CN105238066A - Anti-settle silicon-based wave absorption glue and preparation method thereof - Google Patents
Anti-settle silicon-based wave absorption glue and preparation method thereof Download PDFInfo
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Abstract
The invention relates to an anti-settle silicon-based wave absorption glue and a preparation method thereof. The anti-settle silicon-based wave absorption glue is prepared through mixing the following raw materials, by weight, 40-90 parts of a base material, 0.005-1 part of a coupling agent, 0.0001-0.001 parts of a platinum catalyst, 0.005 parts of an inhibitor, 3-5 parts of a fire retardant, 2-20 parts of hydrosilicone oil and 40-90 parts of a wave absorption agent. The anti-settle silicon-based wave absorption glue has the advantages of good wave absorption performance and easy processing molding, and can be widely used in aviation, spaceflight, ships and other military electronic equipment, and the fields of workstations, computers, data communication and communication equipment.
Description
Technical field
The present invention relates to a kind of glue and preparation method thereof, particularly relate to a kind of sedimentation-prevention type glue and preparation method thereof, belong to organic absorbing material field of electromagnetic shielding interface requirements.
Background technology
Microwave unreflected chamber is mainly used in the measurement of the natural impedance such as radar or communication antenna, guided missile, aircraft, airship, satellite and the degree of coupling, cosmonaut with the installation of the measurement of back shoulder antenna pattern and spaceship, test and adjustment etc., this both can eliminate extraneous noise jamming and improve measuring accuracy and efficiency (indoor can all weather operations), also can keep secret.In future high-tech, three-dimensional war, weaponry is faced with detection and the severe challenge instead detected at any time.Absorbing material is the key link in stealthy technique, and research absorbing material being introduced stealthy technique is subject to the great attention of countries in the world.
At present, the polymer base-material of the absorbing material on market mainly adopts natural rubber, urethane, nitrile rubber, isoprene-isobutylene rubber etc., but they also exist not high-low temperature resistant and the easily shortcoming such as aging; Silicon materials not only high-low temperature resistant are good, and the advantage such as ageing-resistant, corrosion-resistant, radiation hardness, have report silica-base material as shielding material, but shaping cumbersome, need equipment costly.Being prepared into suction ripple glue is feasible method, but inhales ripple powder free settling in glue, brings and stores inconvenience.
Summary of the invention
The present invention is directed to the deficiency that existing absorbing material exists, a kind of sedimentation-prevention type silica-based suction ripple glue and preparation method thereof is provided.
The technical scheme that the present invention solves the problems of the technologies described above is as follows:
A kind of sedimentation-prevention type silica-based suction ripple glue, is characterized in that, by the raw material of following weight part through mixing
Obtained:
Described base-material dewaters blended obtained by vinyl silicone oil 80 ~ 120 parts, thermal silica 10 ~ 30 parts, hexamethyldisilazane 3 ~ 8 parts with distilled water 0.2 ~ 1 part;
Described modification wave absorbing agent refers to that Surface coating has the wave absorbing agent of coupling agent.
Further, described vinyl silicone oil refers to the silicone liquid glue containing vinyl, and the molecular weight of silicone liquid glue is 1 ~ 50w.
Further, described wave absorbing agent is metallic iron micro mist, polycrystalline iron fiber, and ferrite and any one or a few the mixture inhaled in ripple silicon carbide, wave absorbing agent diameter of particle size is 10 ~ 200 μm.
Further, described containing hydrogen silicone oil refers to one or more the mixture in methyl hydrogen silicone oil, phenyl hydrogen-containing silicon oil, hydroxyl hydrogen silicone oil.
Further, described inhibitor is the one in 2-methyl-3-butynyl-2 alcohol, 3-methyl isophthalic acid-ethynyl-3-alcohol, 3,5-dimethyl-1-hexin base-3-alcohol and 1-ethynyl-1-hexalin.
Further, described fire retardant is a kind of in magnesium hydroxide or aluminium hydroxide or both mixtures.
Further, described coupling agent is one or both and above mixture in silane coupling A-174, A-171, A-186, titanate coupling agent KR-TTS.
The invention has the beneficial effects as follows:
1) sedimentation-prevention type of the present invention silica-based suction ripple glue, has stable storage, has excellent electric and physical property, the performance such as weathering resistance, high-low temperature resistant after sulfuration completely;
2) sedimentation-prevention type of the present invention silica-based suction ripple glue has good absorbing property, easy machine-shaping, can be widely used in the Military Electronic Equipment such as Aeronautics and Astronautics, naval vessel, workstation, computer, the field such as data communication and signal equipment.
The preparation method of the present invention's also claimed above-mentioned sedimentation-prevention type silica-based suction ripple glue, comprises the steps:
1) wave absorbing agent is dry: by wave absorbing agent powder drying removing moisture;
2) wave absorbing agent is coated: to step 1) in gained powder adopt wet method carry out surface treatment, by coupling agent with 95% ethanolic soln mix, make it be hydrolyzed, then wave absorbing agent powder is added wherein, gained mixture is after being fully uniformly mixed, ethanol volatilizees by heating in water bath, obtains the wave absorbing agent of Surface coating last layer coupling agent, i.e. modification wave absorbing agent;
3) prepare sedimentation-prevention type base-material: be placed in vacuum kneader by vinyl silicone oil 80 ~ 120 parts, thermal silica 10 ~ 30 parts, hexamethyldisilazane 3 ~ 8 parts and distilled water 0.2 ~ 1 part, in 100 ~ 150 DEG C, dewater under the condition of pressure ﹤ 0.01Mpa blended sedimentation-prevention type base-material;
4) mix: join in double planetary mixer after the raw material of following weight part is mixed and mix, sedimentation-prevention type base-material: 40 ~ 90 parts; Coupling agent: 0.005 ~ 1 part; Platinum catalyst: 0.0001 ~ 0.001 part; Inhibitor: 0.005 part; Fire retardant: 3 ~ 5 parts; Containing hydrogen silicone oil: 2 ~ 20 parts; Wave absorbing agent: 40 ~ 90 parts, obtains sedimentation-prevention type silica-based suction ripple glue;
5) shaping: by step 4) in the suction ripple glue of gained inject difform fixture, at 120 ~ 150 DEG C, solidify 20 ~ 40min, cooling, stripping forming.
