CN109438710A - Preparation method of MDT resin for Molding silica gel - Google Patents
Preparation method of MDT resin for Molding silica gel Download PDFInfo
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- CN109438710A CN109438710A CN201811312601.0A CN201811312601A CN109438710A CN 109438710 A CN109438710 A CN 109438710A CN 201811312601 A CN201811312601 A CN 201811312601A CN 109438710 A CN109438710 A CN 109438710A
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- 229920005989 resin Polymers 0.000 title claims abstract description 14
- 239000011347 resin Substances 0.000 title claims abstract description 14
- 238000000465 moulding Methods 0.000 title claims abstract description 10
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 6
- 239000000741 silica gel Substances 0.000 title claims abstract description 6
- 229910002027 silica gel Inorganic materials 0.000 title claims abstract description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 39
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims abstract description 11
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 11
- 239000002253 acid Substances 0.000 claims abstract description 10
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 8
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910000077 silane Inorganic materials 0.000 claims abstract description 6
- 239000003513 alkali Substances 0.000 claims abstract description 5
- 125000003944 tolyl group Chemical group 0.000 claims abstract description 4
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims abstract description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract 5
- 235000019441 ethanol Nutrition 0.000 claims description 23
- 229920002050 silicone resin Polymers 0.000 claims description 13
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 4
- OBNDGIHQAIXEAO-UHFFFAOYSA-N [O].[Si] Chemical compound [O].[Si] OBNDGIHQAIXEAO-UHFFFAOYSA-N 0.000 claims description 4
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 4
- ARYZCSRUUPFYMY-UHFFFAOYSA-N methoxysilane Chemical compound CO[SiH3] ARYZCSRUUPFYMY-UHFFFAOYSA-N 0.000 claims description 3
- ITMCEJHCFYSIIV-UHFFFAOYSA-N triflic acid Chemical compound OS(=O)(=O)C(F)(F)F ITMCEJHCFYSIIV-UHFFFAOYSA-N 0.000 claims description 3
- YBHBEZSZXFLQMW-UHFFFAOYSA-N [dimethoxy(phenyl)silyl]methanamine Chemical group CO[Si](CN)(OC)C1=CC=CC=C1 YBHBEZSZXFLQMW-UHFFFAOYSA-N 0.000 claims description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- 125000001797 benzyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])* 0.000 claims description 2
- YYLGKUPAFFKGRQ-UHFFFAOYSA-N dimethyldiethoxysilane Chemical compound CCO[Si](C)(C)OCC YYLGKUPAFFKGRQ-UHFFFAOYSA-N 0.000 claims description 2
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 2
- 239000011736 potassium bicarbonate Substances 0.000 claims description 2
- 229910000028 potassium bicarbonate Inorganic materials 0.000 claims description 2
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 2
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 claims description 2
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- IUSHZEZOKQKYCP-UHFFFAOYSA-N (2-phenyl-1,4-dioxan-2-yl)methanamine Chemical compound C=1C=CC=CC=1C1(CN)COCCO1 IUSHZEZOKQKYCP-UHFFFAOYSA-N 0.000 claims 1
- RBIILJCATVGHHI-UHFFFAOYSA-N [diethoxy(phenyl)silyl]methanamine Chemical compound NC[Si](OCC)(OCC)C1=CC=CC=C1 RBIILJCATVGHHI-UHFFFAOYSA-N 0.000 claims 1
- 150000001335 aliphatic alkanes Chemical class 0.000 claims 1
- 239000002585 base Substances 0.000 claims 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 7
- 229910052710 silicon Inorganic materials 0.000 abstract description 5
- 239000010703 silicon Substances 0.000 abstract description 5
- 238000010438 heat treatment Methods 0.000 abstract description 4
- 238000004806 packaging method and process Methods 0.000 abstract description 3
- 239000000853 adhesive Substances 0.000 abstract description 2
- 230000001070 adhesive effect Effects 0.000 abstract description 2
- 150000001875 compounds Chemical class 0.000 abstract description 2
- 238000001816 cooling Methods 0.000 abstract description 2
