CN104945913A - Preparation method of solid silicon rubber composition - Google Patents
Preparation method of solid silicon rubber composition Download PDFInfo
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- CN104945913A CN104945913A CN201510363242.1A CN201510363242A CN104945913A CN 104945913 A CN104945913 A CN 104945913A CN 201510363242 A CN201510363242 A CN 201510363242A CN 104945913 A CN104945913 A CN 104945913A
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Abstract
The invention relates to a preparation method of a solid silicon rubber composition. The preparation method comprises the following steps: preparing base rubber, namely mixing methyl vinyl crude rubber, inorganic filler and a structural control agent according to a mass ratio of 100:(1-80):(1-30), performing heat treatment for 0.5-6 hours at 100-150 DEG C, and cooling to the room temperature to obtain the base rubber; preparing a material A, namely taking 100 mass parts of the base rubber, adding 0.1-10 mass parts of a catalyst and 0.01-10 mass parts of a compression deformation improver, and mixing uniformly to obtain the material A; preparing a material B, namely taking 100 mass parts of the base rubber, adding 0.01-10 mass parts of a crosslinking agent, 0.002-2 mass parts of an inhibitor and 0.1-20 mass parts of a silicon rubber stabilizer, and mixing uniformly to obtain the material B; and vulcanizing the material A and the material B for 5-20 minutes at 100-200 DEG C according to a mass ratio of 1:1, and vulcanizing for the second time to obtain the solid silicon rubber composition.
Description
Technical field
The invention belongs to field of polymer composite material, be specifically related to a kind of preparation method of firm silicone rubber composition.
Background technology
In recent years, along with global growth in the living standard, the requirement of the people to consumer goods is more and more higher, particularly more and more higher to the requirement of the security of the vehicles.The competition of Automobile Enterprises also can be more and more white-hot, and technical requirements is more and more higher, also it is also proposed higher requirement to auto parts machinery simultaneously.
Automobile spark plug, is commonly called as nozzles, and its effect is the high voltage pulse discharge of electricity that high-voltage conducting wires (nozzles line) is sent here, air between disruptive spark plug two electrode, produces the mixed gas that electrical spark ignites in cylinder with this.In high-voltage ignition coil and sparking plug junction; by hi-line, high voltage electric is being flowed in the process of sparking plug; sparking plug rubber sheath is the accessory of a protectiveness outside automobile spark plug, and it plays the effect of insulation, also can play the effect fixing and prevent dust simultaneously.Their common performance decides the performance of engine to a great extent.The operating voltage of rubber sheath up to several ten thousand volts, and will tolerate work high temperature and the severe cold in winter of engine, and bears vibration, greasy dirt etc. to the fatigue of part, the various infringement such as aging.The performance of these situations to elastomeric material proposes very high requirement.
This situation just proposes further requirement to the performance of the silicon rubber that automobile spark plug bushing uses: have higher ageing-resistant performance under (1) high temperature; (2) there is lower compression set rate; (3) there is good oil-proofness; (4) there is extraordinary flame retardant resistance; (5) there is extraordinary electric property; (6) there is very high tensile.So these six character also become the important indicator judging that automobile spark plug bushing colloidality can be good and bad.
The chemical composition that silicon rubber is special and physical structure, determine it there are other same type of material many to be difficult to replace to obtain feature, than if any very high physical strength, good heat resistance, ageing resistance is high, oil-proofness good, flame retardant resistance is high, absorption property is high, stable chemical nature etc., becomes the ideal material of automobile industry.Although the electric property of silicon rubber itself, ageing resistance, oil-proofness are all very good, permanent compression set aspect also will add special filler to realize.Have report to reduce permanent compression set, and what select is be filler with the white carbon black of the precipitator method, but the white carbon black of the precipitator method is reinforcing limited, takes into account high strength while cannot obtaining low permanent compression set.
Summary of the invention
Technical problem to be solved by this invention is the defect overcoming prior art, provides a kind of preparation method of firm silicone rubber composition.
The present invention is achieved in that a kind of preparation method of firm silicone rubber composition, and it comprises the steps:
Prepare base glue: be 100:(1 ~ 80 according to mass ratio): (1 ~ 30) is by Methyl-ethylenvinyl gum, mineral filler and antistructurizing agent mixing, thermal treatment 0.5 ~ 6 hour at 100 DEG C ~ 150 DEG C, is cooled to room temperature and obtains base glue;
The preparation of A material: the base glue getting 100 mass parts, adds the catalyzer of 0.01 ~ 10 mass parts, the compression set improving agent of 0.01 ~ 10 mass parts, evenly mixing, obtains A material;
The preparation of B material: the base glue getting 100 mass parts, then add the linking agent of 0.01 ~ 20 mass parts, the inhibitor of 0.001 ~ 2 mass parts, the silicon rubber stablizer of 0.1 ~ 20 mass parts, evenly mixing, obtain B material;
Be the sulfuration 5 ~ 20 minutes at 100 DEG C ~ 200 DEG C of the ratio of 1:1 by described A material and described B material according to mass ratio, then carry out post cure, obtain described firm silicone rubber composition.
