CN109627767A - A kind of technique and method preparing flame retardant silica gel foam using liquid silica gel - Google Patents
A kind of technique and method preparing flame retardant silica gel foam using liquid silica gel Download PDFInfo
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
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- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
- C08J3/246—Intercrosslinking of at least two polymers
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0061—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof characterized by the use of several polymeric components
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0066—Use of inorganic compounding ingredients
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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- C08J9/009—Use of pretreated compounding ingredients
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- C08J2383/00—Characterised by the use of 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; Derivatives of such polymers
- C08J2383/04—Polysiloxanes
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- C08J2483/00—Characterised by the use of 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; Derivatives of such polymers
- C08J2483/04—Polysiloxanes
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2483/00—Characterised by the use of 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; Derivatives of such polymers
- C08J2483/04—Polysiloxanes
- C08J2483/05—Polysiloxanes containing silicon bound to hydrogen
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2483/00—Characterised by the use of 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; Derivatives of such polymers
- C08J2483/04—Polysiloxanes
- C08J2483/06—Polysiloxanes containing silicon bound to oxygen-containing groups
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- C08J2483/00—Characterised by the use of 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; Derivatives of such polymers
- C08J2483/04—Polysiloxanes
- C08J2483/07—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
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- 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
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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- C—CHEMISTRY; METALLURGY
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/10—Encapsulated ingredients
Abstract
The invention discloses a kind of techniques and method that flame retardant silica gel foam is prepared using liquid silica gel, it is made by following raw material by mass parts: 100 parts of liquid hydroxyl-terminated injecting two methyl siloxane, 10 parts of liquid end hydroxy phenyl siloxanes, 2-5 parts of vinyl silicone oil, 2-5 parts of ethyl orthosilicate, 4-10 parts of containing hydrogen silicone oil, 4-10 parts of hydroxy silicon oil, 40-60 parts of fire retardant, 10-15 parts of white carbon black, 0.2-0.4 parts of platinum catalyst, 0.4-0.6 parts of inhibitor, 4-6 parts of mill base flame retardant silica gel foam fire-retardant ranks produced by the present invention are up to 94V0, it can be used for a long time in the environment of -55-220 degrees Celsius for a long time.
Description
Technical field
The present invention relates to flame retardant silica gel foam manufacture technology fields, specially a kind of to prepare flame retardant silica gel using liquid silica gel
The technique and method of foam.
Background technique
Flame retardant silica gel foam is widely used in aircraft, high-speed rail train, aerospace craft, new energy car battery packet, notebook
The fields such as computer, personal electric product, medical supplies.
Currently, the indexs such as 200 degree of silica gel foam produced domestic or more hot environment adaptability are not up to external
The level of similar product eventually leads to the defects of leakproofness is bad, and damping is bad, it would therefore be highly desirable to which a kind of improved technology solves
Certainly this problem in the presence of the prior art.
Summary of the invention
The purpose of the present invention is to provide a kind of flame retardant silica gel foams and preparation method thereof, to solve in above-mentioned background technique
The problem of proposition.
To achieve the above object, the invention provides the following technical scheme: a kind of flame retardant silica gel prepared using liquid silica gel
Foam is made by following raw material by mass parts: 100 parts of liquid hydroxyl-terminated injecting two methyl siloxane, liquid end hydroxy phenyl silicon oxygen
10 parts of alkane, 2-5 parts of vinyl silicone oil, 2-5 parts of ethyl orthosilicate, 4-10 parts of containing hydrogen silicone oil, 4-10 parts of hydroxy silicon oil, fire retardant
40-60 parts, 10-15 parts of white carbon black, 0.2-0.4 parts of platinum catalyst, 0.4-0.6 parts of inhibitor, 4-6 parts of mill base.
Preferably, it is made by following raw material by mass parts: 100 parts of liquid hydroxyl-terminated injecting two methyl siloxane, liquid end hydroxyl
10 parts of base phenyl siloxane, 4 parts of vinyl silicone oil, 4 parts of ethyl orthosilicate, 7 parts of containing hydrogen silicone oil, 7 parts of hydroxy silicon oil, fire retardant 50
Part, 15 parts of white carbon black, 0.3 part of platinum catalyst, 0.3 part of inhibitor, 5 parts of mill base.
Preferably, the fire retardant can be following one or more: the phosphorus-nitrogen containing flame retardant that is wrapped, silicon powder,
The metal hydroxides being wrapped, the metal oxide being wrapped.
