CN104804704A - Preparation method and applications of additive vulcanized silicon rubber used for encapsulation - Google Patents
Preparation method and applications of additive vulcanized silicon rubber used for encapsulation Download PDFInfo
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Abstract
The invention relates to a preparation method an additive vulcanized silicon rubber. The preparation method comprises following steps: vinyl-terminated polydimettIylsiloxane, micron-grade silica powder, a platinum catalyst, a tackifier, and a selectable coloring agent are mixed so as to obtain a potting adhesive A component; vinyl-terminated polydimethylsiloxane, micron-grade silica powder, nano-grade white carbon black, hydrogen-terminated polydimettIylsiloxane, dimethyl methyl hydrogen polysiloxane, and a hydrosilylation inhibitor are mixed so as to obtain a potting adhesive B component; the potting adhesive A component and the potting adhesive B component are combined at a ratio so as to obtain a hydrosilylation rapid-curing double-component potting adhesive. The invention also relates to the potting adhesive prepared via the above method, and applications of the potting adhesive.
Description
Technical field
The invention belongs to polymer Embedding Material field, particularly a kind of preparation method of addition-type silicon rubber.
Background technology
Organo-silicone rubber has excellent temperature-resistance characteristic, weathering resistance, ultraviolet light resistant, dielectric properties and heat conductivility, is suitable for very much electron device Embedding Material.In the huge expansion of this solar photovoltaic industry; silicon rubber have also been obtained fast development with the advantage of its uniqueness; its main Application Areas is the adhering and sealing of photovoltaic module framework and backboard terminal box; and the embedding of terminal box, for the application under photovoltaic products out of doors environment provides available protecting and thermal control.The stability of photovoltaic module and the development of work-ing life on photovoltaic industry have important impact; possess excellent mechanical, electric property, long service life, organic silicon potting adhesive that constructing operation is easy provide reliably lasting protection for photovoltaic junction box, play the effect of waterproof, protection against the tide, dust-proof, protection against corrosion, weather-proof anti-aging, fire-retardant and heat radiation protection.
At present, on market, photovoltaic module joint sealant comprises condensed type and Si―H addition reaction type.Condensed type joint sealant is moisture-curable, humidity can improve curing speed, have that adhesiveproperties is better, cost is low, catalyzer can not be poisoning etc. advantage, but have when there is solidification that small molecules produces, curing speed is slow, intensity is relatively poor and the problem such as shrinking percentage is larger.The curing mechanism of add-on type joint sealant is Si―H addition reaction, it is made up of A, B two portions liquid ingredient, belong to mobility liquid, curing speed is fast and evenly, can deep cure, has nothing to do with the thickness of embedding and the tightness of environment, solidification is accelerated under room temperature or high temperature, produce without small molecules, form flexible elastomer after solidification, solidify material can be eliminated and impacts and shake the stress produced within the scope of larger temperature and humidity; There is excellent dielectric, fire-retardant, heat conduction and water resistance.
DOW CORNING PV-7321 condensed type joint sealant, adhesive property is excellent, price is low and there is not the problems such as poisoning of catalyst, but palpus self-vulcanizing 72h, shore hardness (Shore A) is 31, cure shrinkage is also larger, the photovoltaic module process-cycle can be made elongated, and the string stress easy butted line box device that after solidification, temperature variation causes causes damage.Chinese patent CN 103073893A describes a kind of terminal box embedding silicon rubber, possesses good mechanical property and high thermal conductivity (0.4-0.9W/m.K), but shrinking percentage comparatively large (0.20-0.40%).At DOW CORNING Sylgard 160 add-on type terminal box joint sealant 100 DEG C, 10min is curable, but blending viscosity slightly high (6400mPa.s), dielectric strength is on the low side (19kV/mm).Liquid embedding composition describing a kind of dual composition addition type silicon rubber and preparation method thereof in Chinese patent CN 101418123A, obtain the joint sealant of excellent performance, but to its viscosity and operability not mentioned, and solidification value (150 DEG C) is too high, butted line box material and internal component destruction to a certain degree may be caused.