The invention provides a kind of preparation method of firm silicone rubber composition, by rational formula and preparation condition, utilize Methyl-ethylenvinyl gum under the reinforcement of mineral filler, after introducing silicon rubber stablizer and compression set improving agent, can significantly reduce compression set performance, and it still has very high tensile strength.After composition hardening physical strength high, have that excellent ageing-resistant performance, low compression set rate, oil-proofness are good, good flame resistance.The rubber composition that this firm silicone rubber preparation method of composition obtains can be widely used in automobile spark plug bushing field, can also be applied to the oil sealing sealing pads such as automobile, locomotive, lathe and some need the silastic product of these performances.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with specific embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
The embodiment of the present invention provides a kind of preparation method of firm silicone rubber composition, and it comprises the steps:
Prepare base glue: be 100:(1 ~ 80 according to mass ratio): (1 ~ 30) is by Methyl-ethylenvinyl gum, mineral filler and antistructurizing agent mixing, thermal treatment 0.5 ~ 6 hour at 100 DEG C ~ 150 DEG C, is cooled to room temperature and obtains base glue;
The preparation of A material: the base glue getting 100 mass parts, adds the catalyzer of 0.01 ~ 10 mass parts, the compression set improving agent of 0.01 ~ 10 mass parts, evenly mixing, obtains A material;
The preparation of B material: the base glue getting 100 mass parts, then add the linking agent of 0.01 ~ 20 mass parts, the inhibitor of 0.001 ~ 2 mass parts, the silicon rubber stablizer of 0.1 ~ 20 mass parts, evenly mixing, obtain B material;
Be the sulfuration 5 ~ 20 minutes at 100 DEG C ~ 200 DEG C of the ratio of 1:1 by described A material and described B material according to mass ratio, then carry out post cure, obtain described rubber composition.
Particularly, described Methyl-ethylenvinyl gum refers to that side chain contains the polydimethylsiloxane of vinyl, described vinyldimethicone can be the mixture of one or more vinyldimethicone, and contents of ethylene is between 0.001% ~ 5%.The polydimethylsiloxane that described side chain contains vinyl refers to that molecular weight at 25 DEG C is 4 × 10
5~ 8 × 10
5the mixture of the different methylvinyl-polysiloxane between g/mol.
Preferably, an average group accepted way of doing sth for described Methyl-ethylenvinyl gum is as follows:
R
1 aR
2 bSiO
(4-a-b)/2
R
1for methyl; R
2for vinyl;
The span of a is: the span of 1.95<a<2.04, b is 0<b<0.185.
As a further improvement on the present invention, described mineral filler is untreated fumed silica micro mist or with one or more the mixture in the fumed silica micro mist of chlorosilane, organoalkoxysilane, hexamethyldisilazane, the process of organo-siloxane oligomer or carbon black.The specific surface area of described fumed silica micro mist is 200 ~ 400m
2/ g, preferred specific surface area is 300 ~ 400m
2/ g.More preferably, the mass ratio of described mineral filler and Methyl-ethylenvinyl gum is 100:(50 ~ 70).
As a further improvement on the present invention, described antistructurizing agent is phenylbenzene glycol or the compound containing functionalized silicon group, as at least one in hydroxyl-terminated injecting two methyl siloxane, dimethyldialkylammonium TMOS, hexamethyldisilazane.Preferably, the mass ratio of described antistructurizing agent and Methyl-ethylenvinyl gum is 100:(15 ~ 25) part.
As a further improvement on the present invention, described catalyzer be for process after platinum, platinum black, Platinic chloride, ethanol modifier Platinic chloride, at least one in Platinic chloride/olefinic siloxane complex compound and Platinic chloride tetramethyl disiloxane complex compound.Catalyst made from platonic can promote the addition reaction of Si-H and vinyl.Preferably, in described catalyzer, the mass content of metal platinum is 0.1 ~ 5000ppm, and preferably, the add-on of described catalyzer is 0.1 ~ 1 mass parts.
As a further improvement on the present invention, described compression set improving agent is 2, at least one in 4-dichlorobenzoperoxide, benzoyl peroxide, dicumyl peroxide, 2,5-dimethyl-2,5-di-t-butyl hexane peroxides, ditertiary butyl peroxide.More preferably, described compression set improving agent add-on is 1 ~ 2 mass parts.
As a further improvement on the present invention, described linking agent is the organopolysiloxane at least containing two Si-H keys.An average group accepted way of doing sth for described linking agent is as follows: R
3 cr
4 dsiO
(4-c-d)/2, wherein, R
3for methyl, R
4for H; The span of c is: the span of 1.5<c<2.5, b is 0<d<0.6.
As a further improvement on the present invention, described inhibitor is at least one in 1-ethynyl-1-hexalin, 2-methyl-3-butine-ol, 3,5-dimethyl-1-hexin-3-alcohol and 3-methyl isophthalic acid-dodecyne-3-alcohol.Can regulate the activity of catalyzer by changing the amount adding inhibitor, preferably, the add-on of described inhibitor is 0.01 ~ 0.1 mass parts.