- 239000012744 reinforcing agent Substances 0.000 abstract description 2
- 238000001704 evaporation Methods 0.000 abstract 2
- 239000003292 glue Substances 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 12
- -1 aminomethyl phenyl Chemical group 0.000 description 6
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 238000005538 encapsulation Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 3
- IRTCJFCIQKNFPP-UHFFFAOYSA-N 2-methyl-1,4-dioxane Chemical compound CC1COCCO1 IRTCJFCIQKNFPP-UHFFFAOYSA-N 0.000 description 2
- CWAFVXWRGIEBPL-UHFFFAOYSA-N ethoxysilane Chemical compound CCO[SiH3] CWAFVXWRGIEBPL-UHFFFAOYSA-N 0.000 description 2
- 229920001296 polysiloxane Polymers 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 229920002379 silicone rubber Polymers 0.000 description 2
- JCVQKRGIASEUKR-UHFFFAOYSA-N triethoxy(phenyl)silane Chemical compound CCO[Si](OCC)(OCC)C1=CC=CC=C1 JCVQKRGIASEUKR-UHFFFAOYSA-N 0.000 description 2
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 1
- PLGMEMWRQAABJX-UHFFFAOYSA-N CCN(CC)[SiH](C)OC1=CC=CC=C1 Chemical compound CCN(CC)[SiH](C)OC1=CC=CC=C1 PLGMEMWRQAABJX-UHFFFAOYSA-N 0.000 description 1
- 125000003545 alkoxy group Chemical group 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- CIQDYIQMZXESRD-UHFFFAOYSA-N dimethoxy(phenyl)silane Chemical compound CO[SiH](OC)C1=CC=CC=C1 CIQDYIQMZXESRD-UHFFFAOYSA-N 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical compound [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000006459 hydrosilylation reaction Methods 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 150000003961 organosilicon compounds Chemical class 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/20—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/70—Siloxanes defined by use of the MDTQ nomenclature
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Silicon Polymers (AREA)
Abstract
The invention relates to a preparation method of MDT resin for Molding silica gel, which comprises the following steps: adding acid, dimethyl dialkoxy silane, methyl phenyl dialkoxy silane, phenyl trialkoxy silane, alcohol and water into a four-mouth bottle, stirring, heating to 25 ℃ for reacting for 1-2 hours, dropwise adding the rest total amount of water, vinyl double end socket and hexamethyldisiloxane at room temperature simultaneously after the reaction is finished, controlling the temperature in the system to be 35-40 ℃, reacting for 2-3 hours at 70 ℃ after the dropwise adding is finished, then evaporating the alcohol in the system, then adding toluene and alkali which are more than the theoretical resin amount to adjust the pH of the system to be 9-10, reacting for 1.5 hours at 90 ℃, then heating to evaporate the rest alcohol and water in the system, finally cooling and washing until the pH of the system is 6-7, and rotationally evaporating and removing the toluene at 130 ℃ to obtain the silicon resin; the prepared MDT silicon resin is mainly used as a reinforcing agent of packaging glue, an organic silicon adhesive and an organic silicon molding compound.
Description
Technical field
The present invention relates to a kind of preparation methods of MDT resin for Molding silica gel, belong to the synthetic technology of silicone resin
Field.
Technical background
In recent years, with the development of semiconductor light emitting technology, semiconductor lighting substitute high energy consumption, low light efficiency incandescent lamp
As inexorable trend, cause the extensive concern in the whole world.Organosilicon material is due to its good resistant of high or low temperature and reproducibility, especially
It is the silicon rubber or silicone resin vulcanized by hydrosilylation mode, is that high power LED device is most ideal so far
Encapsulating material, the silicone resin of MDT type is one of organic siliconresin, it by single functionality silicon oxygen chain link (R3SiO1/2,
M chain link), the organosilicons of two degree of functionality silicon oxygen chain links (R2SiO, D chain link) and three-functionality-degree silicon oxygen chain link (RSiO3/2, T chain link)
Monomer is formed through cohydrolysis-polycondensation reaction.