Summary of the invention
The preparation method of the two component joint sealant of the Si―H addition reaction type fast setting that the object of the present invention is to provide a kind of low viscosity, high heat conduction, low-thermal-expansion and height to insulate, utilize vinyl polysiloxane and hydrogen based polysiloxane, under platinum catalyst effect, addition reaction of silicon with hydrogen occurs, forming materials is solidified, through the acting in conjunction of reinforced filling, tackifier etc., reach the target improving its rheological, thermal conductivity, shrinkability and insulating property.For reaching above-mentioned target; the present invention improves the performance of existing market product by formulating of recipe and functional additive; according to the curing mechanism of addition reaction of silicon with hydrogen consider vinyl silicone oil, reinforced filling, Silicon Containing Hydrogen wet goods basic material kind screening and proportioning; add tackifier and improve adhesive property; obtain that the operation of viscosity low, constructability, solidification rate are fast, excellent in mechanical performance, high heat conduction, low-thermal-expansion and high breakdown strength dual composition addition type silicon rubber, for photovoltaic junction box provides reliably lasting protection.
Technical scheme of the present invention provides a kind of preparation method of addition-type silicon rubber, comprises following steps:
1) ethenyl blocking polydimethyl siloxane fluid, micron silicon micro mist, platinum catalyst, tackifier are mixed according to mass ratio 100:25.00-40.00:0.66-0.90:0.04-0.20, after stirring and evenly mixing, sealing is preserved, and obtains joint sealant component A;
2) ethenyl blocking polydimethyl siloxane fluid, micron silicon micro mist, nano-scale white carbon black, hydrogen base end-blocking polydimethyl siloxane fluid, dimethyl methylhydrogenpolysi,oxane, addition reaction of silicon with hydrogen inhibitor are mixed according to mass ratio 70.00-86.00:25.00-40.00:0.40-0.60:11.81-28.60:0.68-2.74: 0.30-0.75, after stirring and evenly mixing, sealing is preserved, and obtains joint sealant B component;
3) by joint sealant component A and joint sealant B component according to 1:0.5-2 mass ratio with the use of, obtain the two component joint sealant of Si―H addition reaction type fast setting;
Wherein, described tackifier are selected from the silane coupling agent of not sulfur-bearing, nitrogen element; Described platinum catalyst is selected from platinum title complex; Described addition reaction of silicon with hydrogen inhibitor is selected from the organic compound containing alkynyl.
In the inventive solutions, platinum catalyst plays the effect that catalyzing addition reaction of silicon with hydrogen occurs; Tackifier are commercially available not sulfur-bearing, nitrogen element silane coupling agent on the market, play the effect increasing adhesive property; Addition reaction of silicon with hydrogen inhibitor is the compound containing alkynyl, plays the effect of set time when extending preservation period, control use.
According to the preparation method that technique scheme provides, in some embodiments, the contents of ethylene of ethenyl blocking polydimethyl siloxane fluid is 0.2-0.42wt%, and the contents of ethylene of described ethenyl blocking polydimethyl siloxane fluid is 0.16-0.31wt%.In some embodiments, described hydrogen base end-blocking polydimethyl siloxane fluid hydrogen content is 0.05-0.10wt%.Described dimethyl methylhydrogenpolysi,oxane hydrogen content is 0.34-0.67wt% in some embodiments.
In certain embodiments of the present invention, platinum catalyst is the silicon oil solution of divinyl tetramethyl disiloxane platinum title complex, and wherein platinum content is 1000-5000ppm.
In some embodiments of the present invention, the rotating speed of described stirring and evenly mixing is 2000-5000rpm.
In certain embodiments of the present invention, nano-scale white carbon black is the hydrophobic gas-phase silica of H15 type of German Wa Ke company, and specific surface area is 150m
2/ g.
In certain embodiments of the present invention, tackifier are γ-methacryloxypropyl trimethoxy silane, i.e. general trade mark KH570 silane coupling agent.
Root in certain embodiments of the present invention, step 2) described in ethenyl blocking polydimethylsiloxane, micron silicon micro mist, nano-scale white carbon black, hydrogen base end-blocking polydimethyl siloxane fluid, dimethyl methylhydrogenpolysi,oxane, addition reaction of silicon with hydrogen inhibitor weight ratio be 70.00-86.00:25.00-40.00:0.40-0.60:11.81-28.60:0.68-2.74: 0.30-0.75.
In certain embodiments of the present invention, step 1) or step 2) in micron silicon micro mist to be particle diameter the be silicon-dioxide of 3-10 μm.