As a further improvement on the present invention, the magnesium oxide that described silicon rubber stablizer is particle diameter between 1 nanometer ~ 100 micron, the magnesium oxide of preferable particle size between 1 nanometer ~ 50 micron, further, the magnesium oxide that described silicon rubber stablizer is particle diameter between 1 nanometer ~ 20 micron.More preferably, described silicon rubber stablizer add-on is 1 ~ 3 mass parts.
More specifically, A material and B material open refining 10 ~ 20 times, sulfuration 10 minutes at 100 DEG C ~ 200 DEG C on a mill until according to the ratio that mass ratio is 1:1, and then carry out post cure.Described post cure can be adopted international standards, 200 DEG C of sulfuration 4h.
The embodiment of the present invention provides a kind of firm silicone rubber preparation method of composition, it does reinforced filling by selecting the fine silica powder of vapor phase process, realize the high strength of silicon rubber, in silicon rubber, introduce compression set improving agent and silicon rubber stablizer, to reduce permanent compression set rate simultaneously.Before and after introducing examples of such additives, the permanent compression set rate of silicon rubber has dropped to about 10% from 38%.Meet the technical indicator required by automobile spark plug sheath completely.Silicon rubber is after hot sulfurization process, still unreacted vinyl or hydrogen base is completely there is in system, cause crosslinked complete not, thus the ageing resistance that result in sizing material is inadequate and permanent compression set rate is too high, but after introducing low compression deformation improving agent and silicon rubber stablizer, after platinum sulfuration, vinyl can be thorough by the sulfuration of low compression deformation improving agent thoroughly for unreacted, improve the cross-linking density of sizing material, permanent compression set rate can be effectively reduced like this, after making its post cure, 175 DEG C × 22h compression set rate is about 10%.Before rubber composition solidification, processibility is good, is applicable to compression molding and extrusion moulding, has high strength and excellent low permanent compression set rate after solidification.Described firm silicone rubber composition can be applicable to the fields such as automobile spark plug sheath.
Below in conjunction with specific embodiment and comparative example, specific implementation of the present invention is described in detail.
comparative example 1:
Prepare base glue
By the Methyl-ethylenvinyl gum of 200 mass parts, the fumed silica micro mist of 120 mass parts, the dimethyldialkylammonium TMOS of 40 mass parts, and thermal treatment 10 hours at 150 DEG C, be cooled to room temperature and obtain base glue; In this comparative example 1 and following comparative example and embodiment, the dimethyldialkylammonium TMOS used as antistructurizing agent also can replace with the hexamethyldisilazane of low molar mass, phenylbenzene glycol, hexamethyldisilazane and the compound containing functionalized silicon group.
Preparation A1, B1 material
The preparation of A1 material
Get the base glue of above-mentioned 100 mass parts, the platinum content adding 0.6 mass parts is the catalyzer of 5000ppm, and mixes obtained A1 and expect.
The preparation of B1 material
Get the base glue of above-mentioned 100 mass parts, add the linking agent of 10 mass parts, the inhibitor of 0.06 mass parts, and mixing evenly obtained B1 material.
Get the A1 material of 100 mass parts, 100 mass parts B1 material mixing evenly after, compression molding in 10 minutes at 140 DEG C, then post cure 4 hours at 200 DEG C, make the sample of 240mm × 120mm × 2mm and the sample 1 of thick 12mm × diameter 30mm.Survey its physicals and permanent compression set rate, the results are shown in Table 1.
comparative example 2:
Prepare base glue
By the Methyl-ethylenvinyl gum of 200 mass parts, the fumed silica micro mist of 120 mass parts, the dimethyldialkylammonium TMOS of 40 mass parts, and thermal treatment 10 hours at 150 DEG C, be cooled to room temperature and obtain base glue.
Preparation A2, B2 material
The preparation of A2 material
Get the base glue of above-mentioned 100 mass parts, the platinum content adding 0.6 mass parts is the catalyzer of 5000ppm, and mixing evenly obtained A2 material.
The preparation of B2 material
Get the base glue of above-mentioned 100 mass parts, add the linking agent of 10 mass parts, the inhibitor of 0.06 mass parts, the silicon rubber stablizer of 1 mass parts 1.5 microns; And mixing evenly obtained B2 material.
Get the A2 material of 100 mass parts, 100 mass parts B2 material mixing evenly after, compression molding in 140 DEG C × 10 minutes, then post cure 4 hours at 200 DEG C, make the sample of 240mm × 120mm × 2mm and the sample 2 of thick 12mm × diameter 30mm.Survey its physicals and permanent compression set rate, the results are shown in Table 1.
comparative example 3:
Prepare base glue
By the Methyl-ethylenvinyl gum of 200 mass parts, the fumed silica micro mist of 120 mass parts, the dimethyldialkylammonium TMOS of 40 mass parts, and thermal treatment 10 hours at 150 DEG C, be cooled to room temperature and obtain base glue.
