The content of the invention
In view of the shortcomings of the prior art, it is special it is an object of the invention to provide a kind of fire-proof potting compound and preparation method thereof
It is not to provide a kind of low viscosity fire-proof potting compound and preparation method thereof.
To reach this goal of the invention, the present invention uses following technical scheme:
On the one hand, the present invention provides a kind of fire-proof potting compound, and the fire-proof potting compound is mainly made up of A agent and B agent, described
A agent is mainly made up of the component of following parts by weight:
The B agent is mainly made up of the component of following parts by weight:
Fire-proof potting compound of the present invention has good anti-flammability, and viscosity is low, possesses preferable levelability when in use,
And contribute to the discharge of bubble.
Preferably, the mass ratio of the A agent and B agent is 5~6:1, such as 5:1、5.1:1、5.2:1、5.3:1、5.4:1、
5.5:1、5.6:1、5.7:1、5.8:1、5.9:1 or 6:1.
In the present invention, the dosage of base rubber is 5~7 parts by weight in A agent, such as 5 parts by weight, 5.2 parts by weight, 5.4 weight
Part, 5.6 parts by weight, 5.8 parts by weight, 6.0 parts by weight, 6.2 parts by weight, 6.4 parts by weight, 6.5 parts by weight, 6.7 parts by weight, 6.9
Parts by weight or 7 parts by weight.
Preferably, the base rubber is 107 glue;
Preferably, the viscosity of 107 glue is 500~1000mPas, such as 500mPas, 520mPas,
550mPa·s、580mPa·s、600mPa·s、630mPa·s、650mPa·s、680mPa·s、700mPa·s、
750mPas, 780mPas, 800mPas, 870mPas, 900mPas, 950mPas or 1000mPas, preferably
750mPa·s。
By the present invention in that with 107 glue of low viscosity, the overall viscosity of A agent is greatly reduced, is then used in mixed way with B agent
During ensure its preferable levelability and low mixing viscosity, the discharge of bubble and outward appearance during so as to help to be stirred use
It is smooth.
In the present invention, the dosage of diluent is 1~3 parts by weight in A agent, such as 1 parts by weight, 1.2 parts by weight, 1.4 weights
Measure part, 1.6 parts by weight, 1.8 parts by weight, 2.0 parts by weight, 2.2 parts by weight, 2.4 parts by weight, 2.6 parts by weight, 2.8 parts by weight or 3
Parts by weight.
Preferably, diluent is silicone oil in the A agent.
In the present invention, the dosage of aluminium hydroxide is 4~5 parts by weight in A agent, such as 4 parts by weight, 4.1 parts by weight, 4.2
Parts by weight, 4.3 parts by weight, 4.4 parts by weight, 4.5 parts by weight, 4.6 parts by weight, 4.7 parts by weight, 4.8 parts by weight, 4.9 parts by weight
Or 5 parts by weight.
In the present invention, the dosage of titanium dioxide is 0.1~0.2 parts by weight in A agent, such as 0.1 parts by weight, 0.11 weight
Part, 0.12 parts by weight, 0.13 parts by weight, 0.14 parts by weight, 0.15 parts by weight, 0.16 parts by weight, 0.17 parts by weight, 0.18 weight
Part, 0.19 parts by weight or 0.2 parts by weight.
In the present invention, the dosage of TDE is 1.5~2.5 parts by weight in A agent, such as 1.5 parts by weight, 1.7
Parts by weight, 1.9 parts by weight, 2.0 parts by weight, 2.1 parts by weight, 2.2 parts by weight, 2.3 parts by weight, 2.4 parts by weight or 2.5 weight
Part.
In the present invention, the dosage of toner is 0.0006~0.0009 parts by weight in A agent, such as 0.0006 parts by weight,
0.00063 parts by weight, 0.00065 parts by weight, 0.00068 parts by weight, 0.0007 parts by weight, 0.00072 parts by weight, 0.00074
Parts by weight, 0.00076 parts by weight, 0.00078 parts by weight, 0.0008 parts by weight, 0.00083 parts by weight, 0.00085 parts by weight,
0.00088 parts by weight or 0.0009 parts by weight.
