CN104109504A - Deeply-cured ketoxime type single-component room-temperature vulcanized silicon rubber and preparation method thereof - Google Patents
Deeply-cured ketoxime type single-component room-temperature vulcanized silicon rubber and preparation method thereof Download PDFInfo
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- CN104109504A CN104109504A CN201410323853.9A CN201410323853A CN104109504A CN 104109504 A CN104109504 A CN 104109504A CN 201410323853 A CN201410323853 A CN 201410323853A CN 104109504 A CN104109504 A CN 104109504A
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- 229920002379 silicone rubber Polymers 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims description 6
- 239000000463 material Substances 0.000 claims abstract description 13
- 239000000945 filler Substances 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims description 29
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 18
- 239000000203 mixture Substances 0.000 claims description 18
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 12
- -1 methyl siloxane Chemical class 0.000 claims description 12
- 229910000077 silane Inorganic materials 0.000 claims description 12
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 claims description 10
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- 239000004902 Softening Agent Substances 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 5
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 4
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Natural products CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 claims description 4
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 claims description 4
- FSEUPUDHEBLWJY-HWKANZROSA-N diacetylmonoxime Chemical compound CC(=O)C(\C)=N\O FSEUPUDHEBLWJY-HWKANZROSA-N 0.000 claims description 4
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 4
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 claims description 4
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 4
- 150000004756 silanes Chemical class 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 4
- 229920002554 vinyl polymer Polymers 0.000 claims description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 2
- ISKQADXMHQSTHK-UHFFFAOYSA-N [4-(aminomethyl)phenyl]methanamine Chemical compound NCC1=CC=C(CN)C=C1 ISKQADXMHQSTHK-UHFFFAOYSA-N 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims description 2
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 2
- 150000003857 carboxamides Chemical class 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- 239000000470 constituent Substances 0.000 claims description 2
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims description 2
- DROMNWUQASBTFM-UHFFFAOYSA-N dinonyl benzene-1,2-dicarboxylate Chemical compound CCCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCCC DROMNWUQASBTFM-UHFFFAOYSA-N 0.000 claims description 2
- 150000002148 esters Chemical class 0.000 claims description 2
- WIEGKKSLPGLWRN-UHFFFAOYSA-N ethyl 3-oxobutanoate;titanium Chemical compound [Ti].CCOC(=O)CC(C)=O WIEGKKSLPGLWRN-UHFFFAOYSA-N 0.000 claims description 2
- PHQOGHDTIVQXHL-UHFFFAOYSA-N n'-(3-trimethoxysilylpropyl)ethane-1,2-diamine Chemical compound CO[Si](OC)(OC)CCCNCCN PHQOGHDTIVQXHL-UHFFFAOYSA-N 0.000 claims description 2
- KOVKEDGZABFDPF-UHFFFAOYSA-N n-(triethoxysilylmethyl)aniline Chemical compound CCO[Si](OCC)(OCC)CNC1=CC=CC=C1 KOVKEDGZABFDPF-UHFFFAOYSA-N 0.000 claims description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 2
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims description 2
- 239000003054 catalyst Substances 0.000 abstract description 2
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 239000011521 glass Substances 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 239000004575 stone Substances 0.000 abstract description 2
- 239000003431 cross linking reagent Substances 0.000 abstract 1
- 235000013870 dimethyl polysiloxane Nutrition 0.000 abstract 1
- 239000004205 dimethyl polysiloxane Substances 0.000 abstract 1
- 229920001971 elastomer Polymers 0.000 abstract 1
- 238000003912 environmental pollution Methods 0.000 abstract 1
- 239000004014 plasticizer Substances 0.000 abstract 1
- 239000004945 silicone rubber Substances 0.000 description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Natural products CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 4
- 238000005987 sulfurization reaction Methods 0.000 description 4
- 239000012975 dibutyltin dilaurate Substances 0.000 description 3
- 238000004513 sizing Methods 0.000 description 3
- 238000004073 vulcanization Methods 0.000 description 3
- 239000003566 sealing material Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Natural products C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
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- Sealing Material Composition (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a deeply-cured ketoxime type single-component room-temperature vulcanized silicon rubber which comprises the following components in parts by mass: 35-80 parts of hydroxyl-terminated poly-dimethyl siloxane, 25-80 parts of filler, 2-10 parts of plasticizer, 1-8 parts of crosslinking agent, 0.1-5 parts of tackifier, 0.01-1 part of catalyst, 0.1-5 parts of deep curing accelerator and 1-10 parts of color paste. Compared with the prior art, the deeply-cured ketoxime type single-component room-temperature vulcanized silicon rubber has the advantages that the deep curing is greatly improved, the curing depth is greater than 5mm for 24 hours, the rubber is free from corroding base materials of stone, glass, metal and the like, good in binding property and low in energy consumption during production process and has no three wastes and no environmental pollution.
