CN108864709A - A kind of preparation method of silicone rubber crosslinking agent - Google Patents
A kind of preparation method of silicone rubber crosslinking agent Download PDFInfo
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- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/34—Heterocyclic compounds having nitrogen in the ring
- C08K5/3412—Heterocyclic compounds having nitrogen in the ring having one nitrogen atom in the ring
- C08K5/3432—Six-membered rings
- C08K5/3435—Piperidines
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
- C08K2003/382—Boron-containing compounds and nitrogen
- C08K2003/385—Binary compounds of nitrogen with boron
Abstract
The invention discloses a kind of preparation methods of silicone rubber crosslinking agent, belong to chemical technology field.Isopropanol dissolution is added with ethyl orthosilicate in the present invention, forms the stereochemical structure piled up, it is bis- to add 1,3-（3- aminopropyl）- 1,1,3,3- tetramethyl disiloxane is blocked, and polymer is formed；It is bis- that 1,3- is added（3- aminopropyl）- 1,1,3,3- tetramethyl disiloxane carries out amidation process, obtains cross linker base.The polyamino in dendritic structure in cross linker base end group produces Concentrative crosslinking effect during being crosslinked again, add methyl Chloropropylpolysiloxanes compounding, end group has intensive N-H in cross linker base, there are enough activity to be reacted with chloropropyl, Concentrative crosslinking is generated in silicon rubber, so that the stretching of silicon rubber and tearing strength are improved, the present invention is solved for current crosslinking agent there are heat resistances lower, the lower problem of intensity.
Description
Technical field
The invention belongs to chemical technology field more particularly to a kind of preparation methods of silicone rubber crosslinking agent.
Background technique
Crosslinking agent is also referred to as bridging agent, is the important component of poly- hydro carbons photoresist, this photoresist
Photochemical solidification effect, dependent on the crosslinking agent participation reaction for having double photonasty functional groups, generation is double certainly after crosslinking agent exposure
By base, it and poly- hydrocarbon resins phase separation form bridged bond between polymer molecular chain, become the insoluble object of three-dimensional structure
Matter.It is often the substance containing multiple functional groups in molecule, such as organic dibasic acid, polyalcohol；Or intramolecular contains multiple insatiable hungers
With the compound of double bond, such as divinylbenzene and diisocyanate, N, N- methylene-bisacrylamide（MBA）Deng.It can same monomer
It feeds intake together, to polycondensation（Or polymerization）It crosslinks to a certain extent, product is made to become insoluble cross-linked polymer；It can also be online
Retain a certain number of functional groups in type molecule（Or double bond）, add predetermined substance and be crosslinked, such as the solidification of phenolic resin
With the vulcanization of rubber etc..Crosslinking agent is used primarily in high molecular material（Rubber and thermosetting resin）In.Because high molecular material
The molecular structure line long as a rule, intensity is low when not being crosslinked, and easily breaks, and without elasticity, the effect of crosslinking agent be exactly
Chemical bond is generated between the molecule of line style, is connected with each other linear molecule, forms reticular structure, raising rubber is strong in this way
It spends and elastic, the crosslinking agent in rubber is mainly sulphur, in addition to add promotor.The main function of crosslinking agent has：1）It is a variety of
Thermoplastic（Polyethylene, polyvinyl chloride, haloflex, EVA, polystyrene etc.）Crosslinking and modification.Heat cross-linking generally adds
Dosage is 1 ~ 3%, separately plus cumyl peroxide（DCP）It is 0.2 ~ 1%；Cross-linking radiation additive amount is 0.5 ~ 2%, can no longer be added
DCP.Heat resistance, anti-flammability, solvent resistance, mechanical strength and the electrical property etc. of product are remarkably improved after crosslinking.It is than independent
Product quality, and free from extraneous odour will be significantly increased using peroxide systems crosslinking.It is typically used for polyethylene, polyethylene/chlorination
Polyethylene, polyethylene/EVA crosslinked cable and the high and low foaming product of polyethylene.2）The spies such as EP rubbers, various fluorubber, CPE
Kind rubber helps vulcanization（It is used in combination with DCP, general dosage is 0.5-4%）, it can be significantly reduced vulcanization time, intensity is improved, is wear-resisting
Property, solvent resistant and corrosion resistance.3）The crosslinking of acrylic acid, benzethylene type ion exchange resin.It is used than divinylbenzene crosslink agent
It measures less, quality height, the splendid amberlite of performances such as big anti-pollution, intensity, large aperture, heat-resisting, acid and alkali-resistance, anti-oxidant can be prepared
Ester.