Preparation A3, B3 material
The preparation of A3 material
Get the base glue of above-mentioned 100 mass parts, the platinum content adding 0.6 mass parts is the catalyzer of 5000ppm, and mixing evenly obtained A3 material.
The preparation of B3 silica gel
Get the base glue of above-mentioned 100 mass parts, add the linking agent of 10 mass parts, the inhibitor of 0.06 mass parts, the silicon rubber stablizer of 1.5 mass parts 1.5 microns, and mixing evenly obtained B3 material.
Get the A3 material of 100 mass parts, 100 mass parts B3 material mixing evenly after, compression molding in 140 DEG C × 10 minutes, then post cure 4 hours at 200 DEG C, make the sample of 240mm × 120mm × 2mm and the sample 3 of thick 12mm × diameter 30mm.Survey its physicals and permanent compression set rate, the results are shown in Table 1.
comparative example 4:
Prepare base glue
By the Methyl-ethylenvinyl gum of 200 mass parts, the fumed silica micro mist of 120 mass parts, the dimethyldialkylammonium TMOS of 40 mass parts, and thermal treatment 10 hours at 150 DEG C, be cooled to room temperature and obtain base glue.
Preparation A4, B4 material
The preparation of A4 material
Get the base glue of above-mentioned 100 mass parts, the platinum content adding 0.6 mass parts is the catalyzer of 5000ppm, and mixing evenly obtained A4 material.
The preparation of B4 material
Get the base glue of above-mentioned 100 mass parts, add the linking agent of 10 mass parts; The inhibitor of 0.06 mass parts, the silicon rubber stablizer of 2 mass parts 1.5 microns, and mixing evenly obtained B4 material.
Get the A4 material of 100 mass parts, 100 mass parts B4 material mixing evenly after, compression molding in 140 DEG C × 10 minutes, then post cure 4 hours at 200 DEG C, make the sample of 240mm × 120mm × 2mm and the sample 4 of thick 12mm × diameter 30mm.Survey its physicals and permanent compression set rate, the results are shown in Table 1.
comparative example 5:
Prepare base glue
By the Methyl-ethylenvinyl gum of 200 mass parts, the fumed silica micro mist of 120 mass parts, the dimethyldialkylammonium TMOS of 40 mass parts, and thermal treatment 10 hours at 150 DEG C, be cooled to room temperature and obtain base glue.
Preparation A5, B5 material
The preparation of A5 material
Get the base glue of above-mentioned 100 mass parts, the platinum content adding 0.6 mass parts is the catalyzer of 5000ppm, and mixing evenly obtained A5 material.
The preparation of B5 material
Get the base glue of above-mentioned 100 mass parts, add the linking agent of 10 mass parts, the inhibitor of 0.06 mass parts, the silicon rubber stablizer of 2.5 mass parts 1.5 microns, and mixing evenly obtained B5 material.
Get the A5 material of 100 mass parts, 100 mass parts B5 material mixing evenly after, compression molding in 140 DEG C × 10 minutes, then post cure 4 hours at 200 DEG C, make the sample of 240mm × 120mm × 2mm and the sample 5 of thick 12mm × diameter 30mm.Survey its physicals and permanent compression set rate, the results are shown in Table 1.
comparative example 6:
Prepare base glue
By the Methyl-ethylenvinyl gum of 200 mass parts, the fumed silica micro mist of 120 mass parts, the dimethyldialkylammonium TMOS of 40 mass parts, and thermal treatment 10 hours at 150 DEG C, be cooled to room temperature and obtain base glue.
Preparation A6, B6 material
The preparation of A6 material
Get the base glue of above-mentioned 100 mass parts, the platinum content adding 0.6 mass parts is the catalyzer of 5000ppm, and mixing evenly obtained A6 material.
The preparation of B6 material
Get the base glue of above-mentioned 100 mass parts, add the linking agent of 10 mass parts, the inhibitor of 0.06 mass parts, the silicon rubber stablizer of 3 mass parts 1.5 microns, and mixing evenly obtained B6 material.
Get the A6 material of 100 mass parts, 100 mass parts B6 material mixing evenly after, compression molding in 140 DEG C × 10 minutes, then post cure 4 hours at 200 DEG C, make the sample of 240mm × 120mm × 2mm and the sample 6 of thick 12mm × diameter 30mm.Survey its physicals and permanent compression set rate, the results are shown in Table 1.
Table 1
| Sample | Tensile strength (mPa) | Permanent compression set rate (175 DEG C × 22 hours) |
| Sample 1 | 12.35 | 38.3％ |
| Sample 2 | 12.26 | 28.7％ |
| Sample 3 | 12.38 | 26.7％ |
| Sample 4 | 12.41 | 26.9％ |
| Sample 5 | 12.18 | 27.8％ |
| Sample 6 | 12.21 | 29.3％ |
comparative example 7:
Prepare base glue
By the Methyl-ethylenvinyl gum of 200 mass parts, the fumed silica micro mist of 120 mass parts, the dimethyldialkylammonium TMOS of 40 mass parts, and thermal treatment 10 hours at 150 DEG C, be cooled to room temperature and obtain base glue.
