CN103965640A - Foamed liquid silicon rubber and preparation method thereof - Google Patents
Foamed liquid silicon rubber and preparation method thereof Download PDFInfo
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- CN103965640A CN103965640A CN201310655490.4A CN201310655490A CN103965640A CN 103965640 A CN103965640 A CN 103965640A CN 201310655490 A CN201310655490 A CN 201310655490A CN 103965640 A CN103965640 A CN 103965640A
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Abstract
The invention discloses a preparation method of foamed liquid silicon rubber. The preparation method comprises the steps as follows: 1) a basic material is prepared frompolysiloxane composition and reinforcing filler and divided into two parts; 2) a catalyst is added to one part to prepare a material A; 3) an inhibitor and a cross-linking agent are added to the other part to prepare a material B; 4) the material A and the material B are mixed, a gas mixture with the weight ratio of 20-85%, preferably, 60% is added, the gas mixture consists of air, oxygen and CO2, and a finished foamed liquid silicon rubber product is obtained after heating and curing. According to the preparation method, the prepared foamed rubber is even in foam size, complete in foaming, high in elasticity, high in toughness, smooth in surface, capable of saving the production cost and widely applicable to various production fields of the industrial injection molding process.
Description
Technical field
The present invention relates to a kind of silicon rubber and preparation method thereof, relate in particular to a kind of foamed silastic and preparation method thereof.
Background technology
Silicon rubber is one of important organosilicon product.Silicon rubber has many uniquenesses and excellent performance is widely used at aspects such as Aeronautics and Astronautics, electric, light industry, machinery, building, chemical industry, medical science, daily necessities.Liquid silastic is a class organic silica gel of relative mixed milling type semi-solid state silicon rubber and common self cure single component silica gel.
Main existing method is that thermoplastic resin hollow bead powder or the pre-thermoplastic resin hollow bead powder expanding (obtaining low-gravity rubber composition) that when heating expands are prepared in proportion as whipping agent and rubber composition, expansion along with thermoplastic resin hollow bead powder, rubber composition is heated and is cured, thereby obtains the silicon rubber (referring to Japanese patent application H5-209080 or US Patent No. 6300383) of foaming.But the method still has problems: operating process is restive, and whipping agent is difficult to mix, thereby non-homogeneous expansion is even, and the inhomogeneous and proportion of the foamed silastic abscess-size made changes greatly, and the elasticity that foams is inadequate.A kind of liquid silicon rubber composition has been produced in this area research and development, when solidifying, said composition becomes the problem that the foamed silastic (referring to patent application publication number CN1303890A) with low-gravity and low heat conductivity has to a certain degree solved thermoplastic resin hollow bead powder whipping agent married operation difficulty, and the proportion of the foamed silastic of preparation changes low with thermal conductivity greatly problem.But the whipping agent that the method is used is still used the thermoplastic resin hollow bead powder that adds thermal expansion, powder-type whipping agent still exists with the not evenly problem of mixing of silicon rubber, thereby the uniformity coefficient of the abscess-size of the silica-gel sponge body of producing is inadequate, the proportion of the rubber composition of preparing, elasticity, the performances such as hardness need further raising.
Summary of the invention
In order to address the above problem, the invention provides a kind of foamed silastic composition and method of making the same, to solve, use conventional powder type whipping agent to mix even not with silicon rubber, thereby the proportion of the foamed silastic composition of preparing, elasticity, the performances such as hardness do not reach the technical problem of requirement.
The invention provides a kind of foaming liquid silicon rubber preparation method, comprise the steps:
1) by polysiloxane composition and reinforced filling, make basic material, be divided into two parts;
2) in portion, add the finish mix A of catalyzer wherein;
3) in another part, add inhibitor and the finish mix B of linking agent;
Wherein, also comprise that step 4) mixes described material A and material B, and add weight ratio be 20-85% by air, oxygen and CO
2the mixed gas forming, preferred weight ratio is 60%, obtains foaming liquid silicon rubber finished product after being heating and curing.