Summary of the invention
The technical problems to be solved by the invention：For current crosslinking agent, that there are heat resistances is lower, and intensity is lower to ask
Topic, provides a kind of preparation method of silicone rubber crosslinking agent.
In order to solve the above technical problems, the present invention is using technical solution as described below：
A kind of preparation method of silicone rubber crosslinking agent, which is characterized in that the preparation method includes the following steps：
（1）Take ethyl orthosilicate in mass ratio 3 ~ 5：10~13：8 ~ 10 are added water, isopropanol, are passed through nitrogen protection, it is warming up to 45 ~
55 DEG C are stirred, and add the sulfuric acid that the mass fraction of ethyl orthosilicate quality 40 ~ 50% is 80%, mixed in 40 ~ 45 DEG C of stirrings
It closes, obtains stirring mixture；
（2）Take stirring mixture in mass ratio 10 ~ 15：2 ~ 4 addition 1,3- are bis-（3- aminopropyl）Two silicon of -1,1,3,3- tetramethyl
Oxygen alkane is warming up to 65 ~ 75 DEG C and is stirred, obtains mixture, takes mixture in mass ratio 1：5 ~ 7 are added toluene extraction, adjust pH
To 5 ~ 6, extract liquor rotary evaporation is taken, rotary evaporation object is obtained；
（3）Take rotary evaporation object in mass ratio 1：2~4：1 ~ 3 is added toluene, methanol mixing, is passed through argon gas protection, is stirred,
Mixed liquor A is obtained, methyl acrylate in mass ratio 1 ~ 3 is taken：2~4：1 ~ 3 is added toluene, methanol mixing, is stirred in 25 ~ 30 DEG C,
Mixed liquid B is obtained, mixed liquid B in mass ratio 2 ~ 5 is taken：3 ~ 7 are added dropwise in mixed liquor A, control 20 ~ 30min of time for adding, are warming up to
45 ~ 50 DEG C are stirred, and vacuum distillation obtains vacuum distillation object；
（4）Take vacuum distillation object in mass ratio 1：3~5：2 ~ 4 are added toluene, methanol mixing, add vacuum distillation amount of substance 5 ~ 7
1,3- again is bis-（3- aminopropyl）- 1,1,3,3- tetramethyl disiloxane is passed through argon gas protection, is warming up to 45 ~ 50 DEG C of stirrings
Mixing, must stir mixture A, take stirring mixture A in mass ratio 1：4 ~ 6 are added anhydrous methanol, stand, and filtering takes filtrate to revolve
Turn evaporation, obtains crosslinking agent matrix object；
（5）According to the mass fraction, 100 ~ 200 parts of crosslinking agent matrix objects, 12 ~ 15 parts of tetramethyl piperidine amine, 15 ~ 20 parts of oxidation stones are taken
Black alkene, 5 ~ 7 parts of boron nitride, 6 ~ 9 parts of titanium dioxide mixing, are warming up to 45 ~ 55 DEG C and are stirred to get silicone rubber crosslinking agent.
