CN109575602A - A kind of preparation method of silicon rubber foam - Google Patents
A kind of preparation method of silicon rubber foam Download PDFInfo
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- CN109575602A CN109575602A CN201811266273.5A CN201811266273A CN109575602A CN 109575602 A CN109575602 A CN 109575602A CN 201811266273 A CN201811266273 A CN 201811266273A CN 109575602 A CN109575602 A CN 109575602A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/06—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
- C08J9/08—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent developing carbon dioxide
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0014—Use of organic additives
- C08J9/0023—Use of organic additives containing oxygen
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- 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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0095—Mixtures of at least two compounding ingredients belonging to different one-dot groups
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/02—CO2-releasing, e.g. NaHCO3 and citric acid
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- 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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- 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
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/04—Ingredients characterised by their shape and organic or inorganic ingredients
-
- 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
- C08K3/24—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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
- C08K7/28—Glass
Abstract
The present invention relates to a kind of preparation methods of silicon rubber foam, belong to foam technology field.Chemical foaming agent is added using chemical blowing forming technique in the present invention in silicon rubber gross rubber, vulcanizing agent, reinforcing agent, fire retardant and thermal insulating filling, sulfur foam is carried out at a certain temperature after being kneaded uniformly obtains silicon rubber foam, the present invention is using magnesium hydroxide and hollow glass micropearl as fire retardant, magnesium hydroxide has good suppression cigarette and smoke effect, it is nontoxic and environmentally protective, the heated crystallization water that decomposes to give off of magnesium hydroxide forms metal oxide, the crystallization water absorbs a large amount of heat, it undergoes phase transition, generate vapor, on the one hand, the reduction of temperature is so that the rate of combustion reaction reduces, slow down the speed for generating fuel gas；On the other hand, the presence of vapor dilutes the O in burning situation field2With the concentration of imflammable gas so that silicon rubber foam have certain flame retardant efficiency.
Description
Technical field
The present invention relates to a kind of preparation methods of silicon rubber foam, belong to foam technology field.
Background technique
Silicon rubber foam because it has been provided simultaneously with the excellent properties of silicon rubber and foamed material, both had using increasingly extensive
There is a high resiliency of rubber, and there is performance possessed by the foams such as sound absorption, damping, is chiefly used in resilient cushion, gasket, sound insulation, exhausted
The relatively high situations of performance requirements such as edge, aviation be heat-insulated.
According to foam structure, silicon rubber foam is divided into obturator-type, open cell type and mixed type.According to processing method difference, silicon
Rubbery foam can be divided into room temperature vulcanized (RTV) and high temperature vulcanized type (HTV).
RTV type be at room temperature, using hydroxy-end capped (condensed type) silicon rubber be basis material, using certain foaming agent
And catalyst, sulfur foam form.RTV type foamed silastic is suitble to foam-in-site, is mainly used in filler, sealing element, damping
Pad etc..Although this foaming method is simple, expansion ratio is big, since silicone rubber material molecular weight is smaller, so obtain
Foamed material mechanical property is poor, and liquid foam uses alkali metal foaming agent, and price is high.
HTV type is at high temperature, to be added certain vulcanizing agent and foaming agent in silicon rubber gross rubber, when vulcanization, because of foaming
Agent decomposes and discharges bulk gas, and gas is wrapped in vulcanizate and is formed.HTV type foamed silastic can be processed into plate
And foam strip.High-temperature silicon disulfide rubber foamed material, sizing material molecular weight is big, obtained foamed material excellent in mechanical performance, mould
The scantling that foam obtains is more stable.
For silicon rubber as specific rubber, use scope is very wide, and while foaming technique is showing improvement or progress day by day, foamed silastic is
It is applied aerospace, cable, damping etc. are multi-field.But domestic silicon rubber foam product still faces problems, example
Such as: cable requires silicon rubber foam to have certain electric property, and space material requires silicon rubber foam to have certain resistance
Combustion property.But silicon rubber foam anti-flammability itself is poor, need to add fire-retardant filler or improve its fire-retardant, mechanics using modified method
Performance etc..In addition, it is domestic at present still not deep enough to silicon rubber vulcanization-foaming system matching Journal of Sex Research, it is difficult to realize bubble
The controllability of pore structure；Domestic silicon rubber foam product, many apparent densities are higher, are difficult to meet the high-end fields such as aerospace
Demand.So how to advanced optimize each factor of processing technology and formula composition, it need to be furtherd investigate.