Wherein, polysiloxane composition and reinforced filling silicon-dioxide that described step 1) is is (1) by general formula, after mixing with weight ratio 10:1～4, through thermal treatment and vacuum-treat, deviate from low molecular basis material, obtain basic material, wherein, described silicon-dioxide is selected from organosilazanes or silane coupling agent and makes aerosil or the precipitated silica after hydrophobic is processed;
Wherein, described general formula (1) is:
R
2SiO(SiRR’O)n Si R
2
R is vinyl,
R ' and R are identical or different, are vinyl, methyl, alkyl or phenyl,
N is the polymerization degree (30≤n≤2000).
Wherein, the thermal treatment described in step 1) and vacuum-treat step are that under 145-160 ℃ of constant temperature of maintenance, first normal pressure stirred after 1.5-2.5 hour, stirred 2.0-3.5 hour in final vacuum.
Wherein, described step 2) for portion wherein adds 0.1%-0.5%(wt%), be the finish mix A of platinum complex compound catalyst of Platinic chloride and tetramethyl divinyl disiloxane polymkeric substance.
Wherein, in the polymkeric substance of described Platinic chloride and tetramethyl divinyl disiloxane, platinum content is 0.32-0.38%(wt%).
Wherein, described step 3) is for adding the organic hydride polysiloxane that is not less than 3 hydrogen silicon links of general formula (2) to another part, its hydrogen content is 0.12%-1%(wt%), and 0.8%-4.5%(wt%) the finish mix B of alkynol class inhibitor, preferably, described alkynol class curing inhibitors is selected from the alkynyl-3-alcohol, 3 of 3-methyl-, and 5-dimethyl-1-is alkynyl-3-alcohol, 2-methyl-3-butynyl-2-alcohol and/or 2-phenyl-3-butynyl-2-alcohol;
Wherein, described general formula (2) is:
R
2SiO(SiRR’O)
x(SiHR’O)
ySi R
2
R is vinyl,
R ' and R are identical or different, are vinyl, methyl, alkyl or phenyl,
X and y are the polymerization degree (0≤x≤300) (3≤y≤30).
Wherein, described polysiloxane composition is the composition that is selected from following polysiloxane one or more,
I. viscosity is that 5000-10000mPas (25 ℃), contents of ethylene are 0.25%-0.5%(wt%) polysiloxane;
II. viscosity is that 10000-40000mPas (25 ℃), contents of ethylene are 0.15%-0.5%(wt%) polysiloxane;
III. viscosity is that 1000-2000mPas (25 ℃), contents of ethylene are 0.3%-1.0%(wt%) polysiloxane;
IV. viscosity is that 1000-5000mPas (25 ℃), contents of ethylene are 1.0%-10%(wt%) polysiloxane.
Wherein, expect to add described mixed gas after A and material B mix with weight ratio 1:1 in described step 4), 110-180 ℃ of heating obtains foaming liquid silicon rubber finished product after 3-8 minute, preferred, and 3 minutes after fixing of 160 ℃ of heating obtain finished product.
Wherein, described mixed gas consist of weight percent meter: 15%～25% air, 30%～40% oxygen, 40%～50%CO
2, preferred, the composition weight percent of mixed gas is counted: 20% air, 35% oxygen, 45%CO
2.
The present invention also comprises a kind of foaming liquid rubber composition of being prepared by above-mentioned preparation method.
Compare with thermoplastic resin powder's whipping agent that tradition adopts, preparation method of the present invention, use mixing air as whipping agent, can make mix full and uniform with silicon rubber of whipping agent, thereby the bubble producing in foaming process is even, colloidal foam size uniform after foaming, completely, elasticity is high, toughness is large, smooth surface in foaming, and preparation method of the present invention has used the mixed gas of easy easy acquisition as whipping agent, also saved greatly production cost.The high-performance foamed silica gel that preparation method therefore of the present invention produces, can be widely used in each production field of industrial Shooting Technique.
Embodiment
In following specific embodiment, if no special instructions, described part all refers to mass parts, and described per-cent is weight percentage.
Comparative example 1: adopt thermoplasticity hollow bead powder preparation foaming liquid silicon rubber
Step 1): the polysiloxane composition I that adds polysiloxane end-blocking in strong stirring mixing machine. viscosity is that 5000-10000mPas (25 ℃), contents of ethylene are 0.25%-0.5%(wt%) polysiloxane, dosage is 20 parts; And II. viscosity is that 10000-40000mPas (25 ℃), contents of ethylene are 0.15%-0.5%(wt%) polysiloxane dosage be 20 parts.