The present invention is compared with other methods, and advantageous effects are：
（1）Isopropanol dissolution is added with ethyl orthosilicate in the present invention, forms the stereochemical structure piled up, it is bis- to add 1,3-（3- ammonia
Base propyl）- 1,1,3,3- tetramethyl disiloxane is blocked, and polymer is formed, and polymer passes through amine alkene reaction and acrylic acid
Addition reaction occurs for methyl esters, forms ester terminated polysiloxane species, it is bis- to add 1,3-（3- aminopropyl）-1,1,3,3-
Tetramethyl disiloxane carries out amidation process, obtains cross linker base；
（2）The polyamino in dendritic structure in cross linker base end group produced by the present invention produces during being crosslinked again
Concentrative crosslinking effect adds methyl Chloropropylpolysiloxanes compounding, and end group has intensive N-H in cross linker base, there is foot
Enough activity are reacted with chloropropyl, Concentrative crosslinking are generated in silicon rubber, so that the stretching of silicon rubber and tearing strength obtain
To raising, by contact steam hydrolysis occurs rapidly for hydrolyzable functional group in crosslinking agent, generates Si-OH, and then with
Condensation cross-linking reaction occurs for the Si-OH in base rubber, removes small molecule, forms tridimensional network, while inhibiting methyl chloride third
The thermal degradation of based polysiloxane chain and crosslinking points enhances heat resistance to improve its hot property；
（3）The present invention is since silicon rubber is easy to generate free radical under ultraviolet light, although very because of radical reaction activity
Height can be cracked to form gas and small-molecule substance, while free radical will continue to crosslink reaction, obtain cross-linked network, but
Prolonged irradiation can make the mechanicalness of silicon rubber be lower, aging is added tetramethyl piperidine amine, aoxidizes stone so that material becomes fragile
Black alkene has efficient quenching effect to hydroxyl radical free radical, reduces the generation and control cross-linking reaction of radiation cleavage, prevents from handing over
Connection density is excessively high, so that the rearrangement ability of polymer chain reduces when crystallization, to guarantee that crosslinking agent plays a role.
Specific embodiment
A kind of preparation method of silicone rubber crosslinking agent, includes the following steps：
（1）Take ethyl orthosilicate in mass ratio 3 ~ 5：10~13：8 ~ 10 are added water, isopropanol, are passed through nitrogen protection, it is warming up to 45 ~
55 DEG C are stirred 5 ~ 10min, the sulfuric acid that the mass fraction of ethyl orthosilicate quality 40 ~ 50% is 80% are added, in 40 ~ 45 DEG C
It is stirred 1 ~ 2h, obtains stirring mixture；
（2）Take stirring mixture in mass ratio 10 ~ 15：2 ~ 4 addition 1,3- are bis-（3- aminopropyl）Two silicon of -1,1,3,3- tetramethyl
Oxygen alkane is warming up to 65 ~ 75 DEG C and is stirred 2 ~ 3h, obtains mixture, takes mixture in mass ratio 1：5 ~ 7 are added toluene extraction, adjust
PH to 5 ~ 6 is saved, extract liquor rotary evaporation is taken, obtains rotary evaporation object；
（3）Take rotary evaporation object in mass ratio 1：2~4：1 ~ 3 is added toluene, methanol mixing, is passed through argon gas protection, is stirred 30
~ 40min, obtains mixed liquor A, takes methyl acrylate in mass ratio 1 ~ 3：2~4：1 ~ 3 is added toluene, methanol mixing, stirs in 25 ~ 30 DEG C
20 ~ 30min of mixing is mixed, mixed liquid B is obtained, takes mixed liquid B in mass ratio 2 ~ 5：3 ~ 7 are added dropwise in mixed liquor A, control time for adding
20 ~ 30min is warming up to 45 ~ 50 DEG C and is stirred 36 ~ 48h, and vacuum distillation obtains vacuum distillation object；
（4）Take vacuum distillation object in mass ratio 1：3~5：2 ~ 4 are added toluene, methanol mixing, add vacuum distillation amount of substance 5 ~ 7
1,3- again is bis-（3- aminopropyl）- 1,1,3,3- tetramethyl disiloxane is passed through argon gas protection, is warming up to 45 ~ 50 DEG C of stirrings
12 ~ 15h is mixed, mixture A must be stirred, takes stirring mixture A in mass ratio 1：4 ~ 6 are added anhydrous methanol, stand 2 ~ 3h, mistake
Filter, takes filtrate rotary evaporation, obtains crosslinking agent matrix object；
（5）According to the mass fraction, 100 ~ 200 parts of crosslinking agent matrix objects, 50 ~ 60 parts of methyl Chloropropylpolysiloxanes, 12 ~ 15 parts are taken
Tetramethyl piperidine amine, 15 ~ 20 parts of graphene oxides, 5 ~ 7 parts of boron nitride, 6 ~ 9 parts of titanium dioxide mixing, are warming up to 45 ~ 55 DEG C and stir
2 ~ 3h of mixing is mixed to get silicone rubber crosslinking agent.