In certain embodiments of the present invention, described addition reaction of silicon with hydrogen inhibitor is the silicon oil solution of the ethynylcyclohexanol of massfraction 0.5-5%.
According to the preparation method that technique scheme of the present invention provides, in some embodiments, step 1) in, the component of mixing is also comprising toner, and described tinting material is selected from micron-sized inorganic powder dyestuff; The mass ratio of tinting material and ethenyl blocking polydimethyl siloxane fluid is 0.80-1.85:100.
In certain embodiments of the present invention, tinting material to be particle diameter the be carbon black of 5-20 μm.
Another technical scheme of the present invention provides a kind of preparation-obtained addition-type silicon rubber of method provided according to preceding solution.
Another technical scheme of the present invention provide preparation method that preceding solution provides and the addition-type silicon rubber prepared according to preceding method for the application in electron pouring sealant.
By step 1) and step 2) obtain A and B component according to 1:0.5-2 mass ratio with the use of, obtain photovoltaic junction box embedding addition-type silicon rubber of the present invention.During use, A and B component are mixed according to the volume ratio of 1:1 or mass ratio, pour into needing the position of embedding, the possibility adding gas should be considered in mixing and dosing technology, under the condition of <100 millibar, carry out vacuum-treat if desired remove bubble, normal temperature or middle temperature (50-75 DEG C) solidification, obtain a kind of pliable and tough elastomerics, complete solidification process.
Above-mentioned organic silicon electronic potting adhesive can be used as solar photovoltaic assembly packaged material, can be widely used in the fields such as photovoltaic generation, new-energy automobile and electronic product.
The present invention has following advantage and effect relative to prior art:
1. the present invention utilizes low-viscosity vinyl silicone oil and containing hydrogen silicone oil respectively as base glue and linking agent, coordinate the high activated catalyst of suitable proportion and the interaction of addition reaction of silicon with hydrogen inhibitor, carry out joining glue, obtain the organic silicon potting adhesive of viscosity low (2400-2850mPa.s), longevity of service (8-16min), solidification rate fast (75 DEG C/2.4-4.0min), excellent in mechanical performance (tensile strength: 0.54-0.89MPa), constructability operation.
2. utilize the acting in conjunction of micron silica filler silicon powder and nano-scale silica filler white carbon black, reduce the viscosifying effects of filler to a great extent, improve the heat conduction of joint sealant, fire-retardant and insulating property simultaneously, obtain high heat conduction (0.30-0.39W.m
-1.K
-1), low-thermal-expansion (136*10
-6dEG C
-1-262*10
-6. DEG C
-1) and high breakdown strength (22.0-25.4KV.mm
-1) addition-type silicon rubber, improve the performance of organic silicon potting adhesive largely, for photovoltaic junction box provides reliably lasting protection.
Embodiment
The following stated be the preferred embodiment of the present invention, what the present invention protected is not limited to following preferred implementation.It should be pointed out that on the basis of conceiving in these innovation and creation for a person skilled in the art, the some distortion made and improvement, all belong to protection scope of the present invention.
Embodiment 1
Be the ethenyl blocking polydimethyl siloxane fluid of 0.21wt%, 25 mass parts silicon powders, 0.8 mass parts of carbon black, the divinyl tetramethyl disiloxane platinum title complex silicon oil solution of 0.9 mass parts 1000ppm, 0.2 mass parts γ-methacryloxypropyl trimethoxy silane mixing by 100 mass parts contents of ethylene, homogenizer is used to stir 90min with the speed of 3000rpm, seal preservation after mixing, obtain joint sealant component A;
It is the ethynylcyclohexanol silicon oil solution mixing of the ethenyl blocking polydimethylsiloxane of 0.16wt%, 25 mass parts silicon powders, 0.6 mass parts white carbon black, hydrogen base end-blocking polydimethyl siloxane fluid that 11.81 mass parts hydrogen contents are 0.05wt%, dimethyl methylhydrogenpolysi,oxane that 2.74 mass parts hydrogen contents are 0.34wt%, 0.75 mass parts 1% by 86 mass parts contents of ethylene, homogenizer is used to stir 90min with the speed of 3000rpm, seal preservation after mixing, obtain joint sealant B component;
A and B component are mixed according to the mass ratio of 1:1, to needing the position of embedding to pour into, under the condition of <100 millibar, carry out vacuum-treat remove bubble, 50 DEG C of solidifications, obtain a kind of pliable and tough elastomerics, complete solidification process.