Preferably, the toner is ultramarine.
In the present invention, the dosage of curing agent is 0.004~0.008 parts by weight in A agent, such as 0.004 parts by weight,
0.0043 parts by weight, 0.0045 parts by weight, 0.0048 parts by weight, 0.005 parts by weight, 0.0052 parts by weight, 0.0054 parts by weight,
0.0056 parts by weight, 0.0058 parts by weight, 0.006 parts by weight, 0.0065 parts by weight, 0.0068 parts by weight, 0.007 parts by weight,
0.0075 parts by weight, 0.0078 parts by weight or 0.008 parts by weight.
Preferably, the curing agent is diethanol amine.
In the present invention, the anti-flammability of product can be lifted by aluminium hydroxide and TDE, the two is being improved
There is synergy, aluminium hydroxide can prevent from sending out fire-retardant while as inorganic fire-retarded additive in terms of the anti-flammability of product
Cigarette and toxic gas is not produced, and TDE can further lift the heat of product on the basis of aluminium hydroxide
Stability, ultraviolet-resistent property, and have in A developing agent storages relatively low exudative.In the present invention, the dosage of crosslinking agent is in B agent
0.5-2.5 parts by weight, such as 0.5 parts by weight, 0.7 parts by weight, 0.9 parts by weight, 1.0 parts by weight, 1.2 parts by weight, 1.4 weight
Part, 1.6 parts by weight, 18 parts by weight, 2.0 parts by weight, 2.2 parts by weight, 2.4 parts by weight or 2.5 parts by weight.
Preferably, the crosslinking agent is tetraethyl orthosilicate and/or MTMS, preferably tetraethyl orthosilicate and first
The mixture of base trimethoxy silane;
Preferably, when crosslinking agent is the mixture of tetraethyl orthosilicate and MTMS, the positive silicic acid second
The dosage of ester is 0.5-1.5 parts by weight, such as 0.5 parts by weight, 0.7 parts by weight, 0.9 parts by weight, 1.0 parts by weight, 1.2 weight
Part, 1.4 parts by weight or 1.5 parts by weight, the dosage of the MTMS is 0.5-1 parts by weight, such as 0.5 weight
Part, 0.7 parts by weight, 0.9 parts by weight or 1.0 parts by weight.
In the present invention, the dosage of diluent is 1~2 parts by weight in B agent, such as 1 parts by weight, 1.2 parts by weight, 1.4 weights
Measure part, 1.5 parts by weight, 1.6 parts by weight, 1.8 parts by weight or 2 parts by weight.
Preferably, diluent is polyethers in the B agent.
In the present invention, the dosage of coupling agent is 0.24~0.36 parts by weight in B agent, such as 0.24 parts by weight, 0.25 weight
Measure part, 0.27 parts by weight, 0.3 parts by weight, 0.32 parts by weight, 0.34 parts by weight or 0.36 parts by weight.
Preferably, the coupling agent is N- (β-aminoethyl)-gamma-aminopropyl-triethoxy-silanes and/or glycidol ether
Oxygen propyl trimethoxy silicane, preferably N- (β-aminoethyl)-gamma-aminopropyl-triethoxy-silane and glycidyl ether oxygen propyl three
The mixture of methoxy silane.
Preferably, when the coupling agent is N- (β-aminoethyl)-gamma-aminopropyl-triethoxy-silanes and glycidyl ether oxygen
During the mixture of propyl trimethoxy silicane, the dosage of N- (β-the aminoethyl)-gamma-aminopropyl-triethoxy-silane is 0.2-
0.3 parts by weight, such as 0.2 parts by weight, 0.22 parts by weight, 0.24 parts by weight, 0.26 parts by weight, 0.28 parts by weight or 0.3 weight
Part, the dosage of the glycidyl ether oxygen propyl trimethoxy silicane is 0.04~0.06 parts by weight, such as 0.04 parts by weight,
0.043 parts by weight, 0.045 parts by weight, 0.048 parts by weight, 0.05 parts by weight, 0.055 parts by weight, 0.058 parts by weight or 0.06
Parts by weight.
