CN106977724A - A kind of foamed silastic and preparation method thereof - Google Patents
A kind of foamed silastic and preparation method thereof Download PDFInfo
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- C08J9/10—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 nitrogen, the blowing agent being a compound containing a nitrogen-to-nitrogen bond
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- 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
- C08J9/10—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 nitrogen, the blowing agent being a compound containing a nitrogen-to-nitrogen bond
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- C08J9/10—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 nitrogen, the blowing agent being a compound containing a nitrogen-to-nitrogen bond
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- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
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Abstract
The invention provides a kind of foamed silastic and preparation method thereof.The foamed silastic includes the raw material components of following mass fraction：30 60 parts of Vinyl MQ silicon resins, 40 70 parts of containing hydrogen silicone oils, 2 15 parts of hydroxy silicon oils, 20 50 parts of fillers, 0.05 0.5 parts of thermosensitive type foaming agents and 0.02 0.15 parts of catalyst.The preparation method comprises the following steps：The each component in addition to catalyst is mixed by formula ratio first；Then the catalyst of formula ratio and obtained mixed material are stirred and mixed, carried out one step foaming solidification, obtain semi-finished product；Second time of foaming solidification finally is carried out to the semi-finished product, the foamed silastic is obtained.The foamed silastic that the present invention is provided is while relatively low density is ensured, also with higher tearing strength and hardness.
Description
Technical field
The invention belongs to silicon rubber technical field, and in particular to a kind of foamed silastic and preparation method thereof.
Background technology
The existing silicon rubber heat-resisting of foamed silastic, cold-resistant, electrical insulating property and fire-retardant excellent characteristic, have sponge material again
The intrinsic elasticity of material.The characteristic of the characteristic of organosilicon polymer and foamed material is incorporated into one by Silicone foam, because
And the good characteristic that not only there is above-mentioned organosilicon polymer to have, also with good absorption mechanical oscillation or impact and height
The physical characteristic of frequency damping, belongs to high-performance polymer flexible foams.Silicone foam and common flexibel polyurethane
Sponge compared to having the advantages that nontoxic, high-low temperature resistant, it is protection against the tide, uvioresistant, resist chemical, anti-aging and be unlikely to deform, make
Obtain organic foamed silastic material more and more of interest by people.
Foamed silastic can be matrix from the vinyl polysiloxane of macromolecule, can also select liquid ethylene base
Polysiloxanes and hydrogen containing siloxane are matrix, through Si―H addition reaction, and crosslinking curing is simultaneously obtained after foaming.The hair of addition-type silicon rubber
Bubble method mainly has two kinds, and one kind is reduced foaming using thermal sensitivity foaming agent, and expansion ratio is big, but reaction is violent, foaming
Process is difficult to control；Another is the effect using the silicon hydrogen containing activity hydroxy and hydrogen containing siloxane in platinum group metal catalystses
Lower reaction, releases hydrogen and foams, but frothing percentage is relatively low, and the foamed silastic density of preparation is larger.
Foamed silastic needs that there is higher expansion ratio to ensure that it has good anti-impact damping performance.But compared with
High expansion ratio means relatively low density, and this necessarily causes the tear resistance of foamed silastic to decline.And existing hair
Bubble silicon rubber is often difficult to the two and taken into account.
Therefore, foamed silastic how is made on the premise of with relatively low density, also with higher tear resistance,
It is this area urgent problem to be solved.
The content of the invention
In view of the deficienciess of the prior art, it is an object of the invention to provide a kind of foamed silastic and its preparation side
Method.The foamed silastic is while relatively low density is ensured, also with higher tearing strength and hardness.
For up to this purpose, the present invention uses following technical scheme：
On the one hand, the present invention provides a kind of foamed silastic, it is characterised in that the foamed silastic includes following quality
The raw material components of number：
In the present invention, Vinyl MQ silicon resin and containing hydrogen silicone oil are the material of main parts for preparing silicon rubber, pass through addition reaction
Form silicone rubber matrix；Hydroxy silicon oil is both foaming agent, and crosslinking agent can be served as again, realizes one step foaming and the solidification of silicon rubber；
Thermosensitive type foaming agent makes silicon rubber second time of foaming.Above-mentioned each component cooperates under specific ratio, so that obtained hair
Bubble silicon rubber has relatively low density and higher tearing strength and hardness simultaneously.