A kind of preparation method of silicone rubber crosslinking agent, includes the following steps：
（1）Take ethyl orthosilicate in mass ratio 3：10：8 are added water, isopropanol, are passed through nitrogen protection, and it is mixed to be warming up to 45 DEG C of stirrings
5min is closed, the sulfuric acid that the mass fraction of ethyl orthosilicate quality 40% is 80% is added, is stirred 1h in 40 DEG C, must be stirred mixed
Close object；
（2）Take stirring mixture in mass ratio 10：2 addition 1,3- are bis-（3- aminopropyl）- 1,1,3,3- tetramethyl disiloxane,
It is warming up to 65 DEG C and is stirred 2h, obtain mixture, take mixture in mass ratio 1：5 are added toluene extraction, adjust pH to 5, take extraction
Liquid rotary evaporation is taken, rotary evaporation object is obtained；
（3）Take rotary evaporation object in mass ratio 1：2：1 is added toluene, methanol mixing, is passed through argon gas protection, is stirred 30min,
Mixed liquor A is obtained, methyl acrylate in mass ratio 1 is taken：2：1 is added toluene, methanol mixing, is stirred 20min in 25 DEG C, obtains mixed
Liquid B is closed, mixed liquid B in mass ratio 2 is taken：3 are added dropwise in mixed liquor A, control time for adding 20min, and it is mixed to be warming up to 45 DEG C of stirrings
36h is closed, vacuum distillation obtains vacuum distillation object；
（4）Take vacuum distillation object in mass ratio 1：3：2 are added toluene, methanol mixing, add the 1 of 5 times of amount of substance of vacuum distillation,
3- is bis-（3- aminopropyl）- 1,1,3,3- tetramethyl disiloxane is passed through argon gas protection, is warming up to 45 DEG C and is stirred 12h, obtain
Mixture A is stirred, stirring mixture A in mass ratio 1 is taken：4 are added anhydrous methanol, stand 2h, and filtering takes filtrate rotary evaporation,
Obtain crosslinking agent matrix object；
（5）According to the mass fraction, 100 parts of crosslinking agent matrix objects, 50 parts of methyl Chloropropylpolysiloxanes, 12 parts of tetramethyl piperidines are taken
Amine, 15 parts of graphene oxides, 5 parts of boron nitride, 6 parts of titanium dioxide mixing are warming up to 45 DEG C and are stirred 2h to get silicon rubber friendship
Join agent.