In the present invention, the dosage of catalyst is 0.004~0.007 parts by weight in B agent, such as 0.004 parts by weight,
0.0043 parts by weight, 0.0045 parts by weight, 0.0048 parts by weight, 0.005 parts by weight, 0.0053 parts by weight, 0.0055 parts by weight,
0.0058 parts by weight, 0.006 parts by weight, 0.0063 parts by weight, 0.0065 parts by weight, 0.0068 parts by weight or 0.007 parts by weight.
Preferably, the catalyst is dibutyl tin laurate.
As the preferred technical solution of the present invention, A agent is mainly by the component group of following parts by weight in the fire-proof potting compound
Into:
Preferably, the B agent is mainly made up of the component of following parts by weight:
On the other hand, the invention provides the preparation method of the fire-proof potting compound, the described method comprises the following steps:
(1) diluent used in base rubber and A agent is stirred under vacuum;
(2) aluminium hydroxide and titanium dioxide are added in the mixture obtained to step (1), is stirred under normal pressure;
(3) toner and curing agent are added in the mixture obtained to step (2), is stirred under vacuum condition;
(4) TDE is added in the mixture obtained to step (3), be stirred at ambient pressure, then true
It is stirred under empty condition, plastic emitting obtains A agent;
(5) A agent and B agent are mixed to get the fire-proof potting compound.
Preferably, the vacuum of step (1) described vacuum condition is -0.1~-0.09MPa, such as -0.1MPa, -
0.098MPa, -0.095MPa, -0.093MPa or -0.09MPa.
Preferably, the rotating speed of step (1) described stirring is 10~20r/min, such as 10r/min, 11r/min, 12r/
Min, 13r/min, 14r/min, 15r/min, 16r/min, 17r/min, 18r/min, 19r/min or 20r/min.
Preferably, step (1) time for being stirred is 10~15min, for example, 10min, 11min, 12min,
13min, 14min or 15min.
Preferably, the rotating speed of step (2) described stirring is 10~20r/min, such as 10r/min, 11r/min, 12r/
Min, 13r/min, 14r/min, 15r/min, 16r/min, 17r/min, 18r/min, 19r/min or 20r/min.
Preferably, step (2) time for being stirred is 20~25min, for example, 20min, 21min, 22min,
23min, 24min or 25min.
Preferably, 2~3 batches of additions of step (2) described aluminium hydroxide point, because aluminium hydroxide is fleur, once
Property add can because measure it is excessive stir it is uneven.
Preferably, the vacuum of step (3) described vacuum condition is -0.1~-0.09MPa, such as -0.1MPa, -
0.098MPa, -0.095MPa, -0.093MPa or -0.09MPa.
Preferably, the rotating speed of step (3) described stirring is 40~50r/min, such as 40r/min, 41r/min, 42r/
Min, 43r/min, 44r/min, 45r/min, 46r/min, 47r/min, 48r/min, 49r/min or 50r/min.
Preferably, step (3) time for being stirred is 15~20min, for example, 15min, 16min, 17min,
18min, 19min or 20min.
Preferably, the speed of agitator being stirred under step (4) described normal pressure is 10~20r/min, such as 10r/min,
11r/min, 12r/min, 13r/min, 14r/min, 15r/min, 16r/min, 17r/min, 18r/min, 19r/min or 20r/
min。
Preferably, the time being stirred under step (4) described normal pressure is 5~10min, such as 5min, 5.5min,
6min, 6.5min, 7min, 7.5min, 8min, 8.5min, 9min, 9.5min or 10min.