Description
[technical field]
The invention belongs to construction sealing materials category, particularly the technical field of single-component room temperature vulcanized silicon rubber of a kind of deeply-curing ketoxime type and preparation method thereof.
[background technology]
Room temperature vulcanized silicone rubber is because have good dielectric properties, chemical property, well heat-resisting, weathering resistance and bonding strength, can be in the scope of-65~232 DEG C the premium properties such as life-time service, become widely used a kind of sealing material, be called as liquid packing.
Press composition, sulfuration mechanism different with operation, room temperature vulcanized silicone rubber can be divided into single-component, bicomponent condensed type room temperature sulfidization silicon rubber and dual composition addition type room temperature vulcanized silicone rubber.The sulfuration of single-component room temperature vulcanized silicon rubber is undertaken by absorbing airborne moisture, and curing time depends on the thickness of vulcanization system, temperature, humidity and silastic-layer.Sulfuration is from outward appearance to inner essence carried out, and deeply-curing is slow.The sulfuration of double component room temperature vulcanization silicon rubber causes by catalyzer, can carry out on surface and inside simultaneously, can deeply-curing.Curing time can be by catalyst levels control.The curing time of addition type room temperature vulcanized silicone rubber depends primarily on temperature, therefore, utilizes temperature can control its vulcanization rate.
[summary of the invention]
Object of the present invention solves the problems of the prior art exactly, proposes the single-component room temperature vulcanized silicon rubber of a kind of deeply-curing ketoxime type, can overcome the slow problem of single-component room temperature vulcanized silicon rubber deeply-curing in the market.
For achieving the above object, the present invention proposes the single-component room temperature vulcanized silicon rubber of a kind of deeply-curing ketoxime type, comprise that following component and each constituent mass ratio are: hydroxyl-terminated injecting two methyl siloxane: 35~80 parts, filler: 35~80 parts, softening agent: 2~10 parts, linking agent: 1~8 part, tackifier: 0.1~5 part, catalyzer: 0.01~1 part, deeply-curing promotor: 0.1~5 part, mill base: 1~10 part.
As preferably, the viscosity of described hydroxyl-terminated injecting two methyl siloxane in the time that temperature is 25 DEG C is 10000~80000 centipoises.
As preferably, described filler is at least one or two the above mixtures in gas-phase silica, precipitated silica, light calcium carbonate or water-ground limestone, and described light calcium carbonate is nm-class active calcium carbonate.
As preferably, described softening agent is at least one or two the above mixtures in dibutyl phthalate, dioctyl phthalate (DOP), Dinonylphthalate or the different ester of phthalic acid two.
As preferably, described linking agent is at least one or two the above mixtures in dimethyl two Diacetylmonoxime base silanes, methyl tributanoximo silane, vinyl tributyl ketoximyl silane, phenyl tributanoximo silane, propyl group tributanoximo silane or four Diacetylmonoxime base silanes.
As preferably, described tackifier are at least one or two the above mixtures in γ-aminopropyl triethoxysilane, γ-(2,3-glycidoxy) propyl trimethoxy silicane, N-β-aminoethyl-γ-aminopropyltrimethoxysilane or anilinomethyl triethoxysilane.