Further, since H, AC are currently used organic foaming agents, their decomposition temperatures are higher than silicon rubber vulcanization temperature, and
Decomposition reaction has centainly sudden, limits the development of silicon rubber foam foaming technique to a certain extent.Thus, effectively
Foaming agent decomposition temperature is reduced, so that it preferably matches with silicon rubber vulcanization speed, it appears particularly important.But it is domestic at present
Silicon rubber foaming-vulcanization matching correct is still needed to be further increased.Blowing agents and and with being to reduce foaming agent point
The effective ways of temperature are solved, but at present in document in the research of the resolution characteristic in relation to blowing agents mechanism and foaming agent
Not system.
Summary of the invention
The technical problems to be solved by the invention: it for the problem that existing silicon rubber foam material flame retardant property is poor, mentions
A kind of preparation method of silicon rubber foam is supplied.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
(1) according to parts by weight, weigh respectively 20~30 parts of silicon rubber, 1~10 portion of reinforcing agent, 1~5 part of fire retardant, 0.5~
0.7 part of sodium bicarbonate, 0.1~0.5 part of vulcanizing agent, 1~3 part of thermal insulating filling by silicon rubber, reinforcing agent, fire retardant and heat-insulated are filled out
Material mixing, is kneaded and displays, obtain rubber compound A, and rubber compound A is placed in the vacuum oven that temperature is 100~120 DEG C and is heat-treated
2~3h is cooled to room temperature, and obtains rubber compound B, by rubber compound B back mixing, obtains rubber compound C, sodium bicarbonate and vulcanizing agent is added, continue
It is kneaded 10~15min, obtains rubber compound D；
(2) rubber compound D is foamed and is vulcanized, obtained semi-finished product, semi-finished product are heat-treated, be cooled to room temperature to get silicon rubber foam.
Reinforcing agent described in step (1) is that white carbon black and precipitated calcium carbonate in mass ratio 1: 1 mix.
Fire retardant described in step (1) is that hollow glass micropearl and magnesium hydroxide in mass ratio 1: 3 mix.
Vulcanizing agent described in step (1) is dicumyl peroxide.
Thermal insulating filling described in step (1) is that expanded perlite and expanded vermiculite in mass ratio 1: 1 mix.
Mixing described in step (1) is simultaneously displayed to be 70~80 DEG C in temperature, and revolving speed is to be kneaded 20 under 80~100r/min
After~25min, and display at normal temperature 4~6 days.
Back mixing described in step (1) is 3~5min of back mixing in the case where revolving speed is 50~60r/min.
For the vulcanization of foaming described in step (2) to be 120~130 DEG C in temperature, pressure is foaming vulcanization 10 under 8~10MPa
~15min.
Heat treatment described in step (2) is after drying 20~30min in the baking oven for be placed in 150~160 DEG C, to be warming up to 200
~220 DEG C of 1~2h of heat treatment.
The present invention is compared with other methods, and advantageous effects are:
(1) chemical foaming agent, vulcanizing agent, reinforcement is added using chemical blowing forming technique in the present invention in silicon rubber gross rubber
Agent, fire retardant and thermal insulating filling carry out sulfur foam after being kneaded uniformly at a certain temperature and obtain silicon rubber foam, the present invention
Using magnesium hydroxide and hollow glass micropearl as fire retardant, magnesium hydroxide has good suppression cigarette and smoke effect, nontoxic and green
Colour circle is protected, and the heated crystallization water that decomposes to give off of magnesium hydroxide forms metal oxide, and the crystallization water absorbs a large amount of heat, undergoes phase transition,
Generate vapor, on the one hand, the reduction of temperature slows down the speed of generation fuel gas so that the rate of combustion reaction reduces；
On the other hand, the presence of vapor dilutes the O in burning situation field2With the concentration of imflammable gas so that silicon rubber
Foam has certain flame retardant efficiency；
(2) present invention is using sodium bicarbonate as foaming agent, and dicumyl peroxide is as vulcanizing agent, white carbon black and precipitated calcium carbonate
As reinforcing agent, expanded perlite and expanded vermiculite are in activity with the hydroxyl on white carbon black aggregate surface as thermal insulating filling
Molecule segment in the heart, with silicon rubber forms hydrogen bond, and the phase of physics and chemistry occurs with some unsaturated groups on segment
Interaction, to improve the mechanical property of silicon rubber foam.