Further, step 1) and 2) described in wave absorbing agent be metallic iron micro mist, polycrystalline iron fiber, ferrite and any one or a few the mixture inhaled in ripple silicon carbide.
Further, step 3) described in the molecular weight of silicone liquid glue silicone liquid glue that refers to containing vinyl of vinyl silicone oil be 1 ~ 50w.
Further, step 2) described in coupling agent and 95% ethanolic soln mixture in coupling agent account for 2 ~ 10wt%, coupling agent is 0.5 ~ 2wt% of wave absorbing agent weight.
Further, step 4) described in containing hydrogen silicone oil refer to one or more mixture in methyl hydrogen silicone oil, phenyl hydrogen-containing silicon oil, hydroxyl hydrogen silicone oil.
Further, step 2) and 4) described in coupling agent be one or both and above mixture in silane coupling A-174, A-171, A-186, titanate coupling agent KR-TTS.
Further, step 4) described in fire retardant be a kind of in magnesium hydroxide or aluminium hydroxide or both mixtures.
Further, step 4) described in inhibitor be one in 2-methyl-3-butynyl-2 alcohol, 3-methyl isophthalic acid-ethynyl-3-alcohol, 3,5-dimethyl-1-hexin base-3-alcohol and 1-ethynyl-1-hexalin.The beneficial effect of the preparation method of sedimentation-prevention type of the present invention silica-based suction ripple glue is as follows:
1) technical process is simple, raw materials used cheap and easy to get, is easy to realize;
2) products obtained therefrom has stable storage, has excellent electric and physical property, the performance such as weathering resistance, high-low temperature resistant after sulfuration completely.
Embodiment
Be described principle of the present invention and feature below in conjunction with example, example, only for explaining the present invention, is not intended to limit scope of the present invention.
Embodiment 1:
A kind of sedimentation-prevention type silica-based suction ripple glue, obtained through mixing by the raw material of following weight part: base-material: 60 parts, silane coupling A-174:0.5 part, platinum catalyst: 0.0006 part, 1-ethynyl-1-hexalin: 0.005 part, magnesium hydroxide: 4 parts, methyl hydrogen silicone oil: 15 parts, the modified metal iron micro mist of 10-30um: 60 parts, described base-material is the vinyl silicone oil of 1 ~ 15w by molecular weight: 100 parts, particle diameter is the thermal silica of 10 ~ 30nm: 20 parts, hexamethyldisilazane: 6 parts, distilled water: 0.6 part of dehydration is blended obtained.
The preparation method of above-mentioned sedimentation-prevention type silica-based suction ripple glue is as follows:
1) wave absorbing agent is dry, and the metallic iron micro mist getting 10-30um to be placed in air dry oven at 80 DEG C dry 1 hour;
2) wave absorbing agent is coated, to step 1) in the metallic iron micro mist of gained carry out wet process surface treatment, by silane coupling A-174 with 95% ethanolic soln mix and make it be hydrolyzed 30min, wherein by weight, silane coupling A-174 accounts for 5wt%, afterwards metallic iron micro mist is joined silane coupling A-174 with the mixing solutions of ethanol, silane coupling A-174 is the 1wt% of iron micropowder weight, after being fully uniformly mixed 30min, being placed in 80 DEG C of water-baths heats ethanol evaporation, obtains the modified metal iron micro mist of Surface coating last layer coupling agent;
3) prepare sedimentation-prevention type base-material: be the vinyl silicone oil 100 parts of 1 ~ 15w by molecular weight, particle diameter is the thermal silica 20 parts of 10 ~ 30nm, hexamethyldisilazane 6 parts is placed in vacuum kneader with distilled water 0.6 part, in 100 DEG C, dewater under the condition of pressure 0.006Mpa blended sedimentation-prevention type base-material;
4) mix: join in double planetary mixer after the raw material of following weight part is mixed and mix, sedimentation-prevention type base-material: 60 parts; Silane coupling A-174:0.5 part; Platinum catalyst: 0.0006 part; 1-ethynyl-1-hexalin: 0.005 part; Magnesium hydroxide: 4 parts; Methyl hydrogen silicone oil: 15 parts; Step 2) in the modified metal iron micro mist of gained: 60 parts, be uniformly mixed 1 hour and obtain sedimentation-prevention type silica-based suction ripple glue;
5) by step 4) in the suction ripple glue of gained inject difform fixture, at 130 DEG C, solidify 30min, cooling, stripping forming.
Embodiment 2:
A kind of sedimentation-prevention type silica-based suction ripple glue, obtained through mixing by the raw material of following weight part: base-material: 40 parts, titanate coupling agent KR-TTS:0.02 part, platinum catalyst: 0.0002 part, 1-ethynyl-1-hexalin: 0.005 part; Magnesium hydroxide: 5 parts, methyl hydrogen silicone oil: 10 parts, the metallic iron micro mist of 10 ~ 30um: 40 parts, described base-material is the vinyl silicone oil of 1 ~ 15w by molecular weight: 80 parts, particle diameter is the thermal silica of 10 ~ 30nm: 15 parts, hexamethyldisilazane: 5 parts, distilled water: 0.4 part of dehydration is blended obtained.