As preferably, described catalyzer is at least one or two above mixtures in dibutyltin diacetate, dibutyl tin laurate, isopropyl titanate, tetrabutyl titanate, ethylacetoacetate titanium inner complex.
As preferably, described deeply-curing promotor is at least one or two above mixtures in ketone compounds, etheric acid compounds, Carbox amide.
For achieving the above object, the invention allows for the preparation method of the single-component room temperature vulcanized silicon rubber of a kind of deeply-curing ketoxime type, comprise the following steps successively:
1) prepare base-material:
A) after 35~80 parts of hydroxyl-terminated injecting two methyl siloxanes and 35~80 parts of fillers are dropped into kneaders stirring, vacuumize-0.06~-0.1MPa, stir 20~40min;
B) add 2~10 parts of softening agent, vacuumize-0.06~-0.1MPa, stir 20~40min;
C) base-material preparing is proceeded to planet machine for subsequent use.
2) prepare the single-component room temperature vulcanized silicon rubber of deeply-curing ketoxime type:
A) in planet machine, add 1~10 part of mill base and step 1) in the base-material mix and blend for preparing, vacuumize-0.06~-0.1MPa, stir 20~40min;
B) 1~8 part of linking agent is added to planetary mixer, vacuumize-0.06~-0.1MPa, stir 20~40min;
C) 0.1~5 part of tackifier, 0.01~1 part of catalyzer are added to planetary mixer, vacuumize-0.06~-0.1MPa, stir 20~40min;
D) 0.1~5 part of deeply-curing promotor is added to planetary mixer, vacuumize-0.06~-0.1MPa, stir 20~40min; Make the single-component room temperature vulcanized silicon rubber of deeply-curing ketoxime type.
Beneficial effect of the present invention:
1, the room temperature vulcanized silicone rubber deeply-curing that prepared by formula provided by the invention is largely increased, and within 24 hours, curing depth is greater than 5mm.
2, the silicon rubber that prepared by the present invention is corrosion-free to base materials such as stone material, glass, metals, and cementability is good.
3, preparation method provided by the invention, in production process, energy consumption is low, produces environmentally safe without the three wastes.
Feature of the present invention and advantage will be elaborated by embodiment.
[embodiment]
Embodiment:
Sample 1:
After 100g viscosity 20000cps (25 DEG C) hydroxyl-terminated injecting two methyl siloxane and 100g nm-class active calcium carbonate are stirred in kneader, vacuumize-0.096~-0.1MPa, stir 20-40min; Unload vacuum, drop into 8g dibutyl phthalate, vacuumize-0.096~-0.1MPa, stir 20-40min; The sizing material making is proceeded to planetary mixer for subsequent use.
Add planetary mixer to mix with the base-material preparing 10g vinyl tributyl ketoximyl silane, vacuumize-0.096~-0.1MPa, stir 20-40min; 2.5g γ-aminopropyl triethoxysilane, 0.1g dibutyl tin dilaurate are added to planetary mixer, vacuumize-0.096~-0.1MPa, stir 20-40min; 1.5g acetic acid acetyl triethyl is added to planetary mixer, vacuumize-0.096~-0.1MPa, stir 20-40min.Obtain paste and be designated as sample 1, test result is as shown in table 1.
Sample 2:
After 100g viscosity 50000cps (25 DEG C) hydroxyl-terminated injecting two methyl siloxane and 80g nm-class active calcium carbonate are stirred in kneader, vacuumize-0.096~-0.1MPa, stir 20-40min; Unload vacuum, drop into 15g dibutyl phthalate, vacuumize-0.096~-0.1MPa, stir 20-40min; The sizing material making is proceeded to planetary mixer for subsequent use.