In the present invention, the mass fraction of the Vinyl MQ silicon resin can be 30 parts, 32 parts, 34 parts, 35 parts, 36 parts,
38 parts, 40 parts, 42 parts, 44 parts, 45 parts, 46 parts, 48 parts, 50 parts, 52 parts, 54 parts, 55 parts, 56 parts, 58 parts or 60 parts etc..
The mass fraction of the containing hydrogen silicone oil can be 40 parts, 42 parts, 44 parts, 45 parts, 46 parts, 48 parts, 50 parts, 52 parts,
54 parts, 55 parts, 56 parts, 58 parts, 60 parts, 62 parts, 64 parts, 65 parts, 66 parts, 68 parts or 70 parts etc..
The mass fraction of the hydroxy silicon oil can be 2 parts, 3 parts, 4 parts, 5 parts, 6 parts, 7 parts, 8 parts, 9 parts, 10 parts, 11
Part, 12 parts, 13 parts, 14 parts or 15 parts etc..
The mass fraction of the filler can be 20 parts, 22 parts, 24 parts, 25 parts, 26 parts, 28 parts, 30 parts, 32 parts, 34 parts,
35 parts, 36 parts, 38 parts, 40 parts, 42 parts, 44 parts, 45 parts, 46 parts, 48 parts or 50 parts etc..
The mass fraction of the thermosensitive type foaming agent can be 0.05 part, 0.08 part, 0.1 part, 0.12 part, 0.15 part,
0.18 part, 0.2 part, 0.22 part, 0.25 part, 0.28 part, 0.3 part, 0.32 part, 0.35 part, 0.38 part, 0.4 part, 0.42 part,
0.45 part, 0.48 part or 0.5 part etc..
The mass fraction of the catalyst can be 0.02 part, 0.03 part, 0.04 part, 0.05 part, 0.06 part, 0.07 part,
0.08 part, 0.09 part, 0.1 part, 0.11 part, 0.12 part, 0.13 part, 0.14 part or 0.15 part etc..
Preferably, the foamed silastic includes the raw material components of following mass fraction：
Preferably, the number-average molecular weight of the Vinyl MQ silicon resin is 3000-10000；For example can be 3000,
3500th, 4000,4500,5000,5500,6000,6500,7000,7500,8000,8500,9000,9500 or 10000 etc..
Preferably, the content of the Vinyl MQ silicon resin medium vinyl is 0.05-1wt%；For example can be
0.05wt%, 0.1wt%, 0.15wt%, 0.2wt%, 0.25wt%, 0.3wt%, 0.35wt%, 0.4wt%, 0.45wt%,
0.5wt%, 0.55wt%, 0.6wt%, 0.65wt%, 0.7wt%, 0.75wt%, 0.8wt%, 0.85wt%, 0.9wt% or
1wt% etc..
Preferably, the mol ratio of M units and Q unit is 0.6-1.2 in the Vinyl MQ silicon resin；For example can be
0.6th, 0.7,0.8,0.9,1,1.1 or 1.2 etc..
Q unit in Vinyl MQ silicon resin is tetra functional siloxane unit, is the knot of polysiloxane molecule chain connection
Point, the content that Q unit in Vinyl MQ silicon resin is improved within the specific limits is favorably improved the tearing strength of foamed silastic.
During the too high levels of Q unit, Vinyl MQ silicon resin is powder, it is not easy to scattered.
Preferably, the number-average molecular weight of the containing hydrogen silicone oil is 4000-8000；For example can be 4000,4500,5000,
5500th, 6000,6500,7000,7500,8000,8500,9000,9500 or 10000 etc..
Preferably, hydrogen atom (silicon hydrogen) content being directly connected in the containing hydrogen silicone oil with silicon is 0.5-1.5wt%；For example
Can be 0.5wt%, 0.6wt%, 0.7wt%, 0.8wt%, 0.9wt%, 1wt%, 1.1wt%, 1.2wt%, 1.3wt%,
1.4wt% or 1.5wt% etc..
The silicon hydrogen of containing hydrogen silicone oil is active hydrogen, in the presence of platinum group metal catalystses, can occur addition with vinyl
Reaction, forms silicone rubber matrix, also can release hydrogen with active hydroxyl groups reaction.Point of containing hydrogen silicone oil and Vinyl MQ silicon resin
When son amount is excessive, the viscosity for being easily caused system is excessive, is unfavorable for the dispersed of other raw materials；When the two molecular weight is too small,
The viscosity of system is too small, and press foaming pressure is difficult in one step foaming, is easily caused bubbles burst, forms perforate.