And then adding hexamethyldisilazane coupling agent to make the aerosil that hydrophobic is processed, 20 parts of dosages, are uniformly mixed agglomerating 1 hour.
Then be warming up to 150 ℃ of left and right constant temperature normal pressures and stir 2 hours, then vacuum stirring stopped vacuum after 3 hours under these 150 ℃ of left and right constant temperatures.
Be cooled to afterwards after 90 ℃ and add I. viscosity is that 5000-10000mPas (25 ℃), contents of ethylene are 0.25%-0.5%(wt%) polysiloxane, 15 parts of dosages, after evenly mixing, discharging grinds to form base-material, also i.e. low molecular basis material, and this base-material is divided into two parts.
Step 2) adding platinum content in a base-material is wherein the polymkeric substance of (0.32wt%) Platinic chloride and tetramethyl divinyl disiloxane, and dosage is 0.35 part of finish mix A of platinum complex compound.
Step 3) is 0.12%-1%(wt% to adding hydrogen content in another part of base-material) polysiloxane, dosage is 3 parts; 2% alkynol class inhibitor 3,5-dimethyl-1-is alkynyl-3-alcohol, and dosage is 0.04 part; Microballoon hollow foamed particle powder (this microballon of pine F-36D dry powder type, the meeting of this grease of pine pharmacy strain formula) dosage is 5 parts, makes B;
Step 4) adds high speed dispersor fully to mix A and B mixing according to the ratio of A:B=1:1, obtain foaming liquid silica-gel composition, the viscosity of composition is greatly about 250000m Pas, hold in Flat bottom container, put into oven temperature and be heating and curing approximately 10 minutes time 100 ℃ of left and right, obtain solidifying foamed silastic.
The thickness of foamed glue prepared by the method is not send out 1.5 times of left and right before, and the visible foaming of foamed glue sections observation is more inhomogeneous, and elasticity and toughness are poor.
Embodiment 2: the mixing air whipping agent (wt%) of employing 20% is prepared foaming liquid silicon rubber
Step 1): add I at strong stirring mixing machine. viscosity is that 5000-10000mPas (25 ℃), contents of ethylene are 0.25%-0.5%(wt%) polysiloxane, dosage is 20 parts; And II. viscosity is that 10000-40000mPas (25 ℃), contents of ethylene are 0.15%-0.5%(wt%) polysiloxane dosage be 20 parts.
And then adding hexamethyldisilazane coupling agent to make the aerosil that hydrophobic is processed, 20 parts of dosages, are uniformly mixed agglomerating 1 hour.
Then be warming up to 150 ℃ of left and right constant temperature normal pressures and stir 2 hours, then vacuum stirring stopped vacuum after 3 hours under these 150 ℃ of left and right constant temperatures.
Be cooled to afterwards after 90 ℃ and add I. viscosity is that 5000-10000mPas (25 ℃), contents of ethylene are 0.25%-0.5%(wt%) polysiloxane, 15 parts of dosages, after evenly mixing, discharging grinds to form base-material, also i.e. low molecular basis material, and this base-material is divided into two parts.
Step 2) adding platinum content in a base-material is wherein the polymkeric substance of (0.32wt%) Platinic chloride and tetramethyl divinyl disiloxane, and dosage is 0.35 part of finish mix A of platinum complex compound.
Step 3) is 0.12%-1%(wt% to adding hydrogen content in another part of base-material) polysiloxane, dosage is 3 parts; 2% alkynol class inhibitor 3,5-dimethyl-1-is alkynyl-3-alcohol, and dosage is 0.04 part of finish mix B.
Step 4) is mixed A and B to add high speed dispersor fully to mix according to the ratio of A:B=1:1, then to add weight percent be that (mixed gas is by 15% air, 35% oxygen, 50%CO for 20% mixed gas
2form), obtain foaming liquid silica-gel composition, the viscosity of composition is greatly about 200000mPas, hold in Flat bottom container, putting into oven temperature is heating and curing approximately 8 minutes time at 110 ℃, the thickness that obtains curing post-foaming glue is not send out 4.5 times of left and right before, and the visible foaming of foamed glue sections observation is more even, and elasticity and toughness is (in Table 1) better.