A kind of preparation method of silicone rubber crosslinking agent, includes the following steps：
（1）Take ethyl orthosilicate in mass ratio 4：12：9 are added water, isopropanol, are passed through nitrogen protection, and it is mixed to be warming up to 50 DEG C of stirrings
8min is closed, the sulfuric acid that the mass fraction of ethyl orthosilicate quality 45% is 80% is added, is stirred 1.5h in 43 DEG C, must stir
Mixture；
（2）Take stirring mixture in mass ratio 13：3 addition 1,3- are bis-（3- aminopropyl）- 1,1,3,3- tetramethyl disiloxane,
It is warming up to 70 DEG C and is stirred 2.5h, obtain mixture, take mixture in mass ratio 1：6 are added toluene extraction, adjust pH to 5.5,
Extract liquor rotary evaporation is taken, rotary evaporation object is obtained；
（3）Take rotary evaporation object in mass ratio 1：3：2 are added toluene, methanol mixing, are passed through argon gas protection, are stirred 35min,
Mixed liquor A is obtained, methyl acrylate in mass ratio 2 is taken：3：2 are added toluene, methanol mixing, are stirred 25min in 28 DEG C, obtain mixed
Liquid B is closed, mixed liquid B in mass ratio 4 is taken：5 are added dropwise in mixed liquor A, control time for adding 25min, and it is mixed to be warming up to 48 DEG C of stirrings
42h is closed, vacuum distillation obtains vacuum distillation object；
（4）Take vacuum distillation object in mass ratio 1：4：3 are added toluene, methanol mixing, add the 1 of 6 times of amount of substance of vacuum distillation,
3- is bis-（3- aminopropyl）- 1,1,3,3- tetramethyl disiloxane is passed through argon gas protection, is warming up to 48 DEG C and is stirred 14h, obtain
Mixture A is stirred, stirring mixture A in mass ratio 1 is taken：5 are added anhydrous methanol, stand 2.5h, and filtering takes filtrate rotation to steam
Hair, obtains crosslinking agent matrix object；
（5）According to the mass fraction, 150 parts of crosslinking agent matrix objects, 55 parts of methyl Chloropropylpolysiloxanes, 14 parts of tetramethyl piperidines are taken
Amine, 18 parts of graphene oxides, 6 parts of boron nitride, 8 parts of titanium dioxide mixing, are warming up to 50 DEG C and are stirred 2.5h to get silicon rubber
Crosslinking agent.
A kind of preparation method of silicone rubber crosslinking agent, includes the following steps：
（1）Take ethyl orthosilicate in mass ratio 5：13：10 are added water, isopropanol, are passed through nitrogen protection, and it is mixed to be warming up to 55 DEG C of stirrings
10min is closed, the sulfuric acid that the mass fraction of ethyl orthosilicate quality 50% is 80% is added, is stirred 2h in 45 DEG C, must stir
Mixture；
（2）Take stirring mixture in mass ratio 15：4 addition 1,3- are bis-（3- aminopropyl）- 1,1,3,3- tetramethyl disiloxane,
It is warming up to 75 DEG C and is stirred 3h, obtain mixture, take mixture in mass ratio 1：7 are added toluene extraction, adjust pH to 6, take extraction
Liquid rotary evaporation is taken, rotary evaporation object is obtained；
（3）Take rotary evaporation object in mass ratio 1：4：3 are added toluene, methanol mixing, are passed through argon gas protection, are stirred 40min,
Mixed liquor A is obtained, methyl acrylate in mass ratio 3 is taken：4：3 are added toluene, methanol mixing, are stirred 30min in 30 DEG C, obtain mixed
Liquid B is closed, mixed liquid B in mass ratio 5 is taken：7 are added dropwise in mixed liquor A, control time for adding 30min, and it is mixed to be warming up to 50 DEG C of stirrings
48h is closed, vacuum distillation obtains vacuum distillation object；
（4）Take vacuum distillation object in mass ratio 1：5：4 are added toluene, methanol mixing, add the 1 of 7 times of amount of substance of vacuum distillation,
3- is bis-（3- aminopropyl）- 1,1,3,3- tetramethyl disiloxane is passed through argon gas protection, is warming up to 50 DEG C and is stirred 15h, obtain
Mixture A is stirred, stirring mixture A in mass ratio 1 is taken：6 are added anhydrous methanol, stand 3h, and filtering takes filtrate rotary evaporation,
Obtain crosslinking agent matrix object；
（5）According to the mass fraction, 200 parts of crosslinking agent matrix objects, 60 parts of methyl Chloropropylpolysiloxanes, 15 parts of tetramethyl piperidines are taken
Amine, 20 parts of graphene oxides, 7 parts of boron nitride, 9 parts of titanium dioxide mixing are warming up to 55 DEG C and are stirred 3h to get silicon rubber friendship
Join agent.
Comparative example：The crosslinking agent of certain company production in the market.