Preferably, the hydroxy radical content of the hydroxy silicon oil is 5-10wt%；For example can be 5wt%, 5.5wt%,
6wt%, 6.5wt%, 7wt%, 7.5wt%, 8wt%, 8.5wt%, 9wt%, 9.5wt% or 10wt% etc..
Preferably, the number-average molecular weight of the hydroxy silicon oil is 500-1000；For example can be 500,550,600,650,
700th, 750,800,850,900,950 or 1000 etc..
Hydroxy silicon oil, while crosslinking silicone rubber matrix, is improved by making silicon rubber foam with containing hydrogen silicone oil reaction
The tearing strength of foamed silastic.The molecular weight of hydroxy silicon oil should be in suitable scope, and the activity of its hydroxyl is with hydroxyl silicon
The increase of oil molecule amount and reduce.
Preferably, the filler is white carbon.
Preferably, the specific surface area of the white carbon is 100-250m2/g；For example can be 100m2/g、120m2/g、
140m2/g、150m2/g、160m2/g、180m2/g、200m2/g、220m2/g、240m2/ g or 250m2/ g etc..
Preferably, the white carbon is aerosil and/or precipitated silica.
Preferably, the thermosensitive type foaming agent is selected from azodicarbonamide (AC thermosensitive type foaming agents, decomposition temperature 205
DEG C), azodiisobutyronitrile (AIBN, 102 DEG C of decomposition temperature), dinitrosopentamethylene tetramine (DPT, 203 DEG C of decomposition temperature)
Or one kind or at least two in N, N'- dimethyl-N, N'- dinitrosoterephthalamine (NTA, 105 DEG C of decomposition temperature)
Combination；For example can be AC thermosensitive types foaming agent and AIBN combination, the combination of AC thermosensitive types foaming agent and DPT, AC temperature-sensitives
Type foaming agent and NTA combination, AIBN and DPT combination or DPT and NTA combination etc..
Preferably, the catalyst is platinum series metal complex catalyst.
Preferably, the content of active ingredient is 3000-5000ppm in the platinum series metal complex catalyst；For example may be used
To be 3000ppm, 3500ppm, 4000ppm, 4500ppm or 5000ppm etc..
On the other hand, the present invention provides a kind of preparation method of above-mentioned foamed silastic, comprises the following steps：
(1) each component in addition to catalyst is mixed by formula ratio；
(2) mixed material for obtaining the catalyst of formula ratio and step (1), which is stirred, mixes, and carries out one step foaming solidification,
Obtain semi-finished product；
(3) second time of foaming solidification is carried out to the semi-finished product, obtains the foamed silastic.
The present invention is solidified by one step foaming, forms the silicone rubber matrix with some strength and larger cell, then in height
Decompose micro thermosensitive type foaming agent under temperature, less abscess is formed, while making the full cross-linked solidification of silicone rubber matrix.Vesicle
The diameter in hole is much smaller than big abscess, will not destroy the continuity of silicone rubber matrix, therefore foamed silastic remains to keep higher
Tearing strength, density is but substantially reduced.
Preferably, mixing described in step (1) is carried out in high-speed mixer.
Preferably, the stir speed (S.S.) of the high-speed mixer be 300-500r/min, for example can be 300r/min,
320r/min, 350r/min, 380r/min, 400r/min, 420r/min, 450r/min, 480r/min or 500r/min etc.；Stir
The time is mixed for 5-10min, such as can be 5min, 6min, 7min, 8min, 9min or 10min.
Preferably, the speed stirred described in step (2) is 100-200r/min, for example, can be 100r/min, 110r/
Min, 120r/min, 130r/min, 140r/min, 150r/min, 160r/min, 170r/min, 180r/min, 190r/min or
200r/min etc.；The time of stirring is 10-30s, for example, can be 10s, 12s, 15s, 18s, 20s, 22s, 25s, 28s or 30s
Deng.