10g methyl tributanoximo silane is added to planetary mixer, vacuumize-0.096~-0.1MPa, stir 20-40min; Then 1.3gN-β-aminoethyl-γ-aminopropyltrimethoxysilane, 0.1g dibutyl tin dilaurate are added to planetary mixer, vacuumize-0.096~-0.1MPa, stir 20-40min; 1g methane amide is added to planetary mixer, vacuumize-0.096~-0.1MPa, stir 20-40min.Obtain paste and be designated as sample 2, test result is as shown in table 1.
Sample 3:
After 100g viscosity 80000cps (25 DEG C) hydroxyl-terminated injecting two methyl siloxane and 80g nm-class active calcium carbonate are stirred in kneader, vacuumize-0.096~-0.1MPa, stir 20-40min; Unload vacuum, drop into 20g dibutyl phthalate, vacuumize-0.096~-0.1MPa, stir 20-40min; The sizing material making is proceeded to planetary mixer for subsequent use.
2g methyl tributanoximo silane, 8g vinyl tributyl ketoximyl silane are added to planetary mixer, vacuumize-0.096~-0.1MPa, stir 20-40min; Then 1.25g γ-aminopropyl triethoxysilane, 1.25N-β-aminoethyl-γ-aminopropyltrimethoxysilane, 0.1g dibutyl tin dilaurate are added to planetary mixer, vacuumize-0.096~-0.1MPa, stir 20-40min; 1.5g acetic acid acetyl triethyl is added to planetary mixer, vacuumize-0.096~-0.1MPa, stir 20-40min.Obtain paste and be designated as sample 3, test result is as shown in table 1.
Table 1 sample test record
Above-described embodiment is to explanation of the present invention, is not limitation of the invention, any scheme after simple transformation of the present invention is all belonged to protection scope of the present invention.
Claims (9)
1. the single-component room temperature vulcanized silicon rubber of deeply-curing ketoxime type, it is characterized in that: comprise that following component and each constituent mass ratio are: hydroxyl-terminated injecting two methyl siloxane: 35~80 parts, filler: 35~80 parts, softening agent: 2~10 parts, linking agent: 1~8 part, tackifier: 0.1~5 part, catalyzer: 0.01~1 part, deeply-curing promotor: 0.1~5 part, mill base: 1~10 part.
2. the single-component room temperature vulcanized silicon rubber of a kind of deeply-curing ketoxime type as claimed in claim 1, is characterized in that: the viscosity of described hydroxyl-terminated injecting two methyl siloxane in the time that temperature is 25 DEG C is 10000~80000 centipoises.
3. the single-component room temperature vulcanized silicon rubber of a kind of deeply-curing ketoxime type as claimed in claim 1, it is characterized in that: described filler is at least one or two the above mixtures in gas-phase silica, precipitated silica, light calcium carbonate or water-ground limestone, and described light calcium carbonate is nm-class active calcium carbonate.
4. the single-component room temperature vulcanized silicon rubber of a kind of deeply-curing ketoxime type as claimed in claim 1, is characterized in that: described softening agent is at least one or two the above mixtures in dibutyl phthalate, dioctyl phthalate (DOP), Dinonylphthalate or the different ester of phthalic acid two.
5. the single-component room temperature vulcanized silicon rubber of a kind of deeply-curing ketoxime type as claimed in claim 1, is characterized in that: described linking agent is at least one or two the above mixtures in dimethyl two Diacetylmonoxime base silanes, methyl tributanoximo silane, vinyl tributyl ketoximyl silane, phenyl tributanoximo silane, propyl group tributanoximo silane or four Diacetylmonoxime base silanes.
6. the single-component room temperature vulcanized silicon rubber of a kind of deeply-curing ketoxime type as claimed in claim 1, it is characterized in that: described tackifier are at least one or two the above mixtures in γ-aminopropyl triethoxysilane, γ-(2,3-glycidoxy) propyl trimethoxy silicane, N-β-aminoethyl-γ-aminopropyltrimethoxysilane or anilinomethyl triethoxysilane.