Test: the viscosity measuring organic silicon potting adhesive according to GB/T10247-2008; According to the proportion measuring organic silicon potting adhesive under D0792 (23 DEG C) in U.S. material and test association ASTM standard; The working hour of organic silicon potting adhesive is measured according to GB/T 7123.1-2002; According to reach final mechanical property 90% set time of standard test organic silicon potting adhesive; The hardness after organic silicon potting adhesive solidification is measured according to ASTM D2240; The tensile strength after organic silicon potting adhesive solidification and elongation at break is measured according to GBT528-2009; The thermal conductivity after organic silicon potting adhesive solidification is measured according to ASTM D6343; The linear expansivity after organic silicon potting adhesive solidification is measured according to ASTM D696; The disruptive strength after organic silicon potting adhesive solidification is measured according to ASTM D149-09; Flame retardant rating after solidifying completely according to GB 10707-2008-T mensuration organic silicon potting adhesive.
Test result is in table 1.
Embodiment 2
Be the ethenyl blocking polydimethyl siloxane fluid of 0.25wt%, 30 mass parts silicon powders, 1.22 mass parts of carbon black, the divinyl tetramethyl disiloxane platinum title complex silicon oil solution of 0.66 mass parts 3000ppm, 0.08 mass parts γ-methacryloxypropyl trimethoxy silane mixing by 100 mass parts contents of ethylene, homogenizer is used to stir 120min with the speed of 2000rpm, seal preservation after mixing, obtain joint sealant component A;
It is the ethynylcyclohexanol silicon oil solution mixing of the ethenyl blocking polydimethylsiloxane of 0.19wt%, 30 mass parts silicon powders, 0.52 mass parts white carbon black, hydrogen base end-blocking polydimethyl siloxane fluid that 18.3 mass parts hydrogen contents are 0.06wt%, dimethyl methylhydrogenpolysi,oxane that 1.74 mass parts hydrogen contents are 0.40wt%, 0.4 mass parts 5% by 81 mass parts contents of ethylene, homogenizer is used to stir 120min with the speed of 2000rpm, seal preservation after mixing, obtain joint sealant B component;
A and B component are mixed according to the mass ratio of 1:0.5, to needing the position of embedding to pour into, under the condition of <100 millibar, carrying out vacuum-treat remove bubble, 60 DEG C of solidifications, obtain a kind of pliable and tough elastomerics, complete solidification process.
Use and testing method according to described in embodiment 1, gained organic silicon potting adhesive is tested, the results are shown in Table 1.
Embodiment 3
Be the ethenyl blocking polydimethyl siloxane fluid of 0.31wt%, 35 mass parts silicon powders, 1.85 mass parts of carbon black, the divinyl tetramethyl disiloxane platinum title complex silicon oil solution of 0.75 mass parts 5000ppm, 0.04 mass parts γ-methacryloxypropyl trimethoxy silane mixing by 100 mass parts contents of ethylene, homogenizer is used to stir 60min with the speed of 4000rpm, seal preservation after mixing, obtain joint sealant component A;
It is the ethynylcyclohexanol silicon oil solution mixing of the ethenyl blocking polydimethylsiloxane of 0.23wt%, 35 mass parts silicon powders, 0.56 mass parts white carbon black, hydrogen base end-blocking polydimethyl siloxane fluid that 22.8 mass parts hydrogen contents are 0.07wt%, dimethyl methylhydrogenpolysi,oxane that 0.68 mass parts hydrogen content is 0.49wt%, 0.6 mass parts 0.5% by 78 mass parts contents of ethylene, homogenizer is used to stir 60min with the speed of 4000rpm, seal preservation after mixing, obtain joint sealant B component;
A and B component are mixed according to the mass ratio of 1:2, to needing the position of embedding to pour into, under the condition of <100 millibar, carry out vacuum-treat remove bubble, 75 DEG C of solidifications, obtain a kind of pliable and tough elastomerics, complete solidification process.
Use and testing method according to described in embodiment 1, gained organic silicon potting adhesive is tested, the results are shown in Table 1.
