CN118085802A - Single-component ketoxime-removing silicone sealant containing sulfhydryl-amino and preparation method thereof - Google Patents
Single-component ketoxime-removing silicone sealant containing sulfhydryl-amino and preparation method thereof Download PDFInfo
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- CN118085802A CN118085802A CN202410273081.6A CN202410273081A CN118085802A CN 118085802 A CN118085802 A CN 118085802A CN 202410273081 A CN202410273081 A CN 202410273081A CN 118085802 A CN118085802 A CN 118085802A
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- 239000004590 silicone sealant Substances 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000004205 dimethyl polysiloxane Substances 0.000 claims abstract description 31
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims abstract description 31
- -1 polydimethylsiloxane Polymers 0.000 claims abstract description 31
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229910000077 silane Inorganic materials 0.000 claims abstract description 30
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 claims abstract description 20
- BMBTXSDLSUXVQZ-UHFFFAOYSA-N SCO[Si](OC)(OC)CCCN Chemical compound SCO[Si](OC)(OC)CCCN BMBTXSDLSUXVQZ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000007822 coupling agent Substances 0.000 claims abstract description 13
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 12
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 9
- 239000004014 plasticizer Substances 0.000 claims abstract description 8
- 239000012763 reinforcing filler Substances 0.000 claims abstract description 8
- LJTFFORYSFGNCT-UHFFFAOYSA-N Thiocarbohydrazide Chemical compound NNC(=S)NN LJTFFORYSFGNCT-UHFFFAOYSA-N 0.000 claims abstract description 5
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 32
- 238000000034 method Methods 0.000 claims description 20
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 16
- UUEWCQRISZBELL-UHFFFAOYSA-N 3-trimethoxysilylpropane-1-thiol Chemical compound CO[Si](OC)(OC)CCCS UUEWCQRISZBELL-UHFFFAOYSA-N 0.000 claims description 11
- 125000003396 thiol group Chemical group [H]S* 0.000 claims description 11
- 239000003054 catalyst Substances 0.000 claims description 10
- JJLKTTCRRLHVGL-UHFFFAOYSA-L [acetyloxy(dibutyl)stannyl] acetate Chemical compound CC([O-])=O.CC([O-])=O.CCCC[Sn+2]CCCC JJLKTTCRRLHVGL-UHFFFAOYSA-L 0.000 claims description 7
- 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 7
- HRYHMTOUSFNYKV-UHFFFAOYSA-N N[SiH2]S Chemical compound N[SiH2]S HRYHMTOUSFNYKV-UHFFFAOYSA-N 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 239000006229 carbon black Substances 0.000 claims description 3
- AMTWCFIAVKBGOD-UHFFFAOYSA-N dioxosilane;methoxy-dimethyl-trimethylsilyloxysilane Chemical group O=[Si]=O.CO[Si](C)(C)O[Si](C)(C)C AMTWCFIAVKBGOD-UHFFFAOYSA-N 0.000 claims description 3
- 229940083037 simethicone Drugs 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- KSBAEPSJVUENNK-UHFFFAOYSA-L tin(ii) 2-ethylhexanoate Chemical compound [Sn+2].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O KSBAEPSJVUENNK-UHFFFAOYSA-L 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims 2
- 238000006243 chemical reaction Methods 0.000 claims 2
- 239000008096 xylene Substances 0.000 claims 2
- 125000003277 amino group Chemical group 0.000 claims 1
- 229910001385 heavy metal Inorganic materials 0.000 claims 1
- 229910052757 nitrogen Inorganic materials 0.000 claims 1
- 239000002904 solvent Substances 0.000 claims 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 abstract description 5
- 239000012812 sealant material Substances 0.000 abstract description 3
- 239000003566 sealing material Substances 0.000 abstract description 3
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 abstract description 2
- 125000000467 secondary amino group Chemical group [H]N([*:1])[*:2] 0.000 abstract description 2
- 238000003860 storage Methods 0.000 abstract description 2
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 28
- 239000002994 raw material Substances 0.000 description 13
- 229940008099 dimethicone Drugs 0.000 description 11
- 239000000565 sealant Substances 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 7
- 229920002554 vinyl polymer Polymers 0.000 description 7
- 230000000694 effects Effects 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 125000000524 functional group Chemical group 0.000 description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- TXDNPSYEJHXKMK-UHFFFAOYSA-N sulfanylsilane Chemical compound S[SiH3] TXDNPSYEJHXKMK-UHFFFAOYSA-N 0.000 description 3