The preparation method of above-mentioned sedimentation-prevention type silica-based suction ripple glue is as follows:
1) wave absorbing agent is dry, and the metallic iron micro mist getting 10 ~ 30um to be placed in air dry oven at 80 DEG C dry 1 hour;
2) wave absorbing agent is coated, to step 1) in the metallic iron micro mist of gained carry out wet process surface treatment, by silane coupling A-171 with 95% ethanolic soln mix and make it be hydrolyzed 30min, wherein by weight, A-171 accounts for 8wt%, afterwards metallic iron micro mist is joined in the mixing solutions of A-171 and ethanol, A-171 is the 1wt% of iron micropowder weight, after being fully uniformly mixed 40min, being placed in 80 DEG C of water-baths heats ethanol evaporation, obtains the modified metal iron micro mist of Surface coating last layer coupling agent A-171;
3) prepare sedimentation-prevention type base-material: be the vinyl silicone oil 80 parts of 1 ~ 15w by molecular weight, particle diameter is the thermal silica 15 parts of 10 ~ 30nm, hexamethyldisilazane 5 parts is placed in vacuum kneader with distilled water 0.4 part, in 120 DEG C, dewater under the condition of pressure 0.005Mpa blended sedimentation-prevention type base-material;
4) mix: join in double planetary mixer after the raw material of following weight part is mixed and mix, sedimentation-prevention type base-material: 80 parts; Titanate coupling agent KR-TTS:0.02 part; Platinum catalyst: 0.0002 part; 1-ethynyl-1-hexalin: 0.005 part; Magnesium hydroxide: 5 parts; Methyl hydrogen silicone oil: 10 parts; Step 2) in the iron micro mist of gained: 80 parts, be uniformly mixed 1 hour and obtain sedimentation-prevention type silica-based suction ripple glue;
5) by step 4) in the suction ripple glue of gained inject difform fixture, at 120 DEG C, solidify 40min, cooling, stripping forming.
Embodiment 3:
A kind of sedimentation-prevention type silica-based suction ripple glue, obtained through mixing by the raw material of following weight part: base-material: 90 parts, silane coupling A-171:1 part, platinum catalyst: 0.0001 part, 2-methyl-3-butynyl-2 alcohol: 0.005 part, aluminium hydroxide: 5 parts, phenyl hydrogen-containing silicon oil: 20 parts, the polycrystalline iron fiber of 30 ~ 50um: 90 parts, described base-material is the vinyl silicone oil of 15 ~ 30w by molecular weight: 120 parts, particle diameter is the thermal silica of 30 ~ 50nm: 30 parts, hexamethyldisilazane: 8 parts, distilled water: 1 part of dehydration is blended obtained.
The preparation method of above-mentioned sedimentation-prevention type silica-based suction ripple glue is as follows:
1) wave absorbing agent is dry, and the polycrystalline iron fiber getting 30 ~ 50um to be placed in air dry oven at 80 DEG C dry 1 hour;
2) wave absorbing agent is coated, to step 1) in the polycrystalline iron fiber of gained carry out wet process surface treatment, by silane coupling A-171 with 95% ethanolic soln mix and make it be hydrolyzed 30min, wherein by weight, coupling agent accounts for 10wt%, afterwards polycrystalline iron fiber is joined silane coupling A-171 with the mixing solutions of ethanol, silane coupling A-171 is the 0.5wt% of polycrystalline iron fiber weight, after being fully uniformly mixed 30min, being placed in 80 DEG C of water-baths heats ethanol evaporation, obtain the modification polycrystalline iron fiber of Surface coating last layer silane coupling A-171,
3) prepare sedimentation-prevention type base-material: be that thermal silica 30 parts, the hexamethyldisilazane 8 parts of 30 ~ 50nm is placed in vacuum kneader with distilled water 1 part by vinyl silicone oil 120 parts, particle diameter, in 150 DEG C, dewater under the condition of pressure 0.005Mpa blended sedimentation-prevention type base-material;
4) mix: join in double planetary mixer after the raw material of following weight part is mixed and mix, sedimentation-prevention type base-material: 90 parts; Silane coupling A-171:1 part; Platinum catalyst: 0.0001 part; 2-methyl-3-butynyl-2 alcohol: 0.005 part, aluminium hydroxide: 5 parts; Phenyl hydrogen-containing silicon oil: 20 parts; Step 2) in the polycrystalline iron fiber of gained: 90 parts, mix and blend obtains sedimentation-prevention type silica-based suction ripple glue for 1 hour;
5) by step 4) in the suction ripple glue of gained inject difform fixture, at 130 DEG C, solidify 30min, cooling, stripping forming.
Embodiment 4:
A kind of sedimentation-prevention type silica-based suction ripple glue, obtained through mixing by the raw material of following weight part: base-material: 40 parts, silane coupling A-186:0.005 part, platinum catalyst: 0.0001 part, 2-methyl-3-butynyl-2 alcohol: 0.005 part, magnesium hydroxide: 3 parts, hydroxyl hydrogen silicone oil: 2 parts, the ferrite of 30 ~ 50um: 60 parts, described base-material is the vinyl silicone oil of 15 ~ 30w by molecular weight: 80 parts, particle diameter is the thermal silica of 30 ~ 50nm: 10 parts, hexamethyldisilazane: 3 parts, distilled water: 0.2 part of dehydration is blended obtained.