Preparation A7, B7 material
The preparation of A7 material
Get the base glue of above-mentioned 100 mass parts, the platinum content adding 0.6 mass parts is the catalyzer of 5000ppm, the compression set control agent of 0.5 mass parts, and mixing evenly obtained A7 material.
The preparation of B7 material
Get the base glue of above-mentioned 100 mass parts, add the linking agent of 10 mass parts, the inhibitor of 0.06 mass parts, and mixing evenly obtained B7 material.
Get the A7 material of 100 mass parts, 100 mass parts B7 material mixing evenly after, compression molding in 140 DEG C × 10 minutes, then post cure 4 hours at 200 DEG C, make the sample of 240mm × 120mm × 2mm and the sample 7 of thick 12mm × diameter 30mm.Survey its physicals and permanent compression set rate, the results are shown in Table 2.
comparative example 8:
Prepare base glue
By the Methyl-ethylenvinyl gum of 200 mass parts, the fumed silica micro mist of 120 mass parts, the dimethyldialkylammonium TMOS of 40 mass parts, and thermal treatment 10 hours at 150 DEG C, be cooled to room temperature and obtain base glue.
Preparation A8, B8 material
The preparation of A8 material
Get the base glue of above-mentioned 100 mass parts, the platinum content adding 0.6 mass parts is the catalyzer of 5000ppm, the compression set control agent of 1 mass parts, and mixing evenly obtained A8 material.
The preparation of B8 material
Get the base glue of above-mentioned 100 mass parts, add the linking agent of 10 mass parts, the inhibitor of 0.06 mass parts, and mixing evenly obtained B8 material.
Get the A8 material of 100 mass parts, 100 mass parts B8 material mixing evenly after, compression molding in 140 DEG C × 10 minutes, then post cure 4 hours at 200 DEG C, make the sample of 240mm × 120mm × 2mm and the sample 8 of thick 12mm × diameter 30mm.Survey its physicals and permanent compression set rate, the results are shown in Table 2.
comparative example 9:
Prepare base glue
By the Methyl-ethylenvinyl gum of 200 mass parts, the fumed silica micro mist of 120 mass parts, the dimethyldialkylammonium TMOS of 40 mass parts, and thermal treatment 10 hours at 150 DEG C, be cooled to room temperature and obtain base glue.
Preparation A9, B9 material
The preparation of A9 glue
Get the base glue of above-mentioned 100 mass parts, the platinum content adding 0.6 mass parts is the catalyzer of 5000ppm, the compression set control agent of 1.5 mass parts, and mixing evenly obtained A9 material.
The preparation of B9 glue
Get the base glue of above-mentioned 100 mass parts, add the linking agent of 10 mass parts, the inhibitor of 0.06 mass parts, and mixing evenly obtained B9 material.
Get the A9 material of 100 mass parts, 100 mass parts B9 material mixing evenly after, compression molding in 140 DEG C × 10 minutes, then post cure 4 hours at 200 DEG C, make the sample of 240mm × 120mm × 2mm and the sample 9 of thick 12mm × diameter 30mm.Survey its physicals and permanent compression set rate, the results are shown in Table 2.
comparative example 10:
Prepare base glue
By the Methyl-ethylenvinyl gum of 200 mass parts, the fumed silica micro mist of 120 mass parts, the dimethyldialkylammonium TMOS of 40 mass parts, and thermal treatment 10 hours at 150 DEG C, be cooled to room temperature and obtain base glue.
Preparation A10, B10 material
The preparation of A10 material
Get the base glue of above-mentioned 100 mass parts, the platinum content adding 0.6 mass parts is the catalyzer of 5000ppm, the compression set control agent of 2 mass parts, and mixing evenly obtained A10 material.
The preparation of B10 material
Get the base glue of above-mentioned 100 mass parts, add the linking agent of 10 mass parts, the inhibitor of 0.06 mass parts, and mixing evenly obtained B10 material.
Get the A10 material of 100 mass parts, 100 mass parts B10 material mixing evenly after, compression molding in 140 DEG C × 10 minutes, then post cure 4 hours at 200 DEG C, make the sample of 240mm × 120mm × 2mm and the sample 10 of thick 12mm × diameter 30mm.Survey its physicals and permanent compression set rate, the results are shown in Table 2.
comparative example 11:
Prepare base glue
By the Methyl-ethylenvinyl gum of 200 mass parts, the fumed silica micro mist of 120 mass parts, the dimethyldialkylammonium TMOS of 40 mass parts, and thermal treatment 10 hours at 150 DEG C, be cooled to room temperature and obtain base glue.
Preparation A11, B11 material
The preparation of A11 material
Get the base glue of above-mentioned 100 mass parts, the platinum content adding 0.6 mass parts is the catalyzer of 5000ppm, the compression set control agent of 2.5 mass parts, and mixing evenly obtained A11 material.
The preparation of B11 material
Get the base glue of above-mentioned 100 mass parts, add the linking agent of 10 mass parts, the inhibitor of 0.06 mass parts, and mixing evenly obtained B11 material.