Preferably, the vacuum of step (4) described vacuum condition is -0.1~-0.09MPa, such as -0.1MPa, -
0.098MPa, -0.095MPa, -0.093MPa or -0.09MPa.
Preferably, step (4) speed of agitator being stirred under vacuum is 45~50r/min, such as
40r/min、41r/min、42r/min、43r/min、44r/min、45r/min、46r/min、47r/min、48r/min、49r/
Min or 50r/min.
Preferably, step (4) time for being stirred under vacuum is 10~15min, such as 10min,
11min, 12min, 13min, 14min or 15min.
In the step (4) of the present invention, atmospheric agitation and the time sum being stirred under vacuum need to be strict controlled in 15~
25min, such as 15min, 17min, 19min, 20min, 22min, 24min or 25min, the time, too low material stirring was uneven, when
Between it is long storeroom can be made to produce excessive intermolecular force, so as to cause product viscosity too high.
As the preferred technical solution of the present invention, the preparation method of the fire-proof potting compound specifically includes following steps:
(1) by the glue of diluent 107 used in base rubber and A agent and silicone oil in the vacuum condition that vacuum is -0.1~-0.09MPa
Under, it is stirred 10~15min under 10~20r/min speed of agitator;
(2) aluminium hydroxide and titanium dioxide are added in the mixture obtained to step (1), in 10~20r/min's under normal pressure
20~25min is stirred under speed of agitator;
(3) ultramarine toner and curing agent are added in the mixture obtained to step (2), vacuum be -0.1~-
Under 0.09MPa vacuum condition, 15~20min is stirred under 40~50r/min speed of agitator;
(4) TDE is added in the mixture obtained to step (3), at ambient pressure stirring in 10~20r/min
5~10min is stirred under mix rotating speed, then in the case where vacuum is -0.1~-0.09MPa vacuum condition, in 45~50r/
10~15min is stirred under min speed of agitator, plastic emitting obtains A agent;
(5) A agent and B agent are mixed to get the fire-proof potting compound.
The present invention is by using above-mentioned preparation method and controls the vacuum and mixing time of each step so that is prepared into
To two-component casting glue there is more preferable anti-flammability in component operation, while mix viscosity by reducing, have when in use
Standby preferable levelability, and contribute to the discharge of bubble, and the preparation method of the present invention is simply easily achieved, suitable for industrialization
Production.
Relative to prior art, the invention has the advantages that:
Aluminium hydroxide and TDE have synergy, hydroxide for lifting product anti-flammability in the present invention
Aluminium can prevent smoke fire-retardant while and not produce toxic gas, TDE is in hydrogen as inorganic fire-retarded additive
The heat endurance and ultraviolet-resistent property of product can also be further lifted on the basis of aluminum oxide, and is had in A developing agent storages relatively low
It is exudative.Simultaneously by the present invention in that with the base rubber of low viscosity, the overall viscosity of A agent is greatly reduced, is then coordinated with B agent
It can ensure that product has preferable levelability and low mixing viscosity during use, gas during so as to help to be stirred use
The discharge of bubble and outward appearance it is smooth, there is good synthesis by the cooperation fire-proof potting compound of each component raw material in the present invention
Performance, and its preparation method is simply easily achieved, suitable for industrialized production.
Embodiment 5
In the present embodiment, fire-proof potting compound is by below by A agent and B agent with mass ratio 5.3:1 composition, the A agent are main
It is made up of the component of following parts by weight:
The B agent is mainly made up of the component of following parts by weight:
Preparation method is as follows:
(1) by 107 glue that viscosity is 950mPas and silicone oil in the case where vacuum is -0.1MPa vacuum condition, in 10r/
10min is stirred under min speed of agitator;
(2) aluminium hydroxide and titanium dioxide are added in the mixture obtained to step (1), in 10r/min stirring under normal pressure
20min is stirred under rotating speed;
(3) ultramarine and curing agent are added in the mixture obtained to step (2), in the vacuum bar that vacuum is -0.1MPa
Under part, 20min is stirred under 50r/min speed of agitator;
(4) TDE is added in the mixture obtained to step (3), turned at ambient pressure in 20r/min stirring
10min is stirred under speed, then in the case where vacuum is -0.1MPa vacuum condition, is stirred under 45r/min speed of agitator
12min is mixed, plastic emitting obtains A agent;
(5) A agent and B agent are mixed to get the fire-proof potting compound.