Preferably, comprising the following steps:
Step 1: liquid hydroxyl-terminated injecting two methyl siloxane, liquid end hydroxy phenyl siloxanes, vinyl silicon are proportionally added into
Oil, ethyl orthosilicate, white carbon black, hydroxy silicon oil, fire retardant are added in kneader after mixing and are heated to 80 degree of kneadings, mediate speed
Rate is 50-80 revs/min, and the time is -8 hours 3 hours, obtains mixture YA；
Step 2: being added mixture YA high speed for platinum catalyst and mediate, and mediating rate is 30-50 revs/min, time 1-2
Hour, obtain mixture A；
Step 3: containing hydrogen silicone oil, inhibitor, mill base mixing are uniformly dispersed with dispersion machine, rate of dispersion: 1000-1500 turns/
Point, jitter time is to obtain mixture B in 0.5-2 hours；
Step 4: mixture B being added in mixture A and is mediated, and mediating speed is 50-80 revs/min, and the time is to go out for 20-45 minutes
Material obtains mixture C；
Step 5: mixture C is coated in flakes, then vulcanizes 30 minutes through 80-200 degree baking oven up to flame retardant silica gel foam.
Compared with prior art, the beneficial effects of the present invention are:
Preparation method of the present invention is simple, and flame retardant silica gel foam obtained can keep good under 200 degree of environment above of high temperature for a long time
Good mechanical performance, and the burn-in test thickness loss rate that 100 degree of compressions 50% carry out 22 hours is lower than 5%, in addition, the present invention adopts
Production method low manufacture cost, it can be ensured that each component material is sufficiently mixed, and further improves flame retardant silica gel foam
Performance.
Specific embodiment
The following is a clear and complete description of the technical scheme in the embodiments of the invention, it is clear that described embodiment
Only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, the common skill in this field
Art personnel every other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.
The present invention provides a kind of technical solution: a kind of flame retardant silica gel foam prepared using liquid silica gel, by following raw material
It is made by mass parts: 100 parts of liquid hydroxyl-terminated injecting two methyl siloxane, 10 parts of liquid end hydroxy phenyl siloxanes, vinyl silicon
2-5 parts oily, 2-5 parts of ethyl orthosilicate, 4-10 parts of containing hydrogen silicone oil, 4-10 parts of hydroxy silicon oil, 40-60 parts of fire retardant, white carbon black 10-
15 parts, 0.2-0.4 parts of platinum catalyst, 0.4-0.6 parts of inhibitor, 4-6 parts of mill base.
Wherein, fire retardant can be following one or more: the phosphorus-nitrogen containing flame retardant that is wrapped, is wrapped silicon powder
Metal hydroxides, the metal oxide that is wrapped.
Embodiment, it is suitble to spring, winter, autumn.
Embodiment one:
A kind of flame retardant silica gel foam prepared using liquid silica gel, is made by following raw material by mass parts: liquid terminal hydroxy group poly- two
100 parts of methylsiloxane, 10 parts of liquid end hydroxy phenyl siloxanes, 2 parts of vinyl silicone oil, 2 parts of ethyl orthosilicate, containing hydrogen silicone oil
4 parts, 4 parts of hydroxy silicon oil, 40 parts of fire retardant, 10 parts of white carbon black, 0.2 part of platinum catalyst, 0.4 part of inhibitor, 4 parts of mill base.
The preparation method of the present embodiment the following steps are included:
Step 1: 100 parts of hydroxyl-terminated injecting two methyl siloxane, 10 parts of liquid end hydroxy phenyl siloxanes, 2 parts of vinyl silicone oil,
80 degree are heated in addition kneader after 2 parts of ethyl orthosilicate, 10 parts of white carbon black, 4 parts of hydroxy silicon oil, 40 parts of fire retardant mixing to pinch
It closes, mediating rate is 70 revs/min, and the time is 7 hours, obtains mixture YA；
Step 2: being added mixture YA high speed for platinum catalyst and mediate, and mediating rate is 40 revs/min, and the time is 1.5 small
When, obtain mixture A；
Step 3: 4 parts of 4 parts of containing hydrogen silicone oil, 0.4 part of inhibitor, mill base mixing are uniformly dispersed with dispersion machine, rate of dispersion:
1200 revs/min, jitter time is to obtain mixture B in 1.5 hours；
Step 4: mixture B being added in mixture A and is mediated, and mediating speed is 70 revs/min, and the time is that discharging in 45 minutes obtains
Mixture C；
Step 5: mixture C is coated in flakes, then vulcanizes 30 minutes through 160 degree of baking ovens up to flame retardant silica gel foam.
