-proof weather-resisting type casting glue good weatherability of the invention, yellowness index is low, good flame resistance,
0 grade of flame retardant rating, oxygen index (OI) is high, has broad application prospects.
Claims (6)
1. a kind of preparation method of flame-proof weather-resisting type casting glue, it is characterised in that specific preparation step are as follows:
(1) methylvinyldichlorosilane, dimethylphosphite, aluminium chloride are added in reaction kettle, load onto blender, temperature
Meter, nitrogen conduit and condenser and chlorine absorption unit, and nitrogen is passed through until displacing all air, in nitrogen into reaction kettle
Under gas shielded, 60~70 DEG C are heated to, 3~4h is stirred to react, obtains mixture；
(2) flow back 4~5h after said mixture being warming up to 90~100 DEG C, obtains mixed liquor, then mixed liquor is down to room temperature,
Distilled water is added dropwise, until not having gas releasing, reaction was completed, obtains mix products, stands after mix products are stirred, in collection
Layer weak yellow liquid, it is spare；
(3) it weighs ginkgo leaf to be put into tissue pulverizer, 40~50min of crushing obtains ginkgo leaf powder and minces, and ginkgo leaf is crushed
Water bath heating device is moved into after object and sodium hydroxide solution mixing, 60~70 DEG C is heated to, is standing and soaking 40~50min,
Obtain alkali leaching product；
(4) spare weak yellow liquid, above-mentioned alkali leaching product are uniformly mixed, are put into reaction kettle, temperature is set, is stirred to react,
It collects after reaction and obtains reaction product；
(5) 20~30 parts of above-mentioned reaction products, 20~30 parts of Black Warrior stone plain weave fiber cloths, 15~20 parts of flax plain weave fibers are weighed
Cloth, 30~35 parts of epoxy resin, 10~12 parts of peroxide ethyl ketones are uniformly mixed and cold press are added, and pressure, temperature, cold pressing treatment is arranged
After obtain cold pressing treatment product, cold pressing treatment product is put into vulcanizing press after cold pressing, setting temperature be 120~
130 DEG C, pressure is 5.0~6.0MPa, 4~5h of hot-pressing processing, collects treated product, as flame-proof weather-resisting type casting glue.
2. a kind of preparation method of flame-proof weather-resisting type casting glue according to claim 1, it is characterised in that: step (1) institute
The methylvinyldichlorosilane stated, dimethylphosphite, aluminium chloride mass ratio be 2 ︰, 2 ︰ 1.
3. a kind of preparation method of flame-proof weather-resisting type casting glue according to claim 1, it is characterised in that: step (2) institute
The volume for the distilled water stated is the 15% of mixeding liquid volume, and the mixings time of mix products is 30~40min, time of repose is 2~
3h。
4. a kind of preparation method of flame-proof weather-resisting type casting glue according to claim 1, it is characterised in that: step (3) institute
It is 2 ︰ 5 that the ginkgo leaf powder stated, which minces with the mass ratio of sodium hydroxide solution, and the mass fraction of sodium hydroxide solution is 20%.
5. a kind of preparation method of flame-proof weather-resisting type casting glue according to claim 1, it is characterised in that: step (4) institute
The mass ratio of the spare weak yellow liquid, the leaching product mixing of above-mentioned alkali stated is 3 ︰ 2, and the temperature in reaction kettle is 150~200 DEG C,
The time being stirred to react is 2~3h.
6. a kind of preparation method of flame-proof weather-resisting type casting glue according to claim 1, it is characterised in that: step (5) institute
The pressure in cold press stated is 2.0~3.0MPa, and temperature is 50~60 DEG C, and the cold pressing treatment time is 1~2h.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811046806.9A CN109266279A (en) | 2018-09-08 | 2018-09-08 | A kind of preparation method of flame-proof weather-resisting type casting glue |
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|---|---|---|---|
| CN201811046806.9A CN109266279A (en) | 2018-09-08 | 2018-09-08 | A kind of preparation method of flame-proof weather-resisting type casting glue |
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| CN109266279A true CN109266279A (en) | 2019-01-25 |
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| CN201811046806.9A Pending CN109266279A (en) | 2018-09-08 | 2018-09-08 | A kind of preparation method of flame-proof weather-resisting type casting glue |
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