By 1,2,3 sample of embodiment and comparative example of above-mentioned preparation method according to GB/T14683-2003 respectively in temperature height
It is detected under conditions of -10 DEG C, -50 DEG C, 120 DEG C, 150 DEG C, test result is recorded in table 1.
Table 1：
| Test item | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example |
| Cured strength/MPa | 1.62 | 1.69 | 1.72 | 1.05 |
| Colloidal state for 24 hours at -10 DEG C | Without crystal grain | Without crystal grain | Without crystal grain | There is micro crystal to be precipitated |
| Colloidal state for 24 hours at -50 DEG C | Without crystal grain | Without crystal grain | Without crystal grain | There are a large amount of crystal grains |
| Colloidal state for 24 hours at 120 DEG C | Without crystal grain | Without crystal grain | Without crystal grain | There is micro crystal to be precipitated |
| Colloidal state for 24 hours at 150 DEG C | Without crystal grain | Without crystal grain | Without crystal grain | There are a large amount of crystal grains |
In conclusion as shown in Table 1, silicone rubber crosslinking agent heat resistance of the invention is preferable, and intensity is higher than with the production of technology class
Product, be worth promoting use.
Claims (1)
1. a kind of preparation method of silicone rubber crosslinking agent, which is characterized in that the preparation method includes the following steps：
（1）Take ethyl orthosilicate in mass ratio 3 ~ 5：10~13：8 ~ 10 are added water, isopropanol, are passed through nitrogen protection, it is warming up to 45 ~
55 DEG C are stirred, and add the sulfuric acid that the mass fraction of ethyl orthosilicate quality 40 ~ 50% is 80%, mixed in 40 ~ 45 DEG C of stirrings
It closes, obtains stirring mixture；
（2）Take stirring mixture in mass ratio 10 ~ 15：2 ~ 4 addition 1,3- are bis-（3- aminopropyl）Two silicon of -1,1,3,3- tetramethyl
Oxygen alkane is warming up to 65 ~ 75 DEG C and is stirred, obtains mixture, takes mixture in mass ratio 1：5 ~ 7 are added toluene extraction, adjust pH
To 5 ~ 6, extract liquor rotary evaporation is taken, rotary evaporation object is obtained；
（3）Take rotary evaporation object in mass ratio 1：2~4：1 ~ 3 is added toluene, methanol mixing, is passed through argon gas protection, is stirred,
Mixed liquor A is obtained, methyl acrylate in mass ratio 1 ~ 3 is taken：2~4：1 ~ 3 is added toluene, methanol mixing, is stirred in 25 ~ 30 DEG C,
Mixed liquid B is obtained, mixed liquid B in mass ratio 2 ~ 5 is taken：3 ~ 7 are added dropwise in mixed liquor A, control 20 ~ 30min of time for adding, are warming up to
45 ~ 50 DEG C are stirred, and vacuum distillation obtains vacuum distillation object；
（4）Take vacuum distillation object in mass ratio 1：3~5：2 ~ 4 are added toluene, methanol mixing, add vacuum distillation amount of substance 5 ~ 7
1,3- again is bis-（3- aminopropyl）- 1,1,3,3- tetramethyl disiloxane is passed through argon gas protection, is warming up to 45 ~ 50 DEG C of stirrings
Mixing, must stir mixture A, take stirring mixture A in mass ratio 1：4 ~ 6 are added anhydrous methanol, stand, filtering,（5）Take filtrate
Rotary evaporation obtains crosslinking agent matrix object；
According to the mass fraction, 100 ~ 200 parts of crosslinking agent matrix objects, 12 ~ 15 parts of tetramethyl piperidine amine, 15 ~ 20 parts of graphite oxides are taken
Alkene, 5 ~ 7 parts of boron nitride, 6 ~ 9 parts of titanium dioxide mixing, are warming up to 45 ~ 55 DEG C and are stirred to get silicone rubber crosslinking agent.
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| CN111484746A (en) * | 2020-04-28 | 2020-08-04 | 四川童燊防水工程有限公司 | Novel high polymer creeping grouting material and manufacturing process thereof |
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