Embodiment two:
A kind of flame retardant silica gel foam prepared using liquid silica gel, is made by following raw material by mass parts: liquid terminal hydroxy group poly- two
100 parts of methylsiloxane, 10 parts of liquid end hydroxy phenyl siloxanes, 5 parts of vinyl silicone oil, 2 parts of ethyl orthosilicate, containing hydrogen silicone oil
8 parts, 10 parts of hydroxy silicon oil, 60 parts of fire retardant, 15 parts of white carbon black, 0.4 part of platinum catalyst, 0.6 part of inhibitor, 6 parts of mill base.
The preparation method of the present embodiment the following steps are included:
Step 1: 100 parts of hydroxyl-terminated injecting two methyl siloxane, 10 parts of liquid end hydroxy phenyl siloxanes, 5 parts of vinyl silicone oil,
80 degree are heated in addition kneader after 2 parts of ethyl orthosilicate, 15 parts of white carbon black, 8 parts of hydroxy silicon oil, 60 parts of fire retardant mixing to pinch
It closes, mediating rate is 70 revs/min, and the time is 7 hours, obtains mixture YA；
Step 2: being added mixture YA high speed for platinum catalyst and mediate, and mediating rate is 40 revs/min, and the time is 1.5 small
When, obtain mixture A；
Step 3: 6 parts of 8 parts of containing hydrogen silicone oil, 0.6 part of inhibitor, mill base mixing are uniformly dispersed with dispersion machine, rate of dispersion:
1200 revs/min, jitter time is to obtain mixture B in 1.5 hours；
Step 4: mixture B being added in mixture A and is mediated, and mediating speed is 70 revs/min, and the time is that discharging in 45 minutes obtains
Mixture C；
Step 5: mixture C is coated in flakes, then vulcanizes 30 minutes through 160 degree of baking ovens up to flame retardant silica gel foam.
Embodiment three:
A kind of flame retardant silica gel foam prepared using liquid silica gel, is made by following raw material by mass parts: liquid terminal hydroxy group poly- two
100 parts of methylsiloxane, 10 parts of liquid end hydroxy phenyl siloxanes, 4 parts of vinyl silicone oil, 5 parts of ethyl orthosilicate, containing hydrogen silicone oil
6 parts, 6 parts of hydroxy silicon oil, 50 parts of fire retardant, 13 parts of white carbon black, 0.3 part of platinum catalyst, 0.5 part of inhibitor, 5 parts of mill base.
The preparation method of the present embodiment the following steps are included:
Step 1: 100 parts of hydroxyl-terminated injecting two methyl siloxane, 10 parts of liquid end hydroxy phenyl siloxanes, 4 parts of vinyl silicone oil,
80 degree are heated in addition kneader after 5 parts of ethyl orthosilicate, 13 parts of white carbon black, 6 parts of hydroxy silicon oil, 50 parts of fire retardant mixing to pinch
It closes, mediating rate is 70 revs/min, and the time is 7 hours, obtains mixture YA；
Step 2: being added mixture YA high speed for platinum catalyst and mediate, and mediating rate is 40 revs/min, and the time is 1.5 small
When, obtain mixture A；
Step 3: 5 parts of 6 parts of containing hydrogen silicone oil, 0.5 part of inhibitor, mill base mixing are uniformly dispersed with dispersion machine, rate of dispersion:
1200 revs/min, jitter time is to obtain mixture B in 1.5 hours；
Step 4: mixture B being added in mixture A and is mediated, and mediating speed is 70 revs/min, and the time is that discharging in 45 minutes obtains
Mixture C；
Step 5: mixture C is coated in flakes, then vulcanizes 30 minutes through 160 degree of baking ovens up to flame retardant silica gel foam.
Embodiment one ~ tri- is suitble to spring, winter, autumn, tests by Experimental Comparison, embodiment two reaches optimal mechanical
Energy.