Preferably, the temperature of the one step foaming solidification is 20-30 DEG C；For example can be 20 DEG C, 21 DEG C, 22 DEG C, 23 DEG C,
24 DEG C, 25 DEG C, 26 DEG C, 27 DEG C, 28 DEG C, 29 DEG C or 30 DEG C etc..
Preferably, the time of the one step foaming solidification is 10-20min；For example can be 10min, 11min, 12min,
13min, 14min, 15min, 16min, 17min, 18min, 19min or 20min etc..
Preferably, the temperature of the second time of foaming solidification is higher than 10-30 DEG C of the decomposition temperature of the thermosensitive type foaming agent；Example
It such as can be 10 DEG C, 12 DEG C, 15 DEG C, 18 DEG C, 20 DEG C, 22 DEG C, 25 DEG C, 28 DEG C or 30 DEG C.
Preferably, the time of the second time of foaming solidification is 30-60min；For example can be 30min, 32min, 35min,
38min, 40min, 42min, 45min, 48min, 50min, 52min, 55min, 58min or 60min etc..
Preferably, the preparation method comprises the following steps：
(1) each component in addition to catalyst is added in high-speed mixer by formula ratio, in stirring for 300-500r/min
Mix and mix 5-10min under speed；
(2) mixed material for obtaining the catalyst of formula ratio and step (1) is under 100-200r/min stir speed (S.S.)
10-30s is mixed, in 20-30 DEG C of foamed solidification 10-20min next time, semi-finished product are obtained；
(3) by the semi-finished product under conditions of 10-30 DEG C of the decomposition temperature higher than the thermosensitive type foaming agent secondary hair
Bubble solidification 30-60min, obtains the foamed silastic.
Compared with prior art, the invention has the advantages that：
In the present invention, Vinyl MQ silicon resin and containing hydrogen silicone oil are the material of main parts for preparing silicon rubber, pass through addition reaction
Form silicone rubber matrix；Hydroxy silicon oil is both foaming agent, and crosslinking agent can be served as again, realizes one step foaming and the solidification of silicon rubber；
Thermosensitive type foaming agent makes silicon rubber second time of foaming.Above-mentioned each component cooperates under specific ratio, so that obtained hair
Bubble silicon rubber has relatively low density and higher tearing strength and hardness simultaneously.
The density for the foamed silastic that the present invention is provided is 0.17-0.26g/cm3, tearing strength is 58-70kN/m, hardness
(shore A) is 12-25.
Carry out preferably, resulting in the more preferable foamed silastic of combination property, its density is by the consumption to each component
0.19-0.22g/cm3, tearing strength is 65-70kN/m, and hardness (shore A) is 19-25.
Embodiment
Technical scheme is further illustrated below by specific embodiment.Those skilled in the art should be bright
, the embodiment be only to aid in understand the present invention, be not construed as to the present invention concrete restriction.
Embodiment 1
A kind of foamed silastic, includes the raw material components of following mass fraction：
Wherein the number-average molecular weight of Vinyl MQ silicon resin is 3000, and the content of vinyl is 1wt%, M units and Q unit
Mol ratio be 1.2；The number-average molecular weight of containing hydrogen silicone oil is 10000, and the hydrogen atom content being directly connected with silicon is 0.5wt%；
The number-average molecular weight of hydroxy silicon oil is 1000, and hydroxy radical content is 5wt%；The specific surface area of aerosil is 100m2/g。
The preparation method of above-mentioned foamed silastic comprises the following steps：
(1) each component in addition to catalyst is added in high-speed mixer by formula ratio, in 300r/min stirring speed
10min is mixed under rate；
(2) mixed material for obtaining the catalyst of formula ratio and step (1) is mixed under 100r/min stir speed (S.S.)
30s, in 20 DEG C of foamed solidification 20min next time, obtains semi-finished product；
(3) by above-mentioned semi-finished product, second time of foaming solidifies 30min at 215 DEG C, obtains above-mentioned foamed silastic.
Embodiment 2
A kind of foamed silastic, includes the raw material components of following mass fraction：
Wherein the number-average molecular weight of Vinyl MQ silicon resin is 10000, and the content of vinyl is 0.05wt%, M units and Q
The mol ratio of unit is 1.2；The number-average molecular weight of containing hydrogen silicone oil is 4000, and the hydrogen atom content being directly connected with silicon is
1.5wt%；The number-average molecular weight of hydroxy silicon oil is 500, and hydroxy radical content is 10wt%；The specific surface area of aerosil is
250m2/g。
The preparation method of above-mentioned foamed silastic comprises the following steps：
(1) each component in addition to catalyst is added in high-speed mixer by formula ratio, in 500r/min stirring speed
5min is mixed under rate；
(2) mixed material for obtaining the catalyst of formula ratio and step (1) is mixed under 200r/min stir speed (S.S.)