Comparative example 1
The comparative example difference from Example 1 is that the A agent is made up of following raw material:
Raw material composition is same as Example 1 in B agent, and preparation method is as follows:
(1) 107 glue and silicone oil are stirred in the case where vacuum is -0.1MPa vacuum condition under 20r/min speed of agitator
Mix mixing 10min;
(2) calcium carbonate and titanium dioxide are added in the mixture obtained to step (1), the stirring under normal pressure in 20r/min turns
15min is stirred under speed;
(3) ultramarine and curing agent are added in the mixture obtained to step (2), in the vacuum bar that vacuum is -0.1MPa
Under part, 20min is stirred under 40r/min speed of agitator;
(4) mixture that step (3) obtains is stirred 5min under 15r/min speed of agitator at ambient pressure, and
Afterwards in the case where vacuum is -0.1MPa vacuum condition, 10min is stirred under 45r/min speed of agitator, plastic emitting obtains A
Agent;
(5) A agent and B agent are mixed to get the fire-proof potting compound.
Comparative example 2
The comparative example difference from Example 1 is without using aluminium hydroxide and TDE, remaining is former in A agent
Material and raw material dosage are same as Example 1, and preparation method is as follows:
(1) by 107 glue that viscosity is 750mPas and silicone oil in the case where vacuum is -0.09MPa vacuum condition, in
13min is stirred under 15r/min speed of agitator;
(2) titanium dioxide is added in the mixture obtained to step (1), is stirred under normal pressure under 10r/min speed of agitator
Mix 20min;
(3) ultramarine and curing agent are added in the mixture obtained to step (2), in the vacuum bar that vacuum is -0.09MPa
Under part, 15min is stirred under 50r/min speed of agitator;
(4) mixture that step (3) obtains is stirred 5min under 15r/min speed of agitator at ambient pressure, and
Afterwards in the case where vacuum is -0.1MPa vacuum condition, 10min is stirred under 45r/min speed of agitator, plastic emitting obtains A
Agent;
(5) A agent and B agent are mixed to get the fire-proof potting compound.
Comparative example 3
The comparative example difference from Example 1 is being without using TDE, the dosage of aluminium hydroxide in A agent
6.5 parts by weight, remaining raw material and raw material dosage and the mass ratio of A agent and B agent are same as Example 1, and preparation method is the same as right
Ratio 2.
Comparative example 4
The comparative example difference from Example 1 is being without using aluminium hydroxide, the dosage of TDE in A agent
6.5 parts by weight, remaining raw material and raw material dosage and the mass ratio of A agent and B agent are same as Example 1, and preparation method is the same as right
Ratio 2.
Comparative example 5
The dosage of aluminium hydroxide is 3.8 parts by weight, remaining raw material and raw material components in the comparative example, A agent and B agent
Mass ratio and preparation method and condition are same as Example 1.
Comparative example 6
The dosage of aluminium hydroxide is 5.2 parts by weight, remaining raw material and raw material components in the comparative example, A agent and B agent
Mass ratio and preparation method and condition are same as Example 1.
Comparative example 7
TDE dosage is 1.3 parts by weight, remaining raw material and raw material components in the comparative example, A agent and B agent
Mass ratio and preparation method and condition it is same as Example 1.
Comparative example 8
TDE dosage is 2.8 parts by weight, remaining raw material and raw material components in the comparative example, A agent and B agent
Mass ratio and preparation method and condition it is same as Example 1.
Comparative example 9
107 glue dosages are the quality of 4.8 parts by weight, remaining raw material and raw material components, A agent and B agent in the comparative example
Than and preparation method and condition it is same as Example 1.