7. the single-component room temperature vulcanized silicon rubber of a kind of deeply-curing ketoxime type as claimed in claim 1, is characterized in that: described catalyzer is at least one or two above mixtures in dibutyltin diacetate, dibutyl tin laurate, isopropyl titanate, tetrabutyl titanate, ethylacetoacetate titanium inner complex.
8. the single-component room temperature vulcanized silicon rubber of a kind of deeply-curing ketoxime type as described in any one in claim 1 to 7, is characterized in that: described deeply-curing promotor is at least one or two above mixtures in ketone compounds, etheric acid compounds, Carbox amide.
9. a preparation method for the single-component room temperature vulcanized silicon rubber of deeply-curing ketoxime type, is characterized in that: comprise the following steps successively:
1) prepare base-material:
A) after 35~80 parts of hydroxyl-terminated injecting two methyl siloxanes and 35~80 parts of fillers are dropped into kneaders stirring, vacuumize-0.06~-0.1MPa, stir 20~40min;
B) add 2~10 parts of softening agent, vacuumize-0.06~-0.1MPa, stir 20~40min;
C) base-material preparing is proceeded to planet machine for subsequent use.
2) prepare the single-component room temperature vulcanized silicon rubber of deeply-curing ketoxime type:
A) in planet machine, add 1~10 part of mill base and step 1) in the base-material mix and blend for preparing, vacuumize-0.06~-0.1MPa, stir 20~40min;
B) 1~8 part of linking agent is added to planetary mixer, vacuumize-0.06~-0.1MPa, stir 20~40min;
C) 0.1~5 part of tackifier, 0.01~1 part of catalyzer are added to planetary mixer, vacuumize-0.06~-0.1MPa, stir 20~40min;
D) 0.1~5 part of deeply-curing promotor is added to planetary mixer, vacuumize-0.06~-0.1MPa, stir 20~40min; Make the single-component room temperature vulcanized silicon rubber of deeply-curing ketoxime type.
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CN106190015A (en) * | 2016-08-22 | 2016-12-07 | 深圳市新亚新材料有限公司 | A kind of no-solvent type organosilicon coating glue and preparation method thereof |
CN107129790A (en) * | 2017-04-19 | 2017-09-05 | 常熟市恒信粘胶有限公司 | Neutral silicone sealant for stone material |
CN107142074A (en) * | 2017-05-09 | 2017-09-08 | 江苏天辰新材料股份有限公司 | A kind of preparation method of de-oxime type one component room temperature fluid sealant |
CN108219739A (en) * | 2017-12-30 | 2018-06-29 | 广州市白云化工实业有限公司 | Single-component ketonic oxime organosilicon adhesive glue of deeply-curing and preparation method thereof |
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CN102321450A (en) * | 2011-08-23 | 2012-01-18 | 杭州之江有机硅化工有限公司 | Solar energy photovoltaic assembly organosilicon sealant material and preparation method thereof |
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CN106190015A (en) * | 2016-08-22 | 2016-12-07 | 深圳市新亚新材料有限公司 | A kind of no-solvent type organosilicon coating glue and preparation method thereof |
CN107129790A (en) * | 2017-04-19 | 2017-09-05 | 常熟市恒信粘胶有限公司 | Neutral silicone sealant for stone material |
CN107142074A (en) * | 2017-05-09 | 2017-09-08 | 江苏天辰新材料股份有限公司 | A kind of preparation method of de-oxime type one component room temperature fluid sealant |
CN108219739B (en) * | 2017-12-30 | 2020-11-10 | 广州市白云化工实业有限公司 | Deep-cured single-component ketoxime-removed organic silicon adhesive and preparation method thereof |
CN108219739A (en) * | 2017-12-30 | 2018-06-29 | 广州市白云化工实业有限公司 | Single-component ketonic oxime organosilicon adhesive glue of deeply-curing and preparation method thereof |
CN111205650A (en) * | 2018-11-21 | 2020-05-29 | 王长杰 | Production process flow and formula of high-voltage bare conductor insulating material |
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