The preparation method of above-mentioned sedimentation-prevention type silica-based suction ripple glue is as follows:
1) wave absorbing agent is dry, and the ferrite getting 30 ~ 50um to be placed in air dry oven at 80 DEG C dry 1 hour;
2) wave absorbing agent is coated, to step 1) in the ferrite of gained carry out wet process surface treatment, by titanate coupling agent KR-TTS with 95% ethanolic soln mix and make it be hydrolyzed 30min, wherein by weight, titanate coupling agent KR-TTS accounts for 5wt%, afterwards ferrite is joined in the mixing solutions of titanate coupling agent KR-TTS and ethanol, titanate coupling agent KR-TTS is the 0.5wt% of ferrite weight, after being fully uniformly mixed 30min, being placed in 80 DEG C of water-baths heats ethanol evaporation, obtain the Modified Iron oxysome of Surface coating last layer titanate coupling agent KR-TTS,
3) prepare sedimentation-prevention type base-material: be that thermal silica 10 parts, the hexamethyldisilazane 3 parts of 30 ~ 50nm is placed in vacuum kneader with distilled water 0.2 part by vinyl silicone oil 80 parts, particle diameter, in 130 DEG C, dewater under the condition of pressure 0.002Mpa blended sedimentation-prevention type base-material;
4) mix: join in double planetary mixer after the raw material of following weight part is mixed and mix, sedimentation-prevention type base-material: 40 parts, silane coupling A-186:0.005 part, platinum catalyst: 0.0001 part, 2-methyl-3-butynyl-2 alcohol: 0.005 part, magnesium hydroxide: 3 parts, hydroxyl hydrogen silicone oil: 2 parts, step 2) in gained ferrite: 60 parts, be uniformly mixed 1 hour and obtain sedimentation-prevention type silica-based suction ripple glue;
5) by step 4) in the suction ripple glue of gained inject difform fixture, at 120 DEG C, solidify 40min, cooling, stripping forming.
Embodiment 5:
A kind of sedimentation-prevention type silica-based suction ripple glue, obtained through mixing by the raw material of following weight part: base-material: 40 parts, titanate coupling agent KR-TTS:1 part, platinum catalyst: 0.001 part, 3-methyl isophthalic acid-ethynyl-3-alcohol: 0.005 part, aluminium hydroxide: 4 parts, methyl hydrogen silicone oil: 20 parts, the suction ripple silicon carbide of 30 ~ 50um: 90 parts, described base-material is the vinyl silicone oil of 30 ~ 50w by molecular weight: 100 parts, particle diameter is the thermal silica of 30 ~ 50nm: 10 parts, hexamethyldisilazane: 6 parts, distilled water: 0.4 part of dehydration is blended obtained.
The preparation method of above-mentioned sedimentation-prevention type silica-based suction ripple glue is as follows:
1) wave absorbing agent is dry, and the suction ripple silicon carbide getting 30 ~ 50um to be placed in air dry oven at 80 DEG C dry 1 hour;
2) wave absorbing agent is coated, to step 1) in the suction ripple silicon carbide of gained carry out wet process surface treatment, by titanate coupling agent KR-TTS with 95% ethanolic soln mix and make it be hydrolyzed 30min, wherein by weight, titanate coupling agent KR-TTS accounts for 4wt%, afterwards suction ripple silicon carbide is joined in the mixing solutions of titanate coupling agent KR-TTS and ethanol, titanate coupling agent KR-TTS is the 0.5wt% inhaling ripple silicon carbide weight, after being fully uniformly mixed 30min, being placed in 80 DEG C of water-baths heats ethanol evaporation, ripple silicon carbide is inhaled in the modification obtaining Surface coating last layer titanate coupling agent KR-TTS,
3) prepare sedimentation-prevention type base-material: be the vinyl silicone oil 100 parts of 30 ~ 50w by molecular weight, particle diameter is the thermal silica 10 parts of 30 ~ 50nm, hexamethyldisilazane 6 parts is placed in vacuum kneader with distilled water 0.4 part, in 120 DEG C, dewater under the condition of pressure 0.002Mpa blended sedimentation-prevention type base-material;
4) mix: join in double planetary mixer after the raw material of following weight part is mixed and mix, sedimentation-prevention type base-material: 40 parts, titanate coupling agent KR-TTS:1 part, platinum catalyst: 0.001 part, 3-methyl isophthalic acid-ethynyl-3-alcohol: 0.005 part, aluminium hydroxide: 4 parts, methyl hydrogen silicone oil: 20 parts, step 2) in the suction ripple silicon carbide of gained: 90 parts, be uniformly mixed 1 hour and obtain sedimentation-prevention type silica-based suction ripple glue;
5) by step 4) in the suction ripple glue of gained inject difform fixture, at 130 DEG C, solidify 40min, cooling, stripping forming.
Embodiment 6:
A kind of sedimentation-prevention type silica-based suction ripple glue, obtained through mixing by the raw material of following weight part: base-material: 60 parts, silane coupling A-174:0.005 part, platinum catalyst: 0.0001 part, 3-methyl isophthalic acid-ethynyl-3-alcohol: 0.005 part, aluminium hydroxide: 3 parts, hydroxyl hydrogen silicone oil: 2 parts, the metallic iron micro mist of 50 ~ 100um: 40 parts, described base-material is the vinyl silicone oil of 30 ~ 50w by molecular weight: 120 parts, particle diameter is the thermal silica of 50 ~ 80nm: 10 parts, hexamethyldisilazane: 3 parts, distilled water: 1 part of dehydration is blended obtained.