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- 230000006978 adaptation Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 229920005601 base polymer Polymers 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000001808 coupling effect Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 239000000806 elastomer Substances 0.000 description 1
- 238000012395 formulation development Methods 0.000 description 1
- 229910021485 fumed silica Inorganic materials 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000012945 sealing adhesive Substances 0.000 description 1
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical compound [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000011179 visual inspection Methods 0.000 description 1
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- Sealing Material Composition (AREA)
Abstract
The invention provides a single-component ketoxime type silicone sealant containing sulfhydryl-amino and a preparation method thereof, and relates to the field of organic sealant materials. According to the invention, aminopropyl trimethoxy silane and diaminothiourea are reacted to synthesize the mercapto-aminopropyl trimethoxy silane coupling agent, and the mercapto-aminopropyl trimethoxy silane coupling agent is added into alpha, omega-dihydroxy polydimethylsiloxane, reinforcing filler, plasticizer and cross-linking agent, and the mercapto-primary amino and secondary amino-containing modified coupling agent is added into the common organosilicon sealing material component, so that the bonding performance can be satisfied by a small amount of addition, and the requirement of the single-component sealant material on the bonding property of a base material is greatly improved; the coupling agent is stable in storage, increases molecular polarity, and has amino content far higher than that of traditional silane such as gamma-aminopropyl triethoxy silane.
Description
Technical Field
The invention relates to the field of organic sealing adhesive materials, in particular to a single-component ketoxime-removing silicone sealant containing sulfhydryl-amino and a preparation method thereof.
Background
The organic silicon sealant is used as one of the polymer sealing materials with the widest application in the adhesive industry, especially the single-component ketoxime-removing silicone sealant has the excellent properties of wide application temperature range, excellent weather aging resistance, electrical property, adhesion and the like, and has very wide application in the fields of electronic components, photovoltaic module junction boxes, photovoltaic inverter sealing and the like.
The single-component ketoxime-free silicone sealant generally uses organotin as a catalyst, hydroxyl-terminated polydimethylsiloxane as a base polymer, methyltributyloxidoxysilane, vinyltributylketoxime-based silane and the like as cross-linking agents, and forms a three-dimensional reticular elastomer through condensation of a siloxane bond and hydroxyl. Compared with the low hydrolysis activity of the dealcoholized crosslinking agent, the ketoxime crosslinking agent has higher curing speed, and under the condition of adding a certain amount of organotin catalyst and enough amino silane coupling agent, the mercapto silane is required to be additionally added to increase the adhesiveness and balance catalytic activity of the system, so that the process difficulty and the raw material cost are increased to a certain extent in the formulation development and actual production.
Disclosure of Invention
The invention provides a single-component ketoxime-removing silicone sealant containing sulfhydryl-amino and a preparation method thereof, and aims to solve the problem.
In order to achieve the above purpose, the embodiment of the invention provides a single-component ketoxime-removing silicone sealant containing mercapto-amino, which comprises the following components in parts by weight:
a, ω -dihydroxy polydimethylsiloxane: 100 parts of
Reinforcing filler: 80-140 parts
And (3) a plasticizer: 2 to 10 portions
Crosslinking agent: 2 to 20 parts
Mercapto-aminosilane coupling agent: 0.5 to 3 parts
Catalyst: 0.01 to 1.5 parts
Based on one general inventive concept, the embodiment of the invention provides a preparation method of the single-component ketoxime-removing type silicone sealant containing sulfhydryl-amino, which comprises the following steps:
S1: reacting gamma-aminopropyl trimethoxy silane with diaminothiourea to obtain a mercapto-aminosilane coupling agent;
s2: mixing a, omega-dihydroxy polydimethylsiloxane, a reinforcing filler and a plasticizer to obtain a base material;
s3: and mixing the base material with a cross-linking agent, a curing agent, a sulfhydryl-amino silane coupling agent and a catalyst to obtain the sulfhydryl-amino-containing single-component ketoxime-removing silicone sealant.