10s, in 30 DEG C of foamed solidification 10min next time, obtains semi-finished product；
(3) the lower second time of foaming by above-mentioned semi-finished product at 132 DEG C solidifies 60min, obtains above-mentioned foamed silastic.
Embodiment 3
A kind of foamed silastic, includes the raw material components of following mass fraction：
Wherein the number-average molecular weight of Vinyl MQ silicon resin is 8000, and the content of vinyl is 0.2wt%, and M units and Q are mono-
The mol ratio of member is 1；The number-average molecular weight of containing hydrogen silicone oil is 6000, and the hydrogen atom content being directly connected with silicon is 1.2wt%；Hydroxyl
The number-average molecular weight of base silicone oil is 600, and hydroxy radical content is 8wt%；The specific surface area of precipitated silica is 150m2/g。
The preparation method of above-mentioned foamed silastic comprises the following steps：
(1) each component in addition to catalyst is added in high-speed mixer by formula ratio, in 400r/min stirring speed
8min is mixed under rate；
(2) mixed material for obtaining the catalyst of formula ratio and step (1) is mixed under 150r/min stir speed (S.S.)
20s, in 25 DEG C of foamed solidification 15min next time, obtains semi-finished product；
(3) by above-mentioned semi-finished product, second time of foaming solidifies 40min at 125 DEG C, obtains above-mentioned foamed silastic.
Embodiment 4
A kind of foamed silastic, includes the raw material components of following mass fraction：
Wherein the number-average molecular weight of Vinyl MQ silicon resin is 5000, and the content of vinyl is 0.8wt%, and M units and Q are mono-
The mol ratio of member is 0.8；The number-average molecular weight of containing hydrogen silicone oil is 8500, and the hydrogen atom content being directly connected with silicon is 1wt%；Hydroxyl
The number-average molecular weight of base silicone oil is 700, and hydroxy radical content is 6wt%；The specific surface area of aerosil is 200m2/g。
The preparation method of above-mentioned foamed silastic comprises the following steps：
(1) each component in addition to catalyst is added in high-speed mixer by formula ratio, in 450r/min stirring speed
6min is mixed under rate；
(2) mixed material for obtaining the catalyst of formula ratio and step (1) is mixed under 180r/min stir speed (S.S.)
15s, in 25 DEG C of foamed solidification 12min next time, obtains semi-finished product；
(3) by above-mentioned semi-finished product, second time of foaming solidifies 50min at 220 DEG C, obtains above-mentioned foamed silastic.
Embodiment 5
A kind of foamed silastic, includes the raw material components of following mass fraction：
Wherein the number-average molecular weight of Vinyl MQ silicon resin is 5000, and the content of vinyl is 0.8wt%, and M units and Q are mono-
The mol ratio of member is 1；The number-average molecular weight of containing hydrogen silicone oil is 8500, and the hydrogen atom content being directly connected with silicon is 1wt%；Hydroxyl
The number-average molecular weight of silicone oil is 600, and hydroxy radical content is 8wt%；The specific surface area of aerosil is 200m2/g。
The preparation method of above-mentioned foamed silastic comprises the following steps：
(1) each component in addition to catalyst is added in high-speed mixer by formula ratio, in 350r/min stirring speed
7min is mixed under rate；
(2) mixed material for obtaining the catalyst of formula ratio and step (1) is mixed under 120r/min stir speed (S.S.)
25s, in 25 DEG C of foamed solidification 18min next time, obtains semi-finished product；
(3) by above-mentioned semi-finished product, second time of foaming solidifies 40min at 230 DEG C, obtains above-mentioned foamed silastic.