Embodiment 3: the mixing air whipping agent (wt%) of employing 60% is prepared foaming liquid silicon rubber
Step 1): add III at strong stirring mixing machine. viscosity is that 1000-2000mPas (25 ℃), contents of ethylene are 0.3%-1.0%(wt%) polysiloxane, dosage is 30 parts; And II. viscosity is that 10000-40000mPas (25 ℃), contents of ethylene are 0.15%-0.5%(wt%) polysiloxane dosage be 20 parts, dosage is 15 parts;
And then adding hexamethyldisilazane coupling agent to make the aerosil that hydrophobic is processed, 20 parts of dosages, are uniformly mixed agglomerating 1 hour.
Then be warming up to 150 ℃ of left and right constant temperature normal pressures and stir 2 hours, then vacuum stirring stopped vacuum after 3 hours under these 150 ℃ of left and right constant temperatures.
Be cooled to after 90 ℃ and add I. viscosity is that 5000-10000mPas (25 ℃), contents of ethylene are 0.25%-0.5%(wt%) polysiloxane, 15 parts of dosages, after evenly mixing, discharging grinds to form base-material, also i.e. low molecular basis material, and this base-material is divided into two parts.
Step 2) to add platinum content be the polymkeric substance of (0.375wt%) Platinic chloride and tetramethyl divinyl disiloxane to portion, and dosage is 0.25 part of finish mix A of platinum complex compound.
It is 0.12%-1%(wt% that step 3) portion adds hydrogen content) low polymerization degree polysiloxane, dosage is 3 parts; 2% alkynol class inhibitor 3,5-dimethyl-1-is alkynyl-3-alcohol, and dosage is 0.04 part, finish mix B.
Step 4) is mixed A and B to add high speed dispersor fully to mix according to the ratio of A:B=1:1, then to add weight percent be that (mixed gas is by 20% air, 35% oxygen, 45%CO for 60% mixed gas
2form), obtain foaming liquid silica-gel composition, the viscosity of composition is greatly about 150000mPas, hold in Flat bottom container, putting into oven temperature is heating and curing approximately 5 minutes time at 150 ℃, the thickness that obtains curing post-foaming glue is not send out 8 times of left and right before, and the visible foaming of foamed glue sections observation is more even, and elasticity and toughness is (in Table 1) better.
Embodiment 4: the mixing air whipping agent (wt%) of employing 80% is prepared foaming liquid silicon rubber
Step 1): add III at strong stirring mixing machine. viscosity is that 1000-2000mPas (25 ℃), contents of ethylene are 0.3%-1.0%(wt%) polysiloxane, dosage is 30 parts, and I. viscosity is that 5000-10000mPas (25 ℃), contents of ethylene are 0.25%-0.5%(wt%) polysiloxane, dosage is 15 parts.
Add hexamethyldisilazane coupling agent to make the aerosil that hydrophobic is processed, 20 parts of dosages, are uniformly mixed agglomerating 1 hour.
Then be warming up to 150 ℃ of left and right constant temperature normal pressures and stir 2 hours, then vacuum stirring stopped vacuum after 3 hours under these 150 ℃ of left and right constant temperatures.
Be cooled to after 90 ℃ and add IV. viscosity is that 1000-5000mPas (25 ℃), contents of ethylene are 1.0%-10%(wt%) polysiloxane, 5 parts of dosages, after evenly mixing, discharging grinds to form base-material; And base-material is divided into two parts;
Step 2) to add platinum content be the polymkeric substance of (0.375wt%) Platinic chloride and tetramethyl divinyl disiloxane to portion, and dosage is 0.25 part of finish mix A of platinum complex compound.
It is 0.12%-1%(wt% that step 3) portion adds hydrogen content) low polymerization degree polysiloxane, dosage is 3 parts; 2% alkynol class inhibitor 3,5-dimethyl-1-is alkynyl-3-alcohol, and dosage is 0.04 part, finish mix B.
Step 4) is mixed A and B to add high speed dispersor fully to mix according to the ratio of A:B=1:1, then to add weight percent be that (mixed gas is by 25% air, 35% oxygen, 40%CO for 80% mixed gas
2form), obtain foaming liquid silica-gel composition, the viscosity of composition is greatly about 50000m Pas, hold in Flat bottom container, putting into oven temperature is heating and curing approximately 3 minutes time at 180 ℃, the thickness that obtains curing post-foaming glue is not send out 6 times of left and right before, and the visible foaming of foamed glue sections observation is more even, and elasticity and toughness is (in Table 1) better.