Preferably, the mercapto-aminosilane coupling agent has the structural formula
Unlike conventional molecular structure with only amino functional group or mercapto functional group, the coupling agent contains both amino functional group and mercapto functional group and has the coupling property of both functional groups.
Preferably, the viscosity of the alpha, omega-dihydroxy polydimethylsiloxane is 20000-100000 mpa.s at 25 ℃.
Preferably, the reinforcing filler is at least one of nano calcium carbonate, heavy calcium carbonate and white carbon black.
Preferably, the plasticizer is simethicone, and the viscosity at 25 ℃ is 100-1000 mpa.s.
Preferably, the cross-linking agent is at least one of methyltributyloxidoxysilane, vinyltributylketoxime silane and phenyltributylketoxime silane.
Preferably, in the step S1, the mixture is heated to 120-130 ℃ and vacuumized for more than-0.095 MPa for 2-3 hours; in the step S2, stirring is carried out for 20-40 min at the vacuum degree of more than-0.095 MPa.
Preferably, the mercapto-aminosilane coupling agent is at least one of aminopropyl trimethoxysilane, mercaptopropyl trimethoxysilane, and mercapto-aminopropyl trimethoxysilane.
Preferably, the catalyst is at least one of di-n-butyl tin dilaurate, di-n-butyl tin diacetate and stannous octoate.
The scheme of the invention has the following beneficial effects:
(1) According to the invention, aminopropyl trimethoxy silane and diaminothiourea are reacted to synthesize the mercapto-aminopropyl trimethoxy silane coupling agent, and the mercapto-aminopropyl trimethoxy silane coupling agent is added into alpha, omega-dihydroxy polydimethylsiloxane, reinforcing filler, plasticizer and cross-linking agent, and the mercapto-primary amino and secondary amino-containing modified coupling agent is added into the common organosilicon sealing material component, so that the bonding performance can be satisfied by a small amount of addition, and the requirement of the single-component sealant material on the bonding property of a base material is greatly improved; the coupling agent is stable in storage, increases molecular polarity, and has amino content far higher than that of traditional silane such as gamma-aminopropyl triethoxy silane.
(2) Compared with the process of adding the mercaptopropyl trimethoxy silane in the ketoxime removing type sealant, the mercaptopropyl trimethoxy silane is required to inhibit the activity of organic tin, so that the sealant crust in the production process is avoided, and the mercapto-containing amino single-component ketoxime removing type silicone sealant can meet the production process requirement without adding the mercaptosilane.
Detailed Description
In order to make the technical problems, technical solutions and advantages to be solved by the present invention more apparent, the following detailed description will be made with reference to specific embodiments.
Unless defined otherwise, all technical and scientific terms used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the scope of the present invention.
Unless otherwise specifically indicated, the various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or may be prepared by existing methods.
The invention provides a single-component ketoxime-removing silicone sealant containing sulfhydryl-amino and a preparation method thereof, aiming at the existing problems.
Example 1
A single-component ketoxime-removing silicone sealant containing mercapto-amino comprises the following raw materials in parts by mass:
alpha, omega-dihydroxy polydimethylsiloxane: 100 parts of
Nano calcium carbonate: 80 parts of
Dimethicone: 5 parts of
Methyltributylketonoxime silane: 9 parts of
Vinyl tributylketoximino silane: 3 parts of
Mercapto-aminopropyl trimethoxysilane: 0.5 part
Di-n-butyl tin dilaurate: 0.2 part
The preparation method of the single-component ketoxime removing type silicone sealant containing the sulfhydryl-amino group comprises the following steps:
a. adding the a, omega-dihydroxy polydimethylsiloxane, nano calcium carbonate and simethicone into a kneader, uniformly mixing, heating to 120-130 ℃, vacuumizing to-0.095 MPa to-0.1 MPa for 2-3 hours, obtaining a base material, and cooling to room temperature.