The preparation method of above-mentioned sedimentation-prevention type silica-based suction ripple glue is as follows:
1) wave absorbing agent is dry, and the metallic iron micro mist getting 50 ~ 100um to be placed in air dry oven at 80 DEG C dry 1 hour;
2) wave absorbing agent is coated, to step 1) in the metallic iron micro mist of gained carry out wet process surface treatment, by silane coupling A-174 with 95% ethanolic soln mix and make it be hydrolyzed 30min, wherein by weight, silane coupling A-174 accounts for 5wt%, afterwards metallic iron micro mist is joined silane coupling A-174 with the mixing solutions of ethanol, silane coupling A-174 is the 2wt% of metallic iron micropowder weight, after being fully uniformly mixed 30min, being placed in 80 DEG C of water-baths heats ethanol evaporation, obtain the modified metal iron micro mist of Surface coating last layer silane coupling A-174,
3) prepare sedimentation-prevention type base-material: be the vinyl silicone oil 120 parts of 30 ~ 50w by molecular weight, particle diameter is the thermal silica 10 parts of 50 ~ 80nm, hexamethyldisilazane 3 parts is placed in vacuum kneader with distilled water 1 part, in 100 DEG C, dewater under the condition of pressure 0.006Mpa blended sedimentation-prevention type base-material;
4) mix: join in double planetary mixer after the raw material of following weight part is mixed and mix, sedimentation-prevention type base-material: 60 parts, silane coupling A-174:0.005 part, platinum catalyst: 0.0001 part, 3-methyl isophthalic acid-ethynyl-3-alcohol: 0.005 part, aluminium hydroxide: 3 parts, hydroxyl hydrogen silicone oil: 2 parts, step 2) in gained metallic iron micro mist: 40 parts, be uniformly mixed 1 hour and obtain sedimentation-prevention type silica-based suction ripple glue;
5) by step 4) in the suction ripple glue of gained inject difform fixture, at 130 DEG C, solidify 30min, cooling, stripping forming.
Embodiment 7:
A kind of sedimentation-prevention type silica-based suction ripple glue, obtained through mixing by the raw material of following weight part: base-material: 60 parts, titanate coupling agent KR-TTS:1 part, platinum catalyst: 0.001 part, 3,5-dimethyl-1-hexin base-3-alcohol: 0.005 part, magnesium hydroxide: 5 parts, methyl hydrogen silicone oil: 20 parts, the suction ripple silicon carbide of 100 ~ 150um: 90 parts, described base-material is the vinyl silicone oil of 30 ~ 50w by molecular weight: 80 parts, particle diameter is the thermal silica of 50 ~ 80nm: 30 parts, hexamethyldisilazane: 5 parts, distilled water: 0.2 part of dehydration is blended obtained.
The preparation method of above-mentioned sedimentation-prevention type silica-based suction ripple glue is as follows:
1) wave absorbing agent is dry, and the suction ripple silicon carbide getting 100 ~ 150um to be placed in air dry oven at 80 DEG C dry 1 hour;
2) wave absorbing agent is coated, to step 1) in the suction ripple silicon carbide of gained carry out wet process surface treatment, by titanate coupling agent KR-TTS with 95% ethanolic soln mix and make it be hydrolyzed 30min, wherein by weight, titanate coupling agent KR-TTS accounts for 2wt%, afterwards suction ripple silicon carbide is joined in the mixing solutions of titanate coupling agent KR-TTS and ethanol, titanate coupling agent KR-TTS is the 2wt% inhaling ripple silicon carbide weight, after being fully uniformly mixed 30min, being placed in 80 DEG C of water-baths heats ethanol evaporation, ripple silicon carbide is inhaled in the modification obtaining Surface coating last layer coupling agent,
3) prepare sedimentation-prevention type base-material: be the vinyl silicone oil 80 parts of 30 ~ 50w by molecular weight, particle diameter is the thermal silica 20 parts of 50 ~ 80nm, hexamethyldisilazane 5 parts is placed in vacuum kneader with distilled water 0.2 part, in 140 DEG C, dewater under the condition of pressure 0.006Mpa blended sedimentation-prevention type base-material;
4) mix: join in double planetary mixer after the raw material of following weight part is mixed and mix, sedimentation-prevention type base-material: 60 parts, titanate coupling agent KR-TTS:1 part, platinum catalyst: 0.001 part, 3,5-dimethyl-1-hexin base-3-alcohol: 0.005 part, magnesium hydroxide: 5 parts, methyl hydrogen silicone oil: 20 parts, step 2) in the suction ripple silicon carbide of gained: 90 parts, be uniformly mixed 1 hour and obtain sedimentation-prevention type silica-based suction ripple glue;
5) by step 4) in the suction ripple glue of gained inject difform fixture, at 140 DEG C, solidify 30min, cooling, stripping forming.
Embodiment 8:
A kind of sedimentation-prevention type silica-based suction ripple glue, obtained through mixing by the raw material of following weight part: base-material: 90 parts, silane coupling A-171:1 part, platinum catalyst: 0.001 part, 3,5-dimethyl-1-hexin base-3-alcohol: 0.005 part, aluminium hydroxide: 3 parts, phenyl hydrogen-containing silicon oil: 15 parts, the polycrystalline iron fiber of 150 ~ 200um: 60 parts, described base-material is the vinyl silicone oil of 30 ~ 50w by molecular weight: 120 parts, particle diameter is the thermal silica of 50 ~ 80nm: 10 parts, hexamethyldisilazane: 3 parts, distilled water: 1 part of dehydration is blended obtained.
The preparation method of above-mentioned sedimentation-prevention type silica-based suction ripple glue is as follows:
1) wave absorbing agent is dry, and the polycrystalline iron fiber getting 150 ~ 200um to be placed in air dry oven at 80 DEG C dry 1 hour;
2) wave absorbing agent is coated, to step 1) in the polycrystalline iron fiber of gained carry out wet process surface treatment, by silane coupling A-171 with 95% ethanolic soln mix and make it be hydrolyzed 30min, wherein by weight, silane coupling A-171 accounts for 5wt%, afterwards polycrystalline iron fiber is joined silane coupling A-171 with the mixing solutions of ethanol, silane coupling A-171 is the 1wt% of polycrystalline iron fiber weight, after being fully uniformly mixed 30min, being placed in 80 DEG C of water-baths heats ethanol evaporation, obtains the polycrystalline iron fiber of Surface coating last layer coupling agent;
3) prepare sedimentation-prevention type base-material: be the vinyl silicone oil 120 parts of 30 ~ 50w by molecular weight, particle diameter is the thermal silica 10 parts of 50 ~ 80nm, hexamethyldisilazane 3 parts is placed in vacuum kneader with distilled water 1 part, in 100 DEG C, dewater under the condition of pressure 0.006Mpa blended sedimentation-prevention type base-material;
4) mix: join in double planetary mixer after the raw material of following weight part is mixed and mix, sedimentation-prevention type base-material: 90 parts, silane coupling A-171:1 part, platinum catalyst: 0.001 part, 3,5-dimethyl-1-hexin base-3-alcohol: 0.005 part, aluminium hydroxide: 3 parts, phenyl hydrogen-containing silicon oil: 15 parts, step 2) in the polycrystalline iron fiber of gained: 40 parts, be uniformly mixed 1 hour and obtain sedimentation-prevention type silica-based suction ripple glue;
5) by step 4) in the suction ripple glue of gained inject difform fixture, at 130 DEG C, solidify 30min, cooling, stripping forming.