Embodiment, it is suitble to summer
Example IV:
A kind of flame retardant silica gel foam prepared using liquid silica gel, is made by following raw material by mass parts: liquid terminal hydroxy group poly- two
100 parts of methylsiloxane, 10 parts of liquid end hydroxy phenyl siloxanes, 4 parts of vinyl silicone oil, 4 parts of ethyl orthosilicate, containing hydrogen silicone oil
4 parts, 4 parts of hydroxy silicon oil, 60 parts of fire retardant, 15 parts of white carbon black, 0.2 part of platinum catalyst, 0.6 part of inhibitor, 6 parts of mill base.
The preparation method of the present embodiment the following steps are included:
Step 1: 100 parts of liquid hydroxyl-terminated injecting two methyl siloxane, 10 parts of liquid end hydroxy phenyl siloxanes, vinyl silicone oil 4
It is added in kneader after part, 4 parts of ethyl orthosilicate, 15 parts of white carbon black, 4 parts of hydroxy silicon oil, 60 parts of fire retardant mixing and is heated to 80
Degree is mediated, and mediating rate is 70 revs/min, and the time is 4 hours, obtains mixture YA；
Step 2: being added mixture YA high speed for platinum catalyst and mediate, and mediating rate is 40 revs/min, and the time is 1.5 small
When, obtain mixture A；
Step 3: containing hydrogen silicone oil, inhibitor, mill base mixing are uniformly dispersed with dispersion machine, rate of dispersion: 1200 revs/min, dispersion
Time is to obtain mixture B in 30 minutes；
Step 4: mixture B being added in mixture A and is mediated, and mediating speed is 70 revs/min, and the time is that discharging in 30 minutes obtains
Mixture C；
Step 5: mixture C is coated in flakes, then vulcanizes 30 minutes through 160 degree of baking ovens up to flame retardant silica gel foam.
Embodiment five:
A kind of flame retardant silica gel foam prepared using liquid silica gel, is made by following raw material by mass parts: liquid terminal hydroxy group poly- two
100 parts of methylsiloxane, 10 parts of liquid end hydroxy phenyl siloxanes, 3 parts of vinyl silicone oil, 2 parts of ethyl orthosilicate, containing hydrogen silicone oil
6 parts, 10 parts of hydroxy silicon oil, 60 parts of fire retardant, 15 parts of white carbon black, 0.3 part of platinum catalyst, 0.8 part of inhibitor, 6 parts of mill base.
The preparation method of the present embodiment the following steps are included:
Step 1: 100 parts of liquid hydroxyl-terminated injecting two methyl siloxane, 10 parts of liquid end hydroxy phenyl siloxanes, vinyl silicone oil 4
It is added in kneader after part, 4 parts of ethyl orthosilicate, 15 parts of white carbon black, 4 parts of hydroxy silicon oil, 60 parts of fire retardant mixing and is heated to 80
Degree is mediated, and mediating rate is 70 revs/min, and the time is 4 hours, obtains mixture YA；
Step 2: being added mixture YA high speed for platinum catalyst and mediate, and mediating rate is 40 revs/min, and the time is 1.5 small
When, obtain mixture A；
Step 3: containing hydrogen silicone oil, inhibitor, mill base mixing are uniformly dispersed with dispersion machine, rate of dispersion: 1200 revs/min, dispersion
Time is to obtain mixture B in 30 minutes；
Step 4: mixture B being added in mixture A and is mediated, and mediating speed is 70 revs/min, and the time is that discharging in 30 minutes obtains
Mixture C；
Step 5: mixture C is coated in flakes, then vulcanizes 30 minutes through 160 degree of baking ovens up to flame retardant silica gel foam.
Example IV ~ five are suitble to summer, test by Experimental Comparison, embodiment five reaches optimal mechanical properties.