Get the A11 material of 100 mass parts, after the B11 material of 100 mass parts mixes, compression molding in 140 DEG C × 10 minutes, then post cure 4 hours at 200 DEG C, make the sample of 240mm × 120mm × 2mm and the sample 11 of thick 12mm × diameter 30mm.Survey its physicals and permanent compression set rate, the results are shown in Table 2.
comparative example 12:
Prepare base glue
By the Methyl-ethylenvinyl gum of 200 mass parts, the fumed silica micro mist of 120 mass parts, the dimethyldialkylammonium TMOS of 40 mass parts, and thermal treatment 10 hours at 150 DEG C, be cooled to room temperature and obtain base glue.
Preparation A12, B12 material
The preparation of A12 material
Get the base glue of above-mentioned 100 mass parts, the platinum content adding 0.6 mass parts is the catalyzer of 5000ppm, the compression set control agent of 3 mass parts, and mixing evenly obtained A12 material.
The preparation of B12 material
Get the base glue of above-mentioned 100 mass parts, add the linking agent of 10 mass parts, the inhibitor of 0.06 mass parts, and mixing evenly obtained B12 material.
Get the A12 material of 100 mass parts, 100 mass parts B12 material mixing evenly after, compression molding in 140 DEG C × 10 minutes, then post cure 4 hours at 200 DEG C, make the sample of 240mm × 120mm × 2mm and the sample 12 of thick 12mm × diameter 30mm.Survey its physicals and permanent compression set rate, the results are shown in Table 2.
Table two
| Sample | Tensile strength (mPa) | Permanent compression set rate (175 DEG C × 22 hours) |
| Sample 7 | 12.53 | 25.8％ |
| Sample 8 | 12.41 | 21.3％ |
| Sample 9 | 12.49 | 20.1％ |
| Sample 10 | 12.47 | 22.6％ |
| Sample 11 | 12.46 | 24.2％ |
| Sample 12 | 12.38 | 25.7％ |
embodiment 1:
Prepare base glue
By the Methyl-ethylenvinyl gum of 200 mass parts, the fumed silica micro mist of 120 mass parts, the dimethyldialkylammonium TMOS of 40 mass parts, and thermal treatment 10 hours at 150 DEG C, be cooled to room temperature and obtain base glue.
Preparation A13, B13 material
The preparation of A13 material
Get the base glue of above-mentioned 100 mass parts, the platinum content adding 0.6 mass parts is the catalyzer of 5000ppm, the compression set control agent of 0.5 mass parts, and mixing evenly obtained A13 material.
The preparation of B13 material
Get the base glue of above-mentioned 100 mass parts, add the linking agent of 10 mass parts, the inhibitor of 0.06 mass parts, the silicon rubber stablizer of 2 mass parts 1.5 microns, and mixing evenly obtained B13 material.
Get the A13 material of 100 mass parts, after the B13 material of 100 mass parts mixes, compression molding in 140 DEG C × 10 minutes, then post cure 4 hours at 200 DEG C, make the sample of 240mm × 120mm × 2mm and the sample 13 of thick 12mm × diameter 30mm.Survey its physicals and permanent compression set rate, the results are shown in Table 3.
embodiment 2:
Prepare base glue
By the Methyl-ethylenvinyl gum of 200 mass parts, the fumed silica micro mist of 120 mass parts, the dimethyldialkylammonium TMOS of 40 mass parts, and thermal treatment 10 hours at 150 DEG C, be cooled to room temperature and obtain base glue.
Preparation A14, B14 material
The preparation of A14 material
Get the base glue of above-mentioned 100 mass parts, the platinum content adding 0.6 mass parts is the catalyzer of 5000ppm, the compression set control agent of 1 mass parts, and mixing evenly obtained A14 material.
The preparation of B14 material
Get the base glue of above-mentioned 100 mass parts, add the linking agent of 10 mass parts; The inhibitor of 0.06 mass parts, the silicon rubber stablizer of 2 mass parts 1.5 microns, and mixing evenly obtained B14 material.
Get the A14 material of 100 mass parts, after the B14 material of 100 mass parts mixes, compression molding in 140 DEG C × 10 minutes, then post cure 4 hours at 200 DEG C, make the sample of 240mm × 120mm × 2mm and the sample 14 of thick 12mm × diameter 30mm.Survey its physicals and permanent compression set rate, the results are shown in Table 3.
embodiment 3:
Prepare base glue
By the Methyl-ethylenvinyl gum of 200 mass parts, the fumed silica micro mist of 120 mass parts, the dimethyldialkylammonium TMOS of 40 mass parts, and thermal treatment 10 hours at 150 DEG C, be cooled to room temperature and obtain base glue.
Preparation A15, B15 material
The preparation of A15 material
Get the base glue of above-mentioned 100 mass parts, the platinum content adding 0.6 mass parts is the catalyzer of 5000ppm, the compression set control agent of 1.5 mass parts, and mixing evenly obtained A15 material.