Comparative example 10
Silicon oil dosage is the mass ratio of 0.8 parts by weight, remaining raw material and raw material components, A agent and B agent in the comparative example
And preparation method and condition it is same as Example 1.
Comparative example 11
Titanium dioxide dosage is the matter of 0.05 parts by weight, remaining raw material and raw material components, A agent and B agent in the comparative example
Amount than and preparation method and condition it is same as Example 1.
Comparative example 12
Ultramarine dosage is the quality of 0.001 parts by weight, remaining raw material and raw material components, A agent and B agent in the comparative example
Than and preparation method and condition it is same as Example 1.
The fire resistance of embodiment 1-5 and comparative example 1-12 casting glue is determined, is characterized with its burning time, each
Embodiment or comparative example take 5 parallel samples to be tested, and the results are shown in Table 1.
Table 1
The burning time for the fire-proof potting compound that embodiment 1-5 is prepared is well below right it can be seen from the result of table 1
The burning time of ratio 1-12 casting glue, illustrating the fire-proof potting compound of the present invention has good fire resistance.When using normal
Advise (comparative example 1) when casting glue component prepares A agent, the burning time of its casting glue being prepared is longer, and with the phase of embodiment 1
Than same without using (comparative example 2) when aluminium hydroxide and TDE, the burning time of its obtained casting glue in A agent
It is longer, about 50s or so, when using aluminium hydroxide in A agent, and without using (comparative example 3) during TDE, even if by hydrogen
The dosage of aluminum oxide improves, and can not equally significantly improve its fire resistance, and its burning time is 35s or so, when using ten in A agent
Bromine diphenylethane, and without using (comparative example 4) during aluminium hydroxide, even if the dosage of TDE is improved, equally can not
Its fire resistance is significantly improved, its burning time is 30s or so, in addition, (such as right when certain component is excessive or very few in A agent
Ratio 5-12), the burning time of its obtained casting glue is fixed still in 25s or so during both uses simultaneously and by dosage
(embodiment 1-5) within the scope of the present invention, now the burning time of casting glue be less than 10s, there is good flame-retardance energy.
The uvioresistant performance of embodiment 1-5 and comparative example 1-12 casting glue is determined, by the power of sample after ultraviolet irradiation
As a result as shown in table 2 the change for learning performance characterizes,.
Table 2
From table 2 it can be seen that after UV is tested, the tensile strength and elongation at break average attenuation of comparative example
19.2-27.1%, and the decay of the casting glue sample of the embodiment of the present invention is only 12.7-14.2%, from data comparison, this hair
The uvioresistant performance of bright sealing also has a certain upgrade.
Measure embodiment 1 when being mixed with the A agent in comparative example 1 with B agent the viscosity of casting glue change with time situation, tie
Fruit is as shown in table 3 and Fig. 1.
Table 3
From the result of table 3 and Fig. 1, when A agent mixes with B agent, because having been used in the A agent of embodiment 1 lower viscous
The base rubber of degree, so the strand of dimethyl silicone polymer is short and more, so crosslinking reaction by linearly dividing with crosslinking agent
During son becomes adult form molecule, the viscosity that macro manifestations come out is lower, and with the change in reaction time, the increase of its viscosity
It is slower than the conventional casting glue A agent of comparative example 1, so in limited usage time, the levelability of casting glue of the invention
More preferably, bubble is easier to overflow at a low viscosity, so the bubble retained is less.
Applicant states that the present invention illustrates fire-proof potting compound of the present invention and preparation method thereof by above-described embodiment,
But the invention is not limited in above-described embodiment, that is, does not mean that the present invention has to rely on above-described embodiment and could implemented.It is affiliated
Those skilled in the art it will be clearly understood that any improvement in the present invention, equivalence replacement to raw material selected by the present invention and
The addition of auxiliary element, selection of concrete mode etc., within the scope of all falling within protection scope of the present invention and disclosing.