B. adding a cross-linking agent, a coupling agent and a catalyst into the base material cooled to room temperature, stirring for 20-40 min at a vacuum degree of-0.095 MPa to-0.1 MPa, and then discharging and storing in a sealed cylinder.
Example 2
A single-component ketoxime-removing silicone sealant containing mercapto-amino comprises the following raw materials in parts by mass:
alpha, omega-dihydroxy polydimethylsiloxane: 100 parts of
Nano calcium carbonate: 100 parts of
Dimethicone: 5 parts of
Methyltributylketonoxime silane: 9 parts of
Vinyl tributylketoximino silane: 3 parts of
Mercapto-aminopropyl trimethoxysilane: 1 part of
Di-n-butyl tin dilaurate: 0.2 part
The preparation procedure was the same as in example 1.
Example 3
A single-component ketoxime-removing silicone sealant containing mercapto-amino comprises the following raw materials in parts by mass:
alpha, omega-dihydroxy polydimethylsiloxane: 100 parts of
Nano calcium carbonate: 120 parts of
Dimethicone: 10 parts of
Methyltributylketonoxime silane: 9 parts of
Vinyl tributylketoximino silane: 3 parts of
Mercapto-aminopropyl trimethoxysilane: 2 parts of
Di-n-butyl tin dilaurate: 0.2 part
The preparation procedure was the same as in example 1.
Example 4
A single-component ketoxime-removing silicone sealant containing mercapto-amino comprises the following raw materials in parts by mass: alpha, omega-dihydroxy polydimethylsiloxane: 100 parts of
Nano calcium carbonate: 140 parts
Dimethicone: 10 parts of
Methyltributylketonoxime silane: 9 parts of
Phenyltributylketoximino silane: 3 parts of
Mercapto-aminopropyl trimethoxysilane: 3 parts of
Di-n-butyl tin diacetate: 0.2 part
The preparation procedure was the same as in example 1.
Example 5
A single-component ketoxime-removing silicone sealant containing mercapto-amino comprises the following raw materials in parts by mass: alpha, omega-dihydroxy polydimethylsiloxane: 100 parts of
Heavy calcium carbonate: 130 parts of fumed silica: 10
Dimethicone: 5 parts of
Phenyltributylketoximino silane: 9 parts of
Vinyl tributylketoximino silane: 3 parts of
Mercapto-aminopropyl trimethoxysilane: 0.5 part
Aminopropyl trimethoxysilane: 1.5 parts by weight
Di-n-butyl tin diacetate: 0.4 part
The preparation procedure was the same as in example 1.
Example 6
A single-component ketoxime-removing silicone sealant containing mercapto-amino comprises the following raw materials in parts by mass: alpha, omega-dihydroxy polydimethylsiloxane: 100 parts of
Heavy calcium carbonate: 130 parts of
White carbon black by gas phase method: 10 parts of
Dimethicone: 10 parts of
Phenyltributylketoximino silane: 9 parts of
Vinyl tributylketoximino silane: 3 parts of
Mercapto-aminopropyl trimethoxysilane: 1 part of
Aminopropyl trimethoxysilane: 2 parts of
Stannous octoate: 1 part of
The preparation procedure was the same as in example 1.
Comparative example 1
A single-component ketoxime-removing silicone sealant comprises the following raw materials in parts by mass:
alpha, omega-dihydroxy polydimethylsiloxane: 100 parts of
Nano calcium carbonate: 100 parts of
Dimethicone: 5 parts of
Methyltributylketonoxime silane: 9 parts of
Vinyl tributylketoximino silane: 3 parts of
Aminopropyl trimethoxysilane: 0.5 part
Mercaptopropyl trimethoxysilane: 0.5 part
Di-n-butyl tin dilaurate: 0.2 part
The preparation method is the same as in example 1, and aminopropyl trimethoxysilane and mercaptopropyl trimethoxysilane are added separately in the same total amount as in example 2.