Flame retardant silica gel foam made from each embodiment is tested for the property using the present invention, data is obtained and is as follows:
| Project | Test method | Example one | Example two | Example three | Example four | Example five |
| Pressure deflection (KP) | At room temperature, 25% measurement ASTM D 105 of compression | 48 | 50 | 51 | 52 | 49 |
| Compressive deformation (maximum value %) | 100oC, the 50% test ASTM D 1056 of compression in 22 hours | 1 | 1 | 1 | 0 | 1 |
| Tensile strength (kp) | ASTM D412 | 310 | 324 | 313 | 310 | 316 |
| Elongation % | ASTM D412 | 102 | 106 | 103 | 103 | 111 |
| Water absorption rate % | Room temperature 24 hours | 1 | 1 | 1 | 1 | 1.2 |
| Flame retardant rating | UL-94 | V-0 and HF-1 | V-0 and HF-1 | V-0 and HF-1 | V-0 and HF-1 | V-0 and HF-1 |
| It is recommended to use temperature (oC) | - 55 to 220 | - 55 to 220 | - 55 to 220 | - 55 to 220 | - 55 to 220 |
Preparation method of the present invention is simple, and flame retardant silica gel foam obtained can keep good mechanicalness under high temperature environment for a long time
Energy.In addition, the production method low manufacture cost that the present invention uses, it can be ensured that each component material is sufficiently mixed, and is further increased
The performance of flame retardant silica gel foam.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (4)
1. a kind of flame retardant silica gel foam prepared using liquid silica gel, it is characterised in that: be made by following raw material by mass parts: liquid
100 parts of body hydroxyl-terminated injecting two methyl siloxane, 10 parts of liquid end hydroxy phenyl siloxanes, 2-5 parts of vinyl silicone oil, positive silicic acid second
2-5 parts of ester, 4-10 parts of containing hydrogen silicone oil, 4-10 parts of hydroxy silicon oil, 40-60 parts of fire retardant, 10-15 parts of white carbon black, platinum catalyst
0.2-0.4 parts, 0.4-0.6 parts of inhibitor, 4-6 parts of mill base.
2. a kind of flame retardant silica gel foam prepared using liquid silica gel according to claim 1, it is characterised in that: by following
Raw material is made by mass parts: 100 parts of liquid hydroxyl-terminated injecting two methyl siloxane, 10 parts of liquid end hydroxy phenyl siloxanes, ethylene
4 parts of base silicone oil, 4 parts of ethyl orthosilicate, 7 parts of containing hydrogen silicone oil, 7 parts of hydroxy silicon oil, 50 parts of fire retardant, 15 parts of white carbon black, platinum are urged
0.3 part of agent, 0.3 part of inhibitor, 5 parts of mill base.
3. a kind of flame retardant silica gel foam prepared using liquid silica gel according to claim 1, it is characterised in that: the resistance
Combustion agent can be following one or more: the phosphorus-nitrogen containing flame retardant that is wrapped, silicon powder, the metal hydroxides being wrapped,
The metal oxide being wrapped.
4. realizing a kind of preparation method of flame retardant silica gel foam prepared using liquid silica gel described in claim 1, feature
It is: the following steps are included:
Step 1: liquid hydroxyl-terminated injecting two methyl siloxane, liquid end hydroxy phenyl siloxanes, vinyl silicon are proportionally added into
Oil, ethyl orthosilicate, white carbon black, hydroxy silicon oil, fire retardant are added in kneader after mixing and are heated to 80 degree of kneadings, mediate speed
Rate is 50-80 revs/min, and the time is -8 hours 3 hours, obtains mixture YA；
Step 2: being added mixture YA high speed for platinum catalyst and mediate, and mediating rate is 30-50 revs/min, time 1-2
Hour, obtain mixture A；
Step 3: containing hydrogen silicone oil, inhibitor, mill base mixing are uniformly dispersed with dispersion machine, rate of dispersion: 1000-1500 turns/
Point, jitter time is to obtain mixture B in 0.5-2 hours；
Step 4: mixture B being added in mixture A and is mediated, and mediating speed is 50-80 revs/min, and the time is to go out for 20-45 minutes
Material obtains mixture C；
Step 5: mixture C is coated in flakes, then vulcanizes 30 minutes through 80-200 degree baking oven up to flame retardant silica gel foam.
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| CN110684358A (en) * | 2019-10-14 | 2020-01-14 | 东莞市跨越电子有限公司 | Filling foaming encapsulation silica gel for new energy power battery, preparation method and application |
| CN110964325A (en) * | 2019-12-12 | 2020-04-07 | 苏州然创新材料科技有限公司 | Composition for preparing flame-retardant liquid silica gel foam and flame-retardant liquid silica gel foam |
| CN112094500A (en) * | 2019-06-17 | 2020-12-18 | 王孚望 | Formula and manufacturing method of cow tongue belt of cow nipple cleaning robot |
| CN114381123A (en) * | 2022-01-24 | 2022-04-22 | 新纳奇材料科技江苏有限公司 | Preparation method of ceramic flame-retardant foamed silica gel material |
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