In existing technology, in relation to existing for the general refractive index control of MDT silicone resin used in LED packaging silicon rubber
Between 1.50-1.55, belong to high refractive index silicone；But as LED is using more and more extensive, to LED encapsulation material requirement
Also more higher, and the LED of Molding encapsulating structure has the consistent of light emitting angle compared to direct insertion encapsulation in LED encapsulation
Property high, light emitting angle precisely, the advantages that brightness is higher, be just gradually widely applied.A kind of MDT resin of the present invention preferably meets
LED Molding encapsulates the requirement to cooling thermal impact performance and high-power, large scale, high temperature light decay.
Summary of the invention
For the deficiency of existing MDT silicone resin, the present invention provides a kind of by methyl M link, vinyl M link, methyl D chain
It connects, aminomethyl phenyl D is linked, the synthetic method of the MDT resin of phenyl T link composition.
Technical scheme is as follows:
A kind of preparation method of the MDT resin for Molding silica gel, which is characterized in that acid, two are added in four-hole bottle
Methyl dioxane oxysilane, methyl phenyl di-alkoxy silane, phenyl trialkoxysilane, pure and mild suitable water, stirring, heating
To 25 DEG C reaction 1-2 hours, be added dropwise remaining total water and vinyl double seal head, hexamethyl simultaneously at room temperature after the reaction was completed
Disiloxane, the temperature in control system react 2-3 hours at 70 DEG C after being added dropwise between 30-40 DEG C, then steam body
Then the pH=9-10 of the toluene more than theoretical amount of resin and alkali regulation system is added in alcohol in system, 90 DEG C are reacted 1.5 hours,
Then heating steams remaining alcohol and water in system, finally cools down again, is neutralized with acid, is washed to the pH=6-7 of system；130℃
Toluene is evaporated off up to silicone resin in backspin；
The acid, vinyl double seal head, hexamethyldisiloxane, dimethyldimethoxysil,ne, alcohol, water, aminomethyl phenyl
Dialkoxy silicane, phenyl trialkoxysilane mass ratio be (1.18-1.99): (5.58-38.50): (30.46-
113.24): (60.11-240.44): (11.80-19.95): (50.20-120.80): (182.29-210.35): (198.26-
240.37)。
Preferred according to the present invention, the dimethyldialkylammonium oxysilane is dimethyldimethoxysil,ne or dimethyl two
Ethoxysilane；
It is preferred according to the present invention, the compatibility of increase system is played using alcohol is added and inhibits reaction too fast；
Preferred according to the present invention, the phenyl methyl dialkoxy silicane is aminomethyl phenyl dimethoxysilane or methyl
Diethylamino phenyl oxysilane；
Preferred according to the present invention, the phenyl trialkoxysilane is phenyltrimethoxysila,e, phenyl triethoxy
Silane；
Preferred according to the present invention, the acid is hydrochloric acid, sulfuric acid, phosphoric acid, Emathlite, trifluoromethane sulfonic acid and acidity sun
Ion exchange resin；
Preferred according to the present invention, the dosage of water is phenyl trialkoxysilane, methyl phenyl di-alkoxy silane and two
1.4-2.7 times of methyl dioxane oxysilane total moles quality；
Preferred according to the present invention, the alcohol is ethyl alcohol, methanol；The alkali is Na2CO3、NaHCO3、K2CO3、KHCO3、
NaOH,KOH；
Preferred according to the present invention, speed of agitator is 200-500 revs/min；
Preferred according to the present invention, vinyl mass percent is 2%-7%；
Preferred according to the present invention, the value of R/Si is 1.1-1.8；
Preferred according to the present invention, the MDT silicone resin of synthesis can accurately control alkoxy by deviating from the amount of alcohol
Surplus；
Preferred according to the present invention, the reactor is equipped with thermometer, constant pressure funnel, spherical condensation tube, tetrafluoro
The four round flask of stirring rod.