Comparative example 2
A single-component ketoxime-removing silicone sealant comprises the following raw materials in parts by mass:
alpha, omega-dihydroxy polydimethylsiloxane: 100 parts of
Nano calcium carbonate: 120 parts of
Dimethicone: 10 parts of
Methyltributylketonoxime silane: 9 parts of
Vinyl tributylketoximino silane: 3 parts of
Aminopropyl trimethoxysilane: 2 parts of
Mercaptopropyl trimethoxysilane: 2 parts of
Di-n-butyl tin dilaurate: 0.2 part
The preparation method is the same as in example 1, and aminopropyl trimethoxysilane and mercaptopropyl trimethoxysilane are added separately in the same total amount as in example 3.
Comparative example 3
A single-component ketoxime-removing silicone sealant comprises the following raw materials in parts by mass:
alpha, omega-dihydroxy polydimethylsiloxane: 100 parts of
Nano calcium carbonate: 140 parts
Dimethicone: 10 parts of
Methyltributylketonoxime silane: 9 parts of
Phenyltributylketoximino silane: 3 parts of
Aminopropyl trimethoxysilane: 3 parts of
Mercaptopropyl trimethoxysilane: 3 parts of
Di-n-butyl tin diacetate: 0.2 part
The preparation method is the same as in example 1, and aminopropyl trimethoxysilane and mercaptopropyl trimethoxysilane are added separately in the same total amount as in example 4.
Comparative example 4
A single-component ketoxime-removing silicone sealant comprises the following raw materials in parts by mass:
alpha, omega-dihydroxy polydimethylsiloxane: 100 parts of
Nano calcium carbonate: 140 parts
Dimethicone: 10 parts of
Methyltributylketonoxime silane: 9 parts of
Phenyltributylketoximino silane: 3 parts of
Aminopropyl trimethoxysilane: 1 part of
Di-n-butyl tin diacetate: 0.2 part
The preparation method is the same as in example 1, and only aminopropyl trimethoxy silane is added into the coupling agent.
Comparative example 5
A single-component ketoxime-removing silicone sealant comprises the following raw materials in parts by mass:
alpha, omega-dihydroxy polydimethylsiloxane: 100 parts of
Nano calcium carbonate: 140 parts
Dimethicone: 10 parts of
Methyltributylketonoxime silane: 9 parts of
Phenyltributylketoximino silane: 3 parts of
Aminopropyl trimethoxysilane: 2 parts of
Di-n-butyl tin diacetate: 0.2 part
The preparation method is the same as in example 1, and only aminopropyl trimethoxy silane is added into the coupling agent.
Performance testing
The assay standard or method is as follows:
Appearance: visual inspection;
adhesion test: GB 16776-2005 annex D.1.2 method B;
the above examples and comparative examples were tested and the results were determined: as shown in table one below.
List one
According to the embodiments 1-6, the sulfhydryl-aminopropyl trimethoxy silane is added into the single-component ketoxime-removing silicone sealant, and the components of the formula are optimized, so that the sealant with qualified appearance and capable of being bonded with glass and stainless steel is finally prepared.
From examples 1 to 4 and comparative examples 1 to 4, it is apparent that the sealant has a fine and smooth appearance and can achieve good adhesion to both glass and stainless steel when the amount of mercapto-aminopropyl trimethoxy silane added is 2 parts or more. When the mercapto-aminopropyl trimethoxy silane is not added, the aminopropyl trimethoxy silane and the mercaptopropyl trimethoxy silane are added separately, and when the total amount of the two is 4 parts, the sealant has adhesion to glass only, and when the total amount of the two reaches 6 parts, the sealant has good adhesion effect to glass and stainless steel.
From examples 1 to 6 and comparative examples 5 to 6, it is apparent that when mercapto-aminopropyl trimethoxysilane is added, the organic tin activity can be suppressed due to the self-contained mercapto functional group in the molecule, and the sealant has a qualified appearance and meets the production process requirements. When the aminopropyl trimethoxy silane is added singly and the mercapto silane coupling agent is not added, the whole appearance of the sealant is rough, and the process appearance requirement cannot be met.
While the foregoing is directed to the preferred embodiments of the present invention, it will be appreciated by those skilled in the art that various modifications and adaptations can be made without departing from the principles of the present invention, and such modifications and adaptations are intended to be comprehended within the scope of the present invention.