Embodiment 9:
A kind of sedimentation-prevention type silica-based suction ripple glue, obtained through mixing by the raw material of following weight part: base-material: 90 parts, silane coupling A-186:0.005 part, platinum catalyst: 0.0005 part, 1-ethynyl-1-hexalin: 0.005 part, magnesium hydroxide: 4 parts, phenyl hydrogen-containing silicon oil: 2 parts, the polycrystalline iron fiber of 150 ~ 200um: 40 parts, described base-material is the vinyl silicone oil of 30 ~ 50w by molecular weight: 120 parts, particle diameter is the thermal silica of 50 ~ 80nm: 10 parts, hexamethyldisilazane: 3 parts, distilled water: 1 part of dehydration is blended obtained.
The preparation method of above-mentioned sedimentation-prevention type silica-based suction ripple glue is as follows:
1) wave absorbing agent is dry, and the polycrystalline iron fiber getting 150 ~ 200um to be placed in air dry oven at 80 DEG C dry 1 hour;
2) wave absorbing agent is coated, to step 1) in the polycrystalline iron fiber of gained carry out wet process surface treatment, by silane coupling A-186 with 95% ethanolic soln mix and make it be hydrolyzed 30min, wherein by weight, silane coupling A-186 accounts for 5wt%, afterwards polycrystalline iron fiber is joined silane coupling A-186 with the mixing solutions of ethanol, silane coupling A-186 is the 1wt% of polycrystalline iron fiber weight, after being fully uniformly mixed 30min, being placed in 80 DEG C of water-baths heats ethanol evaporation, obtains the modification polycrystalline iron fiber of Surface coating last layer coupling agent;
3) prepare sedimentation-prevention type base-material: be the vinyl silicone oil 120 parts of 30 ~ 50w by molecular weight, particle diameter is the thermal silica 10 parts of 50 ~ 80nm, hexamethyldisilazane 3 parts is placed in vacuum kneader with distilled water 1 part, in 100 DEG C, dewater under the condition of pressure 0.006Mpa blended sedimentation-prevention type base-material;
4) mix: join in double planetary mixer after the raw material of following weight part is mixed and mix, sedimentation-prevention type base-material: 90 parts, silane coupling A-186:0.005 part, platinum catalyst: 0.0005 part, 1-ethynyl-1-hexalin: 0.005 part, magnesium hydroxide: 4 parts, hydroxyl hydrogen silicone oil: 2 parts, step 2) in gained polycrystalline iron fiber: 40 parts, be uniformly mixed 1 hour and obtain sedimentation-prevention type silica-based suction ripple glue;
5) by step 4) in the suction ripple glue of gained inject difform fixture, at 130 DEG C, solidify 30min, cooling, stripping forming.
Comparative example 1:
Each component by embodiment 1: base-material: 60 parts, silane coupling A-174:0.5 part, platinum catalyst: 0.0006 part, 1-ethynyl-1-hexalin: 0.005 part, magnesium hydroxide: 4 parts, methyl hydrogen silicone oil: 15 parts, the metallic iron micro mist of 10 ~ 30um: 60 parts, join in double planetary mixer and be uniformly mixed 1 hour, described base-material is the vinyl silicone oil of 1 ~ 15w by molecular weight: 100 parts, particle diameter is the thermal silica of 10 ~ 30nm: 20 parts, mixing is obtained.
Comparative example 2:
Each component by embodiment 2: base-material: 80 parts, titanate coupling agent KR-TTS:0.02 part, platinum catalyst: 0.0002 part, 1-ethynyl-1-hexalin: 0.005 part, magnesium hydroxide: 5 parts, methyl hydrogen silicone oil: 10 parts, the iron micro mist of 10 ~ 30um: 80 parts, join in double planetary mixer and be uniformly mixed 1 hour, described base-material is the vinyl silicone oil of 1 ~ 15w by molecular weight: 100 parts, particle diameter is the thermal silica of 10 ~ 30nm: 20 parts of mixing are obtained.
Comparative example 3:
Each component by embodiment 3: base-material: 90 parts, silane coupling A-171:1 part, platinum catalyst: 0.0001 part, 2-methyl-3-butynyl-2 alcohol: 0.005 part, aluminium hydroxide: 5 parts, phenyl hydrogen-containing silicon oil: 20 parts, the polycrystalline iron fiber of 30 ~ 50um: 90 parts, join in double planetary mixer and be uniformly mixed 1 hour, described base-material is the vinyl silicone oil of 15 ~ 30w by molecular weight: 120 parts, particle diameter is the thermal silica of 30 ~ 50nm: 30 parts of mixing are obtained.