The MDT silicone resin of invention preparation is mainly used for the reinforcing agent of packaging plastic, organosilicon adhesive and silicone molding compound.
Specific embodiment
Embodiment 1
1.83g concentrated hydrochloric acid, 28.79g dimethyldimethoxysil,ne, 192.34g aminomethyl phenyl two are added in four-hole bottle
Methoxy silane, 200.52g phenyltrimethoxysila,e, 14.78g ethyl alcohol and 5g water stir, are heated to 25 DEG C of reactions 2 hours, instead
62.10g water and 17.25g vinyl double seal head, 68.21g hexamethyldisiloxane should be added dropwise simultaneously at room temperature after the completion, control
Temperature in system processed reacts 2.5 hours at 70 DEG C after being added dropwise between 30-40 DEG C, then steams the alcohol in system, so
300g toluene and suitable Na are added afterwards2CO3The pH=10 of regulation system, 90 DEG C are reacted 1.5 hours, then heat to 130 DEG C of steamings
Remaining alcohol and water in system out finally cools down again, is neutralized with acetic acid, is washed to the pH=6-7 of system；130 DEG C of backspins are evaporated off
Go toluene up to silicone resin；Its yield is 95.6%.
Embodiment 2
1.74g concentrated hydrochloric acid, 31.56g dimethyl diethoxysilane, 198.42g aminomethyl phenyl two are added in four-hole bottle
Ethoxy silane, 231.05g phenyl triethoxysilane, 15.10g ethyl alcohol and 5g water stir, are heated to 25 DEG C of reactions 1.5 hours,
57.40g water and 15.13g vinyl double seal head, 66.42g hexamethyldisiloxane is added dropwise simultaneously at room temperature after the reaction was completed,
Temperature in control system reacts 2 hours at 70 DEG C after being added dropwise between 30-40 DEG C, then steams the alcohol in system, so
300g toluene and suitable NaHCO are added afterwards3The pH=10 of regulation system, 90 DEG C are reacted 1.5 hours, then heat to 130 DEG C
Remaining alcohol and water in system is steamed, is finally cooled down again, is neutralized with acetic acid, is washed to the pH=6-7 of system；It is rotated at 130 DEG C
Toluene is removed up to silicone resin, yield 95%.
Embodiment 3
The 1.58g concentrated sulfuric acid, 32.45g dimethyldimethoxysil,ne, 185.63g aminomethyl phenyl two are added in four-hole bottle
The pure and mild 5g water of methoxy silane, 200.67g phenyltrimethoxysila,e, 15.10g stirs, is heated to 25 DEG C of reactions 2 hours, reaction
57.40g water and 15.13g vinyl double seal head, 68.54g hexamethyldisiloxane is added dropwise simultaneously at room temperature after the completion, controls
Temperature in system reacts 2 hours at 70 DEG C after being added dropwise between 30-40 DEG C, then steams the alcohol in system, then plus
Enter the pH=10 of 300g toluene and suitable NaOH regulation system, 90 DEG C are reacted 1.5 hours, are then heated to 130 DEG C and are steamed body
Remaining alcohol and water in being finally cools down again, is neutralized with acetic acid, is washed to the pH=6-7 of system；First is evaporated off in 130 DEG C of backspins
Benzene is up to silicone resin；Its yield is 94.5%.
Embodiment 4
1.580g trifluoromethane sulfonic acid, 32.45g dimethyldimethoxysil,ne, 187.63g methyl are added in four-hole bottle
Phenyl dimethoxy silane, 197.52g phenyltrimethoxysila,e, 15.10g methanol and 5g water stir, are heated to 25 DEG C of reactions 2
Hour, 57.40g water and 15.13g vinyl double seal head, two silicon of 65.42g hexamethyl is added dropwise simultaneously at room temperature after the reaction was completed
Oxygen alkane, the temperature in control system are reacted 2 hours at 70 DEG C after being added dropwise, are then steamed in system between 30-40 DEG C
Then the pH=10 of 300g toluene and suitable KOH regulation system is added in alcohol, 90 DEG C are reacted 1 hour, then heats to 130 DEG C
Remaining alcohol and water in system is steamed, is finally cooled down again, is neutralized with acetic acid, is washed to the pH=6-7 of system；It is rotated at 130 DEG C
Toluene is removed up to silicone resin；Its yield is 93.9%.