The preparation of B15 material
Get the base glue of above-mentioned 100 mass parts, add the linking agent of 10 mass parts, the inhibitor of 0.06 mass parts, the silicon rubber stablizer of 2 mass parts 1.5 microns, and mixing evenly obtained B15 material.
Get the A15 material of 100 mass parts, 100 mass parts B15 material mixing evenly after, compression molding in 140 DEG C × 10 minutes, then post cure 4 hours at 200 DEG C, make the sample of 240mm × 120mm × 2mm and the sample 15 of thick 12mm × diameter 30mm.Survey its physicals and permanent compression set rate, the results are shown in Table 3.
embodiment 4:
Prepare base glue
By the Methyl-ethylenvinyl gum of 200 mass parts, the fumed silica micro mist of 120 mass parts, the dimethyldialkylammonium TMOS of 40 mass parts, and thermal treatment 10 hours at 150 DEG C, be cooled to room temperature and obtain base glue.
Preparation A16, B16 material
The preparation of A16 material
Get the base glue of above-mentioned 100 mass parts, the platinum content adding 0.6 mass parts is the catalyzer of 5000ppm, the compression set control agent of 2 mass parts, and mixing evenly obtained A16 material.
The preparation of B16 material
Get the base glue of above-mentioned 100 mass parts, add the linking agent of 10 mass parts, the inhibitor of 0.06 mass parts, the silicon rubber stablizer of 2 mass parts 1.5 microns, and mixing evenly obtained B16 material.
Get the A16 material of 100 mass parts, 100 mass parts B16 material mixing evenly after, compression molding in 140 DEG C × 10 minutes, then post cure 4 hours at 200 DEG C, make the sample of 240mm × 120mm × 2mm and the sample 16 of thick 12mm × diameter 30mm.Survey its physicals and permanent compression set rate, the results are shown in Table 3.
embodiment 5:
Prepare base glue
By the Methyl-ethylenvinyl gum of 200 mass parts, the fumed silica micro mist of 120 mass parts, the dimethyldialkylammonium TMOS of 40 mass parts, and thermal treatment 10 hours at 150 DEG C, be cooled to room temperature and obtain base glue.
Preparation A17, B17 material
The preparation of A17 material
Get the base glue of above-mentioned 100 mass parts, the platinum content adding 0.6 mass parts is the catalyzer of 5000ppm, the compression set control agent of 2.5 mass parts, and mixing evenly obtained A17 material.
The preparation of B17 material
Get the base glue of above-mentioned 100 mass parts, add the linking agent of 10 mass parts, the inhibitor of 0.06 mass parts, the silicon rubber stablizer of 2 mass parts 1.5 microns, and mixing evenly obtained B17 material.
Get the A17 material of 100 mass parts, 100 mass parts B17 material mixing evenly after, compression molding in 140 DEG C × 10 minutes, then post cure 4 hours at 200 DEG C, make the sample of 240mm × 120mm × 2mm and the sample 17 of thick 12mm × diameter 30mm.Survey its physicals and permanent compression set rate, the results are shown in Table 3.
embodiment 6:
Prepare base glue
By the Methyl-ethylenvinyl gum of 200 mass parts, the fumed silica micro mist of 120 mass parts, the dimethyldialkylammonium TMOS of 40 mass parts, and thermal treatment 10 hours at 150 DEG C, be cooled to room temperature and obtain base glue.
Preparation A18, B18 material
The preparation of A18 glue
Get the base glue of above-mentioned 100 mass parts, the platinum content adding 0.6 mass parts is the catalyzer of 5000ppm, the compression set control agent of 3 mass parts, and mixing evenly obtained A18 material.
The preparation of B18 material
Get the base glue of above-mentioned 100 mass parts, add the linking agent of 10 mass parts, the inhibitor of 0.06 mass parts, the silicon rubber stablizer of 2 mass parts 1.5 microns, and mixing evenly obtained B18 material.
Get the A18 material of 100 mass parts, 100 mass parts B18 material mixing evenly after, compression molding in 140 DEG C × 10 minutes, then post cure 4 hours at 200 DEG C, make the sample of 240mm × 120mm × 2mm and the sample 18 of thick 12mm × diameter 30mm.Survey its physicals and permanent compression set rate, the results are shown in Table 3.
Table 3
| Sample | Tensile strength (mPa) | Permanent compression set rate (175 DEG C × 22 hours) |
| Sample 13 | 12.41 | 15.1％ |
| Sample 14 | 12.46 | 10.4％ |
| Sample 15 | 12.49 | 8.9％ |
| Sample 16 | 12.51 | 9.2％ |
| Sample 17 | 12.28 | 10.9％ |
| Sample 18 | 12.48 | 13.8％ |
Remarks: the test condition of permanent compression set rate is compression 25%, temperature 175 DEG C, 22 hours time.