Specific embodiment
According to parts by weight, weigh respectively 20~30 parts of silicon rubber, 1~10 portion of reinforcing agent, 1~5 part of fire retardant, 0.5~
0.7 part of sodium bicarbonate, 0.1~0.5 part of vulcanizing agent, 1~3 part of thermal insulating filling by silicon rubber, reinforcing agent, fire retardant and heat-insulated are filled out
Material mixing is 70~80 DEG C in temperature, and revolving speed is after being kneaded 20~25min under 80~100r/min, and display 4 at normal temperature~
6 days, rubber compound A is obtained, rubber compound A is placed in the vacuum oven that temperature is 100~120 DEG C and is heat-treated 2~3h, is cooled to room
Temperature obtains rubber compound B, by rubber compound B in the case where revolving speed is 50~60r/min 3~5min of back mixing, obtain rubber compound C, sodium bicarbonate be added
And vulcanizing agent, continue 10~15min of mixing, obtains rubber compound D；By rubber compound D temperature be 120~130 DEG C, pressure be 8~
10~15min of foaming vulcanization, obtains semi-finished product under 10MPa, and semi-finished product are placed in in 150~160 DEG C of baking oven dry 20~30min
Afterwards, 200~220 DEG C of 1~2h of heat treatment are warming up to, are cooled to room temperature to get silicon rubber foam.
Example 1
According to parts by weight, 20 parts of silicon rubber, 1 portion of reinforcing agent, 1 part of fire retardant, 0.5 part of sodium bicarbonate, 0.1 part of sulphur are weighed respectively
Agent, 1 part of thermal insulating filling mix silicon rubber, reinforcing agent, fire retardant and thermal insulating filling, are 70 DEG C in temperature, revolving speed 80r/
It after being kneaded 20min under min, and displays at normal temperature 4 days, obtains rubber compound A, rubber compound A is placed in the vacuum that temperature is 100 DEG C and is done
Be heat-treated 2h in dry case, be cooled to room temperature, obtain rubber compound B, by rubber compound B revolving speed be 50r/min under back mixing 3min, must be kneaded
Sodium bicarbonate and vulcanizing agent is added in glue C, continues to be kneaded 10min, obtains rubber compound D；By rubber compound D temperature be 120 DEG C, pressure
For foaming vulcanization 10min under 8MPa, semi-finished product are obtained, after semi-finished product to be placed in in 150 DEG C of baking oven dry 20min, are warming up to 200
DEG C heat treatment 1h, be cooled to room temperature to get silicon rubber foam.
Example 2
According to parts by weight, 25 parts of silicon rubber, 5 portions of reinforcing agents, 3 parts of fire retardants, 0.6 part of sodium bicarbonate, 0.3 part of sulphur are weighed respectively
Agent, 2 parts of thermal insulating fillings mix silicon rubber, reinforcing agent, fire retardant and thermal insulating filling, are 75 DEG C in temperature, revolving speed 90r/
It after being kneaded 22min under min, and displays at normal temperature 5 days, obtains rubber compound A, rubber compound A is placed in the vacuum that temperature is 110 DEG C and is done
Be heat-treated 2h in dry case, be cooled to room temperature, obtain rubber compound B, by rubber compound B revolving speed be 55r/min under back mixing 4min, must be kneaded
Sodium bicarbonate and vulcanizing agent is added in glue C, continues to be kneaded 12min, obtains rubber compound D；By rubber compound D temperature be 125 DEG C, pressure
For foaming vulcanization 12min under 9MPa, semi-finished product are obtained, after semi-finished product to be placed in in 155 DEG C of baking oven dry 25min, are warming up to 210
DEG C heat treatment 1h, be cooled to room temperature to get silicon rubber foam.
Example 3
According to parts by weight, 30 parts of silicon rubber, 10 portions of reinforcing agents, 5 parts of fire retardants, 0.7 part of sodium bicarbonate, 0.5 part are weighed respectively
Vulcanizing agent, 3 parts of thermal insulating fillings mix silicon rubber, reinforcing agent, fire retardant and thermal insulating filling, are 80 DEG C in temperature, revolving speed is
It after being kneaded 25min under 100r/min, and displays at normal temperature 6 days, obtains rubber compound A, it is 120 DEG C that rubber compound A, which is placed in temperature,
Be heat-treated 3h in vacuum oven, be cooled to room temperature, obtain rubber compound B, by rubber compound B revolving speed be 60r/min under back mixing 5min,
Rubber compound C is obtained, sodium bicarbonate and vulcanizing agent is added, continues to be kneaded 15min, obtains rubber compound D；By rubber compound D temperature be 130
DEG C, pressure is foaming vulcanization 15min under 10MPa, semi-finished product are obtained, after semi-finished product to be placed in in 160 DEG C of baking oven dry 30min,
220 DEG C of heat treatment 2h are warming up to, are cooled to room temperature to get silicon rubber foam.
Reference examples: the silicon rubber foam of Dongguan company production.
The silicon rubber foam that example and reference examples are prepared is detected, specific detection is as follows:
Flame retardant property: oxygen index (OI) (LOI) of this experiment using oxygen index measurer HC-2 test silicon rubber foam, the preparation of sample
Referring to the standard of GB527.80~150mm of specimen length；6.5 ± 0.5mm of width；With a thickness of foamed silastic thickness.