Embodiment 6
A kind of foamed silastic, includes the raw material components of following mass fraction：
Wherein the number-average molecular weight of Vinyl MQ silicon resin is 5000, and the content of vinyl is 0.8wt%, and M units and Q are mono-
The mol ratio of member is 0.8；The number-average molecular weight of containing hydrogen silicone oil is 8500, and the hydrogen atom content being directly connected with silicon is 1wt%；Hydroxyl
The number-average molecular weight of base silicone oil is 600, and hydroxy radical content is 8wt%；The specific surface area of aerosil is 200m2/g。
The preparation method of above-mentioned foamed silastic comprises the following steps：
(1) each component in addition to catalyst is added in high-speed mixer by formula ratio, in 400r/min stirring speed
8min is mixed under rate；
(2) mixed material for obtaining the catalyst of formula ratio and step (1) is mixed under 150r/min stir speed (S.S.)
15s, in 25 DEG C of foamed solidification 15min next time, obtains semi-finished product；
(3) by above-mentioned semi-finished product, second time of foaming solidifies 45min at 130 DEG C, obtains above-mentioned foamed silastic.
Comparative example 1
Difference with embodiment 1 is that the mass fraction of Vinyl MQ silicon resin is 25 parts, the mass fraction of containing hydrogen silicone oil
For 75 parts, remaining raw material, consumption and preparation method are same as Example 1.
Comparative example 2
Difference with embodiment 2 is that the mass fraction of Vinyl MQ silicon resin is 65 parts, the mass fraction of containing hydrogen silicone oil
For 35 parts, remaining raw material, consumption and preparation method are same as Example 2.
Comparative example 3
Difference with embodiment 1 is that the mass fraction of hydroxy silicon oil is 16 parts, remaining raw material, consumption and preparation method
It is same as Example 1.
Comparative example 4
Difference with embodiment 2 is, the mass fraction of hydroxy silicon oil is 1 part, remaining raw material, consumption and preparation method with
Embodiment 2 is identical.
Comparative example 5
Difference with embodiment 1 is that the consumption of thermosensitive type foaming agent is 0, remaining raw material, consumption and preparation method and reality
Apply example 1 identical.
Comparative example 6
Difference with embodiment 2 is that the mass fraction of thermosensitive type foaming agent is 0.6 part, remaining raw material, consumption and preparation
Method is same as Example 2.
The performance data and performance test standard for the foamed silastic that above-described embodiment 1-6 and comparative example 1-6 is provided are as follows
Shown in table 1.
Table 1
| Test event | Density (g/cm3) | Tearing strength (kN/m) | Hardness (shore A) |
| Testing standard | ASTM D3574 | ASTM D1056 | ASTM D1056 |
| Embodiment 1 | 0.17 | 58 | 12 |
| Embodiment 2 | 0.26 | 61 | 16 |
| Embodiment 3 | 0.25 | 63 | 15 |
| Embodiment 4 | 0.19 | 65 | 19 |
| Embodiment 5 | 0.22 | 67 | 20 |
| Embodiment 6 | 0.2 | 70 | 23 |
| Comparative example 1 | 0.16 | 47 | 5 |
| Comparative example 2 | 0.31 | 53 | 9 |
| Comparative example 3 | 0.16 | 54 | 11 |
| Comparative example 4 | 0.4 | 58 | 18 |
| Comparative example 5 | 0.37 | 60 | 17 |
| Comparative example 6 | 0.18 | 50 | 7 |
From the performance data of table 1, when the consumption of Vinyl MQ silicon resin is very few, when the consumption of containing hydrogen silicone oil is excessive
(comparative example 1), is fully carried out, cross-linking reaction is incomplete, therefore the density of foamed silastic does not have due to foaming twice
Substantially reduction, tearing strength and hardness decline to a great extent on the contrary, lose practical value；When the consumption of Vinyl MQ silicon resin is excessive,
When the consumption of containing hydrogen silicone oil is very few (comparative example 2), because one step foaming and crosslinking are insufficient, therefore obtained foamed silastic
Density it is larger, tearing strength and hardness have also declined；(comparative example 3), small-molecular-weight when the consumption of hydroxy silicon oil is excessive
Hydroxy silicon oil it is superfluous, can not further reduce the density of foamed silastic, instead result in its overall intensity and decline；Work as hydroxyl
When the consumption of base silicone oil is very few (comparative example 4), foaming and crosslinking are insufficient, and causing the density of foamed silastic increases, tear
Intensity declines on the contrary；When without thermosensitive type foaming agent (comparative example 5), although the tearing strength and hardness of foamed silastic
Lifted, but density is also significantly increased；When the consumption of thermosensitive type foaming agent is excessive (comparative example 6), although foamed silastic enters one
The stomata that the stomata that step foaming, density reduction, but second time of foaming are produced easily is produced with one step foaming is connected, and reduces silicon rubber base
The continuity of body simultaneously forms perforate, causes the tearing strength and hardness of foamed silastic to decline to a great extent.Only when the use of each component
When amount is in the framework of the present definition, it can just obtain having concurrently the foamed silastic of low-density, high-tear strength and high rigidity.