The foaming liquid rubber composition Performance Ratio that the preparation method of table 1 embodiment 1-4 obtains
Experimental data by above comparative example 1 and embodiment 2-4 is visible, the successful that embodiment 2-4 is used mixed gas of the present invention to foam as whipping agent is better than traditional method, as comparative example 1 is used the foaming of thermoplastic resin lipoid microsphere, adopt the preparation method of embodiment of the present invention 2-4, whipping agent can evenly also fully mix with liquid silica gel, fully sneak into after mixed gas, bubble in liquid silica gel keeps certain tension force and bubble even, make the colloid elasticity after foaming high, toughness is large, smooth surface, foam size is even, foaming completely, and use preparation method of the present invention also to save greatly cost, the high performance foamed silica gel that the closed pore perforate of producing is evenly distributed, can be widely used in industrial Shooting Technique and produce multiple product.
Also surprised discovery of the present invention, use the air of different ratios, oxygen and titanium dioxide mixed gas are used as whipping agent, as long as ratio changes within the scope of aforementioned proportion, all can play good foaming effect, it is little that the concrete ratio of the component of its mixed gas affects difference to foaming effect, but the add-on of mixed gas affects significantly on foaming effect, in the scope of mixed gas that adds weight ratio 20%-80%, than the performance of the foamed silica gel that adopts traditional thermoplastic resin lipoid microsphere whipping agent foam production to prepare, have significantly and improve, when preferably adding ratio of gas mixture to be 60%, effect is optimum, foaming thickness 8 times of thickness when not foaming, colloid is more flexible, toughness, foam size is also more even.In addition, contriver also finds, 100 ℃ of following curing moldings of the general employing of tradition preparation method, and 110-180 ℃ of hot setting moulding for the inventive method, this has also to a certain degree improved the coefficient of expansion and the speed of expansion of silica gel, improved the elastic performance of foamed silica gel, and accelerated speed of response, the high-performance silica gel that therefore prepared by method of the present invention is applicable to field more widely.
It should be noted that: above embodiment is only unrestricted in order to the present invention to be described, the present invention is also not limited in above-mentioned giving an example, and all do not depart from technical scheme and the improvement thereof of the spirit and scope of the present invention, and it all should be encompassed in claim scope of the present invention.
Claims (10)
1. a foaming liquid silicon rubber preparation method, comprises the steps:
1) by polysiloxane composition and reinforced filling, make basic material, be divided into two parts;
2) in portion, add the finish mix A of catalyzer wherein;
3) in another part, add inhibitor and the finish mix B of linking agent;
It is characterized in that, also comprise that step 4) mixes described material A and material B, and add weight ratio be 20-85% by air, oxygen and CO
2the mixed gas forming, preferred weight ratio is 60%, obtains foaming liquid silicon rubber finished product after being heating and curing.
2. foaming liquid silicon rubber preparation method according to claim 1, it is characterized in that, polysiloxane composition and reinforced filling silicon-dioxide that described step 1) is is (1) by general formula, after mixing with weight ratio 10:1～4, through thermal treatment and vacuum-treat, deviate from low molecular basis material, obtain basic material, wherein, described silicon-dioxide is selected from organosilazanes or silane coupling agent is made aerosil or the precipitated silica after hydrophobic is processed;
Wherein, described general formula (1) is:
R
2SiO(SiRR’O)n Si R
2
R is vinyl,
R ' and R are identical or different, are vinyl, methyl, alkyl or phenyl,
N is the polymerization degree (30≤n≤2000).
3. foaming liquid silicon rubber preparation method according to claim 2, it is characterized in that thermal treatment described in step 1) and vacuum-treat step are for keeping under 145-160 ℃ of constant temperature, first normal pressure stirred after 1.5-2.5 hour, stirred 2.0-3.5 hour in final vacuum.
4. foaming liquid silicon rubber preparation method according to claim 1, it is characterized in that, described step 2) for portion wherein adds 0.1%-0.5%(wt%), be the finish mix A of platinum complex compound catalyst of Platinic chloride and tetramethyl divinyl disiloxane polymkeric substance.