Before rubber composition solidification, processibility is good, is applicable to compression molding and extrusion moulding, has high strength and excellent low permanent compression set rate after solidification.The firm silicone rubber composition that described firm silicone rubber preparation method of composition obtains has the feature of low permanent compression set, high strength, can be applicable to the fields such as automobile spark plug sheath.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. a preparation method for firm silicone rubber composition, is characterized in that, comprises the steps:
Prepare base glue: be 100:(1 ~ 80 according to mass ratio): (1 ~ 30) is by Methyl-ethylenvinyl gum, mineral filler and antistructurizing agent mixing, thermal treatment 0.5 ~ 6 hour at 100 DEG C ~ 150 DEG C, is cooled to room temperature and obtains base glue;
The preparation of A material: the base glue getting 100 mass parts, adds the catalyzer of 0.01 ~ 10 mass parts, the compression set improving agent of 0.01 ~ 10 mass parts, evenly mixing, obtains A material;
The preparation of B material: the base glue getting 100 mass parts, then add the linking agent of 0.01 ~ 20 mass parts, the inhibitor of 0.001 ~ 2 mass parts, the silicon rubber stablizer of 0.1 ~ 20 mass parts, evenly mixing, obtain B material;
Be the sulfuration 5 ~ 20 minutes at 100 DEG C ~ 200 DEG C of the ratio of 1:1 by described A material and described B material according to mass ratio, then carry out post cure, obtain described firm silicone rubber composition.
2. the preparation method of firm silicone rubber composition according to claim 1, it is characterized in that, described Methyl-ethylenvinyl gum is the polydimethylsiloxane that side chain contains vinyl, described vinyldimethicone can be the mixture of one or more vinyldimethicone, and contents of ethylene is between 0.001% ~ 5%.
3. the preparation method of firm silicone rubber composition according to claim 1, it is characterized in that, described mineral filler is untreated fumed silica micro mist or with one or more the mixture in the fumed silica micro mist of chlorosilane, organoalkoxysilane, hexamethyldisilazane, the process of organo-siloxane oligomer or carbon black.
4. the preparation method of firm silicone rubber composition according to claim 1, it is characterized in that, described antistructurizing agent is at least one in the hydroxyl-terminated injecting two methyl siloxane of low molar mass, phenylbenzene glycol, dimethyldialkylammonium TMOS, hexamethyldisilazane.
5. the preparation method of firm silicone rubber composition according to claim 1, is characterized in that, described linking agent is the organopolysiloxane at least containing two Si-H keys.
6. the preparation method of firm silicone rubber composition according to claim 1, it is characterized in that, described catalyzer is the Platinic chloride of platinum after process, platinum black, Platinic chloride, ethanol modifier, at least one in Platinic chloride/olefinic siloxane complex compound and Platinic chloride tetramethyl disiloxane complex compound.
7. the preparation method of firm silicone rubber composition according to claim 1, it is characterized in that, described inhibitor is at least one in 1-ethynyl-1-hexalin, 2-methyl-3-butine-ol, 3,5-dimethyl-1-hexin-3-alcohol and 3-methyl isophthalic acid-dodecyne-3-alcohol.
8. the preparation method of firm silicone rubber composition according to claim 1, is characterized in that, the magnesium oxide that described silicon rubber stablizer is particle diameter between 1 nanometer ~ 100 micron.
9. the preparation method of firm silicone rubber composition according to claim 1, it is characterized in that, described compression set improving agent is 2,4-dichlorobenzoperoxide, benzoyl peroxide, dicumyl peroxide, 2, at least one in 5-dimethyl-2,5-di-t-butyl hexane peroxide, ditertiary butyl peroxide.
10. the preparation method of firm silicone rubber composition according to claim 1, is characterized in that, described silicon rubber stablizer add-on is 0.1 ~ 20 mass parts, and described compression set improving agent add-on is 0.01 ~ 10 mass parts.
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|---|---|---|---|---|
| CN1170736A (en) * | 1996-07-17 | 1998-01-21 | 瓦克化学有限公司 | Liquid silicone rubber with low compression set |
| CN101983989A (en) * | 2010-11-01 | 2011-03-09 | 深圳市森日有机硅材料有限公司 | Liquid silicon rubber composition and preparation method thereof |
| CN102936415A (en) * | 2012-11-22 | 2013-02-20 | 深圳市森日有机硅材料有限公司 | Liquid silicone rubber composition having low permanent compression deformation and preparation method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1170736A (en) * | 1996-07-17 | 1998-01-21 | 瓦克化学有限公司 | Liquid silicone rubber with low compression set |
| CN101983989A (en) * | 2010-11-01 | 2011-03-09 | 深圳市森日有机硅材料有限公司 | Liquid silicon rubber composition and preparation method thereof |
| CN102936415A (en) * | 2012-11-22 | 2013-02-20 | 深圳市森日有机硅材料有限公司 | Liquid silicone rubber composition having low permanent compression deformation and preparation method thereof |
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Address after: Longgang District of Shenzhen City, Guangdong province 518000 Ping Street in the community square Po Village building I No. 1, C building Applicant after: Shenzhen Square Silicone Co., Ltd. Address before: Longgang District of Shenzhen City, Guangdong province 518112 Ping Street in the community square Po Village building I No. 1, C building Applicant before: Shenzhen Square Silicone Materials Co., Ltd. |
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Application publication date: 20150930 |