Comparative example 4:
Each component by embodiment 4: base-material: 40 parts, silane coupling A-186:0.005 part, platinum catalyst: 0.0001 part, 2-methyl-3-butynyl-2 alcohol: 0.005 part, magnesium hydroxide: 3 parts, hydroxyl hydrogen silicone oil: 2 parts, the ferrite of 30 ~ 50um: 60 parts, join in double planetary mixer and be uniformly mixed 1 hour, described base-material is the vinyl silicone oil of 15 ~ 30w by molecular weight: 80 parts, particle diameter is the thermal silica of 30 ~ 50nm: 10 parts of mixing are obtained.
Comparative example 5:
Each component by embodiment 5: base-material: 40 parts, titanate coupling agent KR-TTS:1 part, platinum catalyst: 0.001 part, 3-methyl isophthalic acid-ethynyl-3-alcohol: 0.005 part, aluminium hydroxide: 4 parts, methyl hydrogen silicone oil: 20 parts, the suction ripple silicon carbide of 30 ~ 50um: 90 parts, join in double planetary mixer and be uniformly mixed 1 hour, described base-material is the vinyl silicone oil of 30 ~ 50w by molecular weight: 100 parts, particle diameter is the thermal silica of 30 ~ 50nm: 10 parts of mixing are obtained.
Comparative example 6:
Each component by embodiment 6: base-material: 60 parts, silane coupling A-174:0.005 part, platinum catalyst: 0.0001 part, 3-methyl isophthalic acid-ethynyl-3-alcohol: 0.005 part, aluminium hydroxide: 3 parts, hydroxyl hydrogen silicone oil: 2 parts, the metallic iron micro mist of 50 ~ 100um: 40 parts, join in double planetary mixer and be uniformly mixed 1 hour, described base-material is the vinyl silicone oil of 30 ~ 50w by molecular weight: 120 parts, particle diameter is the thermal silica of 50 ~ 80nm: 10 parts of mixing are obtained.
Comparative example 7:
Each component by embodiment 7: base-material: 60 parts, titanate coupling agent KR-TTS:1 part, platinum catalyst: 0.001 part, 3,5-dimethyl-1-hexin base-3-alcohol: 0.005 part, magnesium hydroxide: 5 parts, methyl hydrogen silicone oil: 20 parts, the suction ripple silicon carbide of 100 ~ 150um: 90 parts, join in double planetary mixer and be uniformly mixed 1 hour, described base-material is the vinyl silicone oil of 30 ~ 50w by molecular weight: 80 parts, particle diameter is the thermal silica of 50 ~ 80nm: 30 parts of mixing are obtained.
Comparative example 8:
Each component by embodiment 8: base-material: 90 parts, silane coupling A-171:1 part, platinum catalyst: 0.001 part, 3,5-dimethyl-1-hexin base-3-alcohol: 0.005 part, aluminium hydroxide: 3 parts, phenyl hydrogen-containing silicon oil: 15 parts, the polycrystalline iron fiber of 150 ~ 200um: 60 parts, join in double planetary mixer and be uniformly mixed 1 hour, described base-material is the vinyl silicone oil of 30 ~ 50w by molecular weight: 120 parts, particle diameter is the thermal silica of 50 ~ 80nm: 10 parts of mixing are obtained.
Comparative example 9:
Each component by embodiment 9: base-material: 90 parts, silane coupling A-186:0.005 part, platinum catalyst: 0.0005 part, 1-ethynyl-1-hexalin: 0.005 part, magnesium hydroxide: 4 parts, phenyl hydrogen-containing silicon oil: 2 parts, the polycrystalline iron fiber of 150 ~ 200um: 40 parts, join in double planetary mixer and be uniformly mixed 1 hour, described base-material is the vinyl silicone oil of 30 ~ 50w by molecular weight: 120 parts, particle diameter is the thermal silica of 50 ~ 80nm: 10 parts of mixing are obtained.
For verifying the performance of product of the present invention, We conducted following test:
(1) sedimentation-prevention type test
By the silica-based suction ripple glue that embodiment 1 ~ 9 and comparative example 1 ~ 9 obtain, filling with identical bucket, store 6 months at-5 ~ 0 DEG C, the change of the test the superiors and orlop viscosity, result is as shown in table 1.
(2) wave-absorbing effect test
By the silica-based suction ripple glue that embodiment 1 ~ 9 and comparative example 1 ~ 9 obtain, by the rectangular sheet at 140 DEG C of mold pressings, 30 minutes obtained thick 2mm, 120mm × 120mm, under 1GHz frequency, record its effectiveness of shielding, result is as shown in table 1.
(3) tensile strength, elongation at break and tear strength test
The silica-based absorbing material that embodiment 1 ~ 9 and comparative example 1 ~ 9 obtain is tested its tensile strength by GB/T528-1998 and GB/T529-1999, and elongation at break and tear strength, result is as shown in table 1.
(4) ageing-resistant performance test
Weathering test 1: silica-based suction ripple glue embodiment 1 ~ 9 and comparative example 1 ~ 9 obtained, by the rectangular sheet at 140 DEG C of mold pressings, 30 minutes obtained thick 2mm, 120mm × 120mm, toast 72 hours at 150 DEG C, survey its tensile strength, elongation at break and tear strength, result is as shown in table 1.
Weathering test 2: the silica-based suction ripple glue that embodiment 1 ~ 9 and comparative example 1 ~ 9 are obtained, according to GB/T7759-1996, by in 140 DEG C of mold pressings sulfuration in 30 minutes, after sample compression 25%, 70 DEG C of bakings 22 hours, survey its compression set amount, shown in result (see table 1).
According to table 1 data results, silica-based suction ripple glue prepared by the present invention has good anti-settling, wave absorbtion, and mechanical property, ageing resistance are excellent, rebound resilience good.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Table 1: embodiment 1-9 and comparative example 1-9 products obtained therefrom performance test data
Claims (10)
1. a sedimentation-prevention type silica-based suction ripple glue, is characterized in that, obtained through mixing by the raw material of following weight part:
Described base-material dewaters blended obtained by vinyl silicone oil 80 ~ 120 parts, thermal silica 10 ~ 30 parts, hexamethyldisilazane 3 ~ 8 parts with distilled water 0.2 ~ 1 part;
Described modification wave absorbing agent refers to that Surface coating has the wave absorbing agent of coupling agent.