Embodiment 4
Be the ethenyl blocking polydimethyl siloxane fluid of 0.37wt%, 40 mass parts silicon powders, 1.04 mass parts of carbon black, the divinyl tetramethyl disiloxane platinum title complex silicon oil solution of 0.48 mass parts 3000ppm, 0.12 mass parts γ-methacryloxypropyl trimethoxy silane mixing by 100 mass parts contents of ethylene, homogenizer is used to stir 90min with the speed of 3000rpm, seal preservation after mixing, obtain joint sealant component A;
It is the ethynylcyclohexanol silicon oil solution mixing of the ethenyl blocking polydimethylsiloxane of 0.27wt%, 40 mass parts silicon powders, 0.4 mass parts white carbon black, hydrogen base end-blocking polydimethyl siloxane fluid that 28.6 mass parts hydrogen contents are 0.08wt%, dimethyl methylhydrogenpolysi,oxane that 2.34 mass parts hydrogen contents are 0.58wt%, 0.3 mass parts 3% by 70 mass parts contents of ethylene, homogenizer is used to stir 90min with the speed of 3000rpm, seal preservation after mixing, obtain joint sealant B component;
A and B component are mixed according to the mass ratio of 1:1, to needing the position of embedding to pour into, under the condition of <100 millibar, carry out vacuum-treat remove bubble, 70 DEG C of solidifications, obtain a kind of pliable and tough elastomerics, complete solidification process.
Use and testing method according to described in embodiment 1, gained organic silicon potting adhesive is tested, the results are shown in Table 1.
Embodiment 5
Be the ethenyl blocking polydimethyl siloxane fluid of 0.42wt%, 35 mass parts silicon powders, 1.42 mass parts of carbon black, the divinyl tetramethyl disiloxane platinum title complex silicon oil solution of 0.7 mass parts 3000ppm, 0.16 mass parts γ-methacryloxypropyl trimethoxy silane mixing by 100 mass parts contents of ethylene, use homogenizer stirs 30min with the speed of 5000, seal preservation after mixing, obtain joint sealant component A;
It is the ethynylcyclohexanol silicon oil solution mixing of the ethenyl blocking polydimethylsiloxane of 0.31wt%, 35 mass parts silicon powders, 0.46 mass parts white carbon black, hydrogen base end-blocking polydimethyl siloxane fluid that 25.3 mass parts hydrogen contents are 0.10wt%, dimethyl methylhydrogenpolysi,oxane that 1.04 mass parts hydrogen contents are 0.67wt%, 0.48 mass parts 1% by 75 mass parts contents of ethylene, homogenizer is used to stir 30min with the speed of 5000rpm, seal preservation after mixing, obtain joint sealant B component;
A and B component are mixed according to the mass ratio of 1:1, to needing the position of embedding to pour into, under the condition of <100 millibar, carry out vacuum-treat remove bubble, 50 DEG C of solidifications, obtain a kind of pliable and tough elastomerics, complete solidification process.
Use and testing method according to described in embodiment 1, gained organic silicon potting adhesive is tested, the results are shown in Table 1.
Comparative example
Buy the Si―H addition reaction type organic silicon potting adhesive PV-7030R commodity that Dow Corning Corporation produces, with reference to its product description, be cured.
Its results of property is tested in table 1 according to testing method described in embodiment 1.
The performance comparison data sheet of each embodiment joint sealant of table 1
By known compared with comparative example's Si―H addition reaction type organic silicon potting adhesive; organic silicon potting adhesive viscosity prepared by embodiment 1-5 is low, longevity of service; constructability operates; have that solidification rate is fast simultaneously, excellent in mechanical performance, high heat conduction, low-thermal-expansion and high breakdown strength; the performance of organic silicon potting adhesive is improve, for photovoltaic junction box provides reliably lasting protection largely.