Mechanical property: tensile strength, elongation at break are referring to the relevant standard testing of country.
Specific test result such as table 1.
1 performance characterization contrast table of table
| Detection project | Example 1 | Example 2 | Example 3 | Reference examples |
| LOI | 30 | 31 | 32 | 10 |
| Tensile strength/MPa | 0.885 | 0.891 | 0.886 | 0.510 |
| Elongation at break/% | 293 | 292 | 289 | 228 |
As shown in Table 1, silicon rubber foam prepared by the present invention has good mechanical property and flame retardant property.
Claims (9)
1. a kind of preparation method of silicon rubber foam, it is characterised in that specific preparation step are as follows:
(1) according to parts by weight, weigh respectively 20~30 parts of silicon rubber, 1~10 portion of reinforcing agent, 1~5 part of fire retardant, 0.5~
0.7 part of sodium bicarbonate, 0.1~0.5 part of vulcanizing agent, 1~3 part of thermal insulating filling by silicon rubber, reinforcing agent, fire retardant and heat-insulated are filled out
Material mixing, is kneaded and displays, obtain rubber compound A, and rubber compound A is placed in the vacuum oven that temperature is 100~120 DEG C and is heat-treated
2~3h is cooled to room temperature, and obtains rubber compound B, by rubber compound B back mixing, obtains rubber compound C, sodium bicarbonate and vulcanizing agent is added, continue
It is kneaded 10~15min, obtains rubber compound D；
(2) rubber compound D is foamed and is vulcanized, obtained semi-finished product, semi-finished product are heat-treated, be cooled to room temperature to get silicon rubber foam.
2. a kind of preparation method of silicon rubber foam according to claim 1, it is characterised in that: benefit described in step (1)
Strong agent is that white carbon black and precipitated calcium carbonate in mass ratio 1: 1 mix.
3. a kind of preparation method of silicon rubber foam according to claim 1, it is characterised in that: resistance described in step (1)
Firing agent is that hollow glass micropearl and magnesium hydroxide in mass ratio 1: 3 mix.
4. a kind of preparation method of silicon rubber foam according to claim 1, it is characterised in that: sulphur described in step (1)
Agent is dicumyl peroxide.
5. a kind of preparation method of silicon rubber foam according to claim 1, it is characterised in that: described in step (1) every
Hot filler is that expanded perlite and expanded vermiculite in mass ratio 1: 1 mix.
6. a kind of preparation method of silicon rubber foam according to claim 1, it is characterised in that: mixed described in step (1)
It refines and displays to be 70~80 DEG C in temperature, after revolving speed is is kneaded 20~25min under 80~100r/min, and display at normal temperature
4~6 days.
7. a kind of preparation method of silicon rubber foam according to claim 1, it is characterised in that: step is returned described in (1)
Refining is 3~5min of back mixing in the case where revolving speed is 50~60r/min.
8. a kind of preparation method of silicon rubber foam according to claim 1, it is characterised in that: hair described in step (2)
To be 120~130 DEG C in temperature, pressure is 10~15min of foaming vulcanization under 8~10MPa for bubble vulcanization.
9. a kind of preparation method of silicon rubber foam according to claim 1, it is characterised in that: heat described in step (2)
After processing is is placed in 150~160 DEG C of baking oven dry 20~30min, it is warming up to 200~220 DEG C of 1~2h of heat treatment.
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Cited By (4)
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| CN110551397A (en) * | 2019-08-23 | 2019-12-10 | 张昌录 | Aerogel-containing heat-insulating silicone rubber foam material and preparation method thereof |
| CN112480686A (en) * | 2020-12-03 | 2021-03-12 | 常州市沃科科技有限公司 | Foaming silicon rubber core material and foaming heat-insulation buffering composite material |
| CN112876847A (en) * | 2020-12-30 | 2021-06-01 | 嘉兴依赛新材料科技有限公司 | Foaming silicone rubber and preparation method thereof |
| CN115029003A (en) * | 2022-07-14 | 2022-09-09 | 歌尔股份有限公司 | Liquid silica gel, silica gel part and electronic equipment |
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Cited By (5)
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| CN112480686A (en) * | 2020-12-03 | 2021-03-12 | 常州市沃科科技有限公司 | Foaming silicon rubber core material and foaming heat-insulation buffering composite material |
| CN112876847A (en) * | 2020-12-30 | 2021-06-01 | 嘉兴依赛新材料科技有限公司 | Foaming silicone rubber and preparation method thereof |
| CN115029003A (en) * | 2022-07-14 | 2022-09-09 | 歌尔股份有限公司 | Liquid silica gel, silica gel part and electronic equipment |
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Application publication date: 20190405 |