Claims (10)
1. The single-component ketoxime-removing silicone sealant containing the mercapto-amino group is characterized by comprising the following components in parts by weight:
a, ω -dihydroxy polydimethylsiloxane: 100 parts of
Reinforcing filler: 80-140 parts
And (3) a plasticizer: 2 to 10 portions
Crosslinking agent: 2 to 20 parts
Mercapto-aminosilane coupling agent: 0.5 to 3 parts
Catalyst: 0.01 to 1.5 portions.
2. A method for preparing the single-component ketoxime-removing type silicone sealant containing mercapto-amino group according to claim 1, which is characterized by comprising the following steps:
S1: 1mol of diaminothiourea is dissolved in a certain amount of xylene solvent, heavy metal Pt is used as a catalyst, a reaction system is heated to 80-90 ℃ under the protection of nitrogen, and 0.8-0.9 mol of gamma-aminopropyl trimethoxy silane is slowly dripped into the diaminothiourea dissolved in xylene for reaction for 8-12 h;
s2: mixing a, omega-dihydroxy polydimethylsiloxane, a reinforcing filler and a plasticizer to obtain a base material;
s3: and mixing the base material with a cross-linking agent, a curing agent, a sulfhydryl-amino silane coupling agent and a catalyst to obtain the sulfhydryl-amino-containing single-component ketoxime-removing silicone sealant.
3. The method for preparing the single-component ketoxime-free silicone sealant containing the mercapto group-amino group according to claim 2, wherein the mercapto group-amino silane coupling agent has the structural formula:
4. The method for preparing the single-component ketoxime-removing type silicone sealant containing the mercapto-amino group according to claim 2, wherein the viscosity of the alpha, omega-dihydroxypolydimethylsiloxane is 20000-100000 mpa.s at 25 ℃.
5. The method for preparing the single-component ketoxime-removing type silicone sealant containing the mercapto group-amino group according to claim 2, wherein the reinforcing filler is at least one of nano calcium carbonate, heavy calcium carbonate and white carbon black.
6. The method for preparing the single-component ketoxime-removing type silicone sealant containing the mercapto group-amino group according to claim 2, wherein the plasticizer is simethicone, and the viscosity at 25 ℃ is 100-1000 mpa.s.
7. The method for preparing the single-component ketoxime-free silicone sealant containing the mercapto group-amino group according to claim 2, wherein the cross-linking agent is at least one of methyltributyloxidoxime silane, vinyltributylketoxime silane and phenyltributylketoxime silane.
8. The method for preparing the single-component ketoxime-free silicone sealant containing the mercapto-amino group according to claim 2, wherein the mercapto-amino silane coupling agent is at least one of aminopropyl trimethoxy silane, mercaptopropyl trimethoxy silane and mercapto-aminopropyl trimethoxy silane.
9. The method for preparing the single-component ketoxime-removing type silicone sealant containing the mercapto group-amino group according to claim 2, wherein the catalyst is at least one of di-n-butyl tin dilaurate, di-n-butyl tin diacetate and stannous octoate.
10. The preparation method of the single-component ketoxime-removing type silicone sealant containing mercapto groups and amino groups according to claim 2, wherein the step S2 is characterized in that the single-component ketoxime-removing type silicone sealant is heated to 120-130 ℃ and vacuumized for more than-0.095 MPa for 2-3 h; in the step S3, stirring is carried out for 20-40 min at the vacuum degree of more than-0.095 MPa.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410273081.6A CN118085802A (en) | 2024-03-11 | 2024-03-11 | Single-component ketoxime-removing silicone sealant containing sulfhydryl-amino and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410273081.6A CN118085802A (en) | 2024-03-11 | 2024-03-11 | Single-component ketoxime-removing silicone sealant containing sulfhydryl-amino and preparation method thereof |
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| CN118085802A true CN118085802A (en) | 2024-05-28 |
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| CN202410273081.6A Pending CN118085802A (en) | 2024-03-11 | 2024-03-11 | Single-component ketoxime-removing silicone sealant containing sulfhydryl-amino and preparation method thereof |
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| CN (1) | CN118085802A (en) |
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2024
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