5. foaming liquid silicon rubber preparation method according to claim 4, is characterized in that, in the polymkeric substance of described Platinic chloride and tetramethyl divinyl disiloxane, platinum content is 0.32-0.38%(wt%).
6. foaming liquid silicon rubber preparation method according to claim 1, it is characterized in that, described step 3) is for adding the organic hydride polysiloxane that is not less than 3 hydrogen silicon links of general formula (2) to another part, its hydrogen content is 0.12%-1%(wt%), and 0.8%-4.5%(wt%) the finish mix B of alkynol class inhibitor, preferably, described alkynol class curing inhibitors is selected from the alkynyl-3-alcohol, 3 of 3-methyl-, and 5-dimethyl-1-is alkynyl-3-alcohol, 2-methyl-3-butynyl-2-alcohol and/or 2-phenyl-3-butynyl-2-alcohol;
Wherein, described general formula (2) is:
R
2SiO(SiRR’O)
x(SiHR’O)
ySi R
2
R is vinyl,
R ' and R are identical or different, are vinyl, methyl, alkyl or phenyl,
X and y are the polymerization degree (0≤x≤300) (3≤y≤30).
7. foaming liquid silicon rubber preparation method according to claim 1 and 2, is characterized in that, described polysiloxane composition is the composition that is selected from following polysiloxane one or more,
I. viscosity is that 5000-10000mPas (25 ℃), contents of ethylene are 0.25%-0.5%(wt%) polysiloxane;
II. viscosity is that 10000-40000mPas (25 ℃), contents of ethylene are 0.15%-0.5%(wt%) polysiloxane;
III. viscosity is that 1000-2000mPas (25 ℃), contents of ethylene are 0.3%-1.0%(wt%) polysiloxane;
IV. viscosity is that 1000-5000mPas (25 ℃), contents of ethylene are 1.0%-10%(wt%) polysiloxane.
8. foaming liquid silicon rubber preparation method according to claim 1, it is characterized in that, in described step 4), expect to add described mixed gas after A and material B mix with weight ratio 1:1,110-180 ℃ of heating obtains foaming liquid silicon rubber finished product after 3-8 minute, preferably, 3 minutes after fixing of 160 ℃ of heating obtain finished product.
9. foaming liquid silicon rubber preparation method according to claim 8, is characterized in that, described mixed gas consist of weight percent meter: 15%～25% air, 30%～40% oxygen, 40%～50%CO
2, preferred, the composition weight percent of mixed gas is counted: 20% air, 35% oxygen, 45%CO
2.
10. a foaming liquid rubber composition of preparing according to the preparation method described in any one in claim 1-9.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105331117A (en) * | 2015-11-17 | 2016-02-17 | 镇江高美新材料有限公司 | Foamed liquid silicone rubber and preparation method thereof |
| CN105602444A (en) * | 2016-03-07 | 2016-05-25 | 惠州赛力珑新材料有限公司 | Yoga mat and preparation method |
| CN105778144A (en) * | 2016-03-15 | 2016-07-20 | 惠州赛力珑新材料有限公司 | Production method for organic silicone sponge |
| CN107815288A (en) * | 2017-10-19 | 2018-03-20 | 东莞市兆科电子材料科技有限公司 | Adiabatic gum, heat shield, the preparation method of the preparation method of adiabatic gum and heat shield |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105331117A (en) * | 2015-11-17 | 2016-02-17 | 镇江高美新材料有限公司 | Foamed liquid silicone rubber and preparation method thereof |
| CN105602444A (en) * | 2016-03-07 | 2016-05-25 | 惠州赛力珑新材料有限公司 | Yoga mat and preparation method |
| CN105602444B (en) * | 2016-03-07 | 2018-05-15 | 惠州赛力珑新材料有限公司 | A kind of Yoga mat and preparation method |
| CN105778144A (en) * | 2016-03-15 | 2016-07-20 | 惠州赛力珑新材料有限公司 | Production method for organic silicone sponge |
| CN107815288A (en) * | 2017-10-19 | 2018-03-20 | 东莞市兆科电子材料科技有限公司 | Adiabatic gum, heat shield, the preparation method of the preparation method of adiabatic gum and heat shield |
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