Claims (10)
1. a preparation method for addition-type silicon rubber, is characterized in that comprising following steps:
1) ethenyl blocking polydimethyl siloxane fluid, micron silicon micro mist, platinum catalyst, tackifier are mixed according to mass ratio 100:25.00-40.00:0.66-0.90:0.04-0.20, after stirring and evenly mixing, sealing is preserved, and obtains joint sealant component A;
2) ethenyl blocking polydimethyl siloxane fluid, micron silicon micro mist, nano-scale white carbon black, hydrogen base end-blocking polydimethyl siloxane fluid, dimethyl methylhydrogenpolysi,oxane, addition reaction of silicon with hydrogen inhibitor are mixed according to mass ratio 70.00-86.00:25.00-40.00:0.40-0.60:11.81-28.60:0.68-2.74: 0.30-0.75, after stirring and evenly mixing, sealing is preserved, and obtains joint sealant B component;
3) by joint sealant component A and joint sealant B component according to 1:0.5-2 mass ratio with the use of, obtain the two component joint sealant of Si―H addition reaction type fast setting;
Wherein, described tackifier are selected from the silane coupling agent of not sulfur-bearing, nitrogen element; Described platinum catalyst is selected from platinum title complex; Described addition reaction of silicon with hydrogen inhibitor is selected from the organic compound containing alkynyl.
2. preparation method according to claim 1, is characterized in that, the contents of ethylene of described ethenyl blocking polydimethyl siloxane fluid is 0.2-0.42wt%, and the contents of ethylene of described ethenyl blocking polydimethyl siloxane fluid is 0.16-0.31wt%; Described hydrogen base end-blocking polydimethyl siloxane fluid hydrogen content is 0.05-0.10wt%; Described dimethyl methylhydrogenpolysi,oxane hydrogen content is 0.34-0.67wt%.
3. preparation method according to claim 1, is characterized in that, described platinum catalyst is the silicon oil solution of divinyl tetramethyl disiloxane platinum title complex; In platinum catalyst, platinum content is 1000-5000ppm.
4. preparation method according to claim 1, is characterized in that, described tackifier are γ-methacryloxypropyl trimethoxy silane.
5. preparation method according to claim 1, is characterized in that, step 1) or step 2) in micron silicon micro mist to be particle diameter the be silicon-dioxide of 3-10 μm.
6. preparation method according to claim 1, is characterized in that, described addition reaction of silicon with hydrogen inhibitor is the silicon oil solution of the ethynylcyclohexanol of massfraction 0.5-5%.
7. preparation method according to claim 1, is characterized in that: step 1) in, the component of mixing is also comprising toner; Described tinting material is selected from micron-sized inorganic powder dyestuff; The mass ratio of tinting material and ethenyl blocking polydimethyl siloxane fluid is 0.80-1.85:100.
8. preparation method according to claim 7, is characterized in that, described tinting material to be particle diameter the be carbon black of 5-20 μm.
9. the addition-type silicon rubber that the method according to any one of claim 1-8 prepares.
10. silicon rubber according to claim 9 is used for the application in electron pouring sealant.
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CN105838321A (en) * | 2016-05-19 | 2016-08-10 | 李金平 | Organic silicon electronic pouring sealant |
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CN105838321A (en) * | 2016-05-19 | 2016-08-10 | 李金平 | Organic silicon electronic pouring sealant |
CN107915999A (en) * | 2016-10-11 | 2018-04-17 | 华成新材料(惠州)有限公司 | A kind of addition thermal conductive fire retardant insulating silicon rubber and preparation method thereof |
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CN108587560A (en) * | 2018-05-25 | 2018-09-28 | 唐山三友硅业有限责任公司 | Resinification organic silicon electronic encapsulates glue composition |
CN108641669A (en) * | 2018-05-25 | 2018-10-12 | 唐山三友硅业有限责任公司 | High-strength anti-flaming casting glue and preparation method thereof |
CN108587560B (en) * | 2018-05-25 | 2021-04-23 | 唐山三友硅业有限责任公司 | Resinated organic silicon electronic packaging adhesive composition |
CN109825089A (en) * | 2018-12-27 | 2019-05-31 | 华南协同创新研究院 | A kind of heat conductive silica gel material and the preparation method and application thereof |
CN111909655A (en) * | 2020-07-27 | 2020-11-10 | 深圳市新亚新材料有限公司 | Pouring sealant and preparation method and application thereof |
CN112679963A (en) * | 2020-12-29 | 2021-04-20 | 睿合科技有限公司 | Integrated black silica gel OCR (optical character recognition) based on crosslinking density improvement performance and preparation method thereof |
CN116179150A (en) * | 2021-11-26 | 2023-05-30 | 中国工程物理研究院化工材料研究所 | Impact-resistant energy-absorbing organosilicon pouring sealant and preparation method thereof |
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