2. a kind of sedimentation-prevention type according to claim 1 silica-based suction ripple glue, is characterized in that, described vinyl silicone oil refers to the poly-diorganosiloxane liquid glue containing vinyl, and its molecular weight is 1 ~ 50w.
3. a kind of sedimentation-prevention type according to claim 1 silica-based suction ripple glue, it is characterized in that, described wave absorbing agent is metallic iron micro mist, polycrystalline iron fiber, ferrite and any one or a few the mixture inhaled in ripple silicon carbide, wave absorbing agent diameter of particle size is 10 ~ 200 μm.
4. a kind of sedimentation-prevention type according to claim 1 silica-based suction ripple glue, it is characterized in that, described containing hydrogen silicone oil refers to the methyl hydrogen silicone oil containing siloxane bond, phenyl hydrogen-containing silicon oil, one or more mixture in hydroxyl hydrogen silicone oil, described fire retardant is a kind of in magnesium hydroxide or aluminium hydroxide or both mixtures, described coupling agent is silane coupling A-174, A-171, A-186, one or both and above mixture in titanate coupling agent KR-TTS, described inhibitor is 2-methyl-3-butynyl-2 alcohol, 3-methyl isophthalic acid-ethynyl-3-alcohol, 3, one in 5-dimethyl-1-hexin base-3-alcohol and 1-ethynyl-1-hexalin.
5. a preparation method for sedimentation-prevention type silica-based suction ripple glue, is characterized in that, comprise the steps:
1) wave absorbing agent is dry: by wave absorbing agent powder drying removing moisture;
2) wave absorbing agent is coated: to step 1) in gained powder adopt wet method carry out surface treatment, by coupling agent with 95% ethanolic soln mix, make it be hydrolyzed, then wave absorbing agent powder is added wherein, gained mixture is after being fully uniformly mixed, ethanol volatilizees by heating in water bath, obtains the wave absorbing agent of Surface coating last layer coupling agent, i.e. modification wave absorbing agent;
3) prepare sedimentation-prevention type base-material: be placed in vacuum kneader by vinyl silicone oil 80 ~ 120 parts, thermal silica 10 ~ 30 parts, hexamethyldisilazane 3 ~ 8 parts and distilled water 0.2 ~ 1 part, in 100 ~ 150 DEG C, dewater under the condition of pressure ﹤ 0.01Mpa blended sedimentation-prevention type base-material;
4) mix: join in double planetary mixer after the raw material of following weight part is mixed and mix, sedimentation-prevention type base-material: 40 ~ 90 parts; Coupling agent: 0.005 ~ 1 part; Platinum catalyst: 0.0001 ~ 0.001 part; Inhibitor: 0.005 part; Fire retardant: 3 ~ 5 parts; Containing hydrogen silicone oil: 2 ~ 20 parts; Modification wave absorbing agent: 40 ~ 90 parts, obtains sedimentation-prevention type silica-based suction ripple glue;
5) shaping: by step 4) in the suction ripple glue of gained inject difform fixture, at 120 ~ 150 DEG C, solidify 20 ~ 40min, cooling, stripping forming.
6. the preparation method of a kind of sedimentation-prevention type according to claim 5 silica-based suction ripple glue, it is characterized in that, step 1) and 2) described in wave absorbing agent be metallic iron micro mist, polycrystalline iron fiber, ferrite and any one or a few the mixture inhaled in ripple silicon carbide.
7. the preparation method of a kind of sedimentation-prevention type according to claim 5 silica-based suction ripple glue, is characterized in that, step 3) described in vinyl silicone oil refer to silicone liquid glue containing vinyl, its molecular weight is 1 ~ 50w.
8. the preparation method of a kind of sedimentation-prevention type according to claim 5 silica-based suction ripple glue, it is characterized in that, step 2) described in coupling agent and 95% ethanolic soln mixture in coupling agent account for 2 ~ 10wt%, coupling agent is 0.5 ~ 2wt% of wave absorbing agent weight.
9. the preparation method of a kind of sedimentation-prevention type according to claim 5 silica-based suction ripple glue, it is characterized in that, step 4) described in containing hydrogen silicone oil refer to one or more mixture in methyl hydrogen silicone oil, phenyl hydrogen-containing silicon oil, hydroxyl hydrogen silicone oil, described fire retardant is a kind of in magnesium hydroxide or aluminium hydroxide or both mixtures, described inhibitor is the one in 2-methyl-3-butynyl-2 alcohol, 3-methyl isophthalic acid-ethynyl-3-alcohol, 3,5-dimethyl-1-hexin base-3-alcohol and 1-ethynyl-1-hexalin.
10. the preparation method of a kind of sedimentation-prevention type silica-based suction ripple glue according to any one of claim 5-9, it is characterized in that, step 2) and 4) described in coupling agent be one or both and above mixture in silane coupling A-174, A-171, A-186, titanate coupling agent KR-TTS.
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| CN106190018A (en) * | 2016-08-08 | 2016-12-07 | 岳胜武 | Sprayable self-adhesion direct type environment-friendly silica gel glue and preparation method thereof |
| CN106433247A (en) * | 2016-09-29 | 2017-02-22 | 广东美的厨房电器制造有限公司 | Hydrophilic type anti-sedimentation far infrared wave-absorbing material and preparation method thereof |
| CN106479355A (en) * | 2016-09-29 | 2017-03-08 | 广东美的厨房电器制造有限公司 | A kind of hydrophobic type anti-settling absorbing material and preparation method thereof |
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