Applicant states, the foregoing is only the embodiment of the present invention, but protection scope of the present invention not office
It is limited to this, person of ordinary skill in the field is it will be clearly understood that any belong to those skilled in the art and taken off in the present invention
In the technical scope of dew, the change or replacement that can be readily occurred in, within the scope of all falling within protection scope of the present invention and being open.
Claims (10)
1. a kind of foamed silastic, it is characterised in that the foamed silastic includes the raw material components of following mass fraction：
2. foamed silastic according to claim 1, it is characterised in that the foamed silastic includes following mass fraction
Raw material components：
3. foamed silastic according to claim 1 or 2, it is characterised in that the number of the Vinyl MQ silicon resin is divided equally
Son amount is 3000-10000；
Preferably, the content of the Vinyl MQ silicon resin medium vinyl is 0.05-1wt%；
Preferably, the mol ratio of M units and Q unit is 0.6-1.2 in the Vinyl MQ silicon resin.
4. the foamed silastic according to claim any one of 1-3, it is characterised in that the equal molecule of number of the containing hydrogen silicone oil
Measure as 4000-10000；
Preferably, the hydrogen atom content being directly connected in the containing hydrogen silicone oil with silicon is 0.5-1.5wt%；
Preferably, the hydroxy radical content of the hydroxy silicon oil is 5-10wt%；
Preferably, the number-average molecular weight of the hydroxy silicon oil is 500-1000.
5. the foamed silastic according to claim any one of 1-4, it is characterised in that the filler is white carbon；
Preferably, the specific surface area of the white carbon is 100-250m2/g；
Preferably, the white carbon is aerosil and/or precipitated silica.
6. the foamed silastic according to claim any one of 1-5, it is characterised in that the thermosensitive type foaming agent is selected from even
Nitrogen diformamide, azodiisobutyronitrile, dinitrosopentamethylene tetramine or N, N'- dimethyl-N, N'- dinitroso are to benzene two
One kind or at least two combination in formamide.
7. the foamed silastic according to claim any one of 1-6, it is characterised in that the catalyst is platinum metal network
Mixture catalyst；
Preferably, the content of active ingredient is 3000-5000ppm in the platinum series metal complex catalyst.
8. the preparation method of the foamed silastic according to claim any one of 1-7, it is characterised in that the preparation method
Comprise the following steps：
(1) each component in addition to catalyst is mixed by formula ratio；
(2) mixed material for obtaining the catalyst of formula ratio and step (1), which is stirred, mixes, and carries out one step foaming solidification, obtains
Semi-finished product；
(3) second time of foaming solidification is carried out to the semi-finished product, obtains the foamed silastic.
9. preparation method according to claim 8, it is characterised in that mixing is in high-speed mixer described in step (1)
It is middle to carry out；
Preferably, the stir speed (S.S.) of the high-speed mixer is 300-500r/min, and mixing time is 5-10min；
Preferably, the speed stirred described in step (2) is 100-200r/min, and the time of stirring is 10-30s；
Preferably, the temperature of the one step foaming solidification is 20-30 DEG C；
Preferably, the time of the one step foaming solidification is 10-20min；
Preferably, the temperature of the second time of foaming solidification is higher than 10-30 DEG C of the decomposition temperature of the thermosensitive type foaming agent；
Preferably, the time of the second time of foaming solidification is 30-60min.
10. preparation method according to claim 8 or claim 9, it is characterised in that the preparation method comprises the following steps：
(1) each component in addition to catalyst is added in high-speed mixer by formula ratio, in 300-500r/min stirring speed
5-10min is mixed under rate；
(2) mixed material for obtaining the catalyst of formula ratio and step (1) is mixed under 100-200r/min stir speed (S.S.)
10-30s, in 20-30 DEG C of foamed solidification 10-20min next time, obtains semi-finished product；
(3) by the semi-finished product, second time of foaming is consolidated under conditions of 10-30 DEG C of the decomposition temperature higher than the thermosensitive type foaming agent
Change 30-60min, obtain the foamed silastic.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109161205A (en) * | 2018-09-04 | 2019-01-08 | 杭州之江新材料有限公司 | A kind of flame-retardant expanded silicon rubber and preparation method thereof |
| CN110396295A (en) * | 2019-08-02 | 2019-11-01 | 北京化工大学 | A kind of room temperature vulcanization organosilicon foaming sealant of high temperature resistant heat insulation and preparation method thereof |
| CN110698713A (en) * | 2019-10-08 | 2020-01-17 | 浙江杰上杰新材料有限公司 | High-dispersity silica gel foaming agent and preparation method thereof |
| CN113214652A (en) * | 2021-06-28 | 2021-08-06 | 东莞市兆科电子材料科技有限公司 | Foaming silica gel and preparation method and application thereof |
| CN115894927A (en) * | 2022-12-07 | 2023-04-04 | 西安近代化学研究所 | Thermal insulation material of foaming organic silicon gel and preparation method |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1016442A2 (en) * | 1998-12-31 | 2000-07-05 | Dow Corning Corporation | Antifoam compositions containing ultra high molecular weight resins |
| CN101280112A (en) * | 2008-05-16 | 2008-10-08 | 卢儒 | Foamed silastic |
| CN102746674A (en) * | 2012-07-31 | 2012-10-24 | 西安科技大学 | High heat-resistant porous organic silicon alloy elastomer material and method for preparing same |
| CN103992649A (en) * | 2014-03-27 | 2014-08-20 | 江阴海达橡塑股份有限公司 | Long service life silicon rubber sponge for environmental protection fire retardation vibration reduction sealing, and preparation method thereof |
| CN105238061A (en) * | 2015-11-25 | 2016-01-13 | 泸州北方化学工业有限公司 | Foaming silicone rubber compound, low-density silicone rubber sponge and preparing method of low-density silicone rubber sponge |
-
2017
- 2017-05-17 CN CN201710346686.3A patent/CN106977724B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1016442A2 (en) * | 1998-12-31 | 2000-07-05 | Dow Corning Corporation | Antifoam compositions containing ultra high molecular weight resins |
| CN101280112A (en) * | 2008-05-16 | 2008-10-08 | 卢儒 | Foamed silastic |
| CN102746674A (en) * | 2012-07-31 | 2012-10-24 | 西安科技大学 | High heat-resistant porous organic silicon alloy elastomer material and method for preparing same |
| CN103992649A (en) * | 2014-03-27 | 2014-08-20 | 江阴海达橡塑股份有限公司 | Long service life silicon rubber sponge for environmental protection fire retardation vibration reduction sealing, and preparation method thereof |
| CN105238061A (en) * | 2015-11-25 | 2016-01-13 | 泸州北方化学工业有限公司 | Foaming silicone rubber compound, low-density silicone rubber sponge and preparing method of low-density silicone rubber sponge |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109161205A (en) * | 2018-09-04 | 2019-01-08 | 杭州之江新材料有限公司 | A kind of flame-retardant expanded silicon rubber and preparation method thereof |
| CN110396295A (en) * | 2019-08-02 | 2019-11-01 | 北京化工大学 | A kind of room temperature vulcanization organosilicon foaming sealant of high temperature resistant heat insulation and preparation method thereof |
| CN110698713A (en) * | 2019-10-08 | 2020-01-17 | 浙江杰上杰新材料有限公司 | High-dispersity silica gel foaming agent and preparation method thereof |
| CN110698713B (en) * | 2019-10-08 | 2022-05-13 | 浙江杰上杰新材料有限公司 | High-dispersity silica gel foaming agent and preparation method thereof |
| CN113214652A (en) * | 2021-06-28 | 2021-08-06 | 东莞市兆科电子材料科技有限公司 | Foaming silica gel and preparation method and application thereof |
| CN115894927A (en) * | 2022-12-07 | 2023-04-04 | 西安近代化学研究所 | Thermal insulation material of foaming organic silicon gel and preparation method |
| CN115894927B (en) * | 2022-12-07 | 2024-05-28 | 西安近代化学研究所 | Heat insulation material of foaming organic silicon gel and preparation method thereof |
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