Claims (2)
1. a kind of preparation method of the MDT resin for Molding silica gel, which is characterized in that acid, diformazan are added in four-hole bottle
Base dialkoxy silicane, methyl phenyl di-alkoxy silane, phenyl trialkoxysilane, alcohol and water stir, are heated to 25 DEG C instead
It answers 1-2 hours, remaining total water and vinyl double seal head, two silicon oxygen of hexamethyl is added dropwise simultaneously at room temperature after the reaction was completed
Alkane, the temperature in control system are reacted 2-3 hours at 70 DEG C after being added dropwise, are then steamed in system between 30-40 DEG C
Then the pH=9-10 of the toluene more than theoretical amount of resin and alkali regulation system is added in alcohol, 90 DEG C are reacted 1.5 hours, then rises
Temperature steams remaining alcohol and water in system, finally cools down again, is neutralized with acid, is washed to the pH=6-7 of system；It is rotated at 130 DEG C
Toluene is removed up to silicone resin；
The acid, vinyl double seal head, hexamethyldisiloxane, dimethyldimethoxysil,ne, alcohol, water, aminomethyl phenyl dioxane
Oxysilane, phenyl trialkoxysilane mass ratio be (1.18-1.99): (5.58-38.50): (30.46-113.24):
(60.11-240.44): (11.80-19.95): (50.20-120.80): (182.29-210.35): (198.26-240.37).
2. preparation method according to claim 1, which is characterized in that the dimethyldialkylammonium oxysilane is dimethyl two
Methoxy silane or dimethyl diethoxysilane；The phenyl methyl dialkoxy silicane is aminomethyl phenyl dimethoxysilane
Or aminomethyl phenyl diethoxy silane；The acid be hydrochloric acid, sulfuric acid, phosphoric acid, Emathlite, trifluoromethane sulfonic acid and acid sun from
One of sub-exchange resin；The alcohol is one of ethyl alcohol, methanol；The alkali is Na2CO3、NaHCO3、K2CO3、KHCO3、
One of NaOH, KOH.
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| Application Number | Priority Date | Filing Date | Title |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111592766A (en) * | 2020-05-20 | 2020-08-28 | 宿迁市同创化工科技股份有限公司 | Preparation method of high-insulation solvent-free silicone resin for composite insulator |
| CN113025054A (en) * | 2019-12-25 | 2021-06-25 | 新特能源股份有限公司 | Silicon rubber composition, preparation method thereof and packaging adhesive |
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| CN108003347A (en) * | 2017-11-23 | 2018-05-08 | 烟台德邦先进硅材料有限公司 | A kind of preparation method for high-power encapsulation MDT silicones |
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2018
- 2018-11-06 CN CN201811312601.0A patent/CN109438710A/en active Pending
Patent Citations (2)
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| CN106866968A (en) * | 2017-03-02 | 2017-06-20 | 烟台德邦先进硅材料有限公司 | A kind of cyclohexyl organic siliconresin and preparation method thereof |
| CN108003347A (en) * | 2017-11-23 | 2018-05-08 | 烟台德邦先进硅材料有限公司 | A kind of preparation method for high-power encapsulation MDT silicones |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113025054A (en) * | 2019-12-25 | 2021-06-25 | 新特能源股份有限公司 | Silicon rubber composition, preparation method thereof and packaging adhesive |
| CN111592766A (en) * | 2020-05-20 | 2020-08-28 | 宿迁市同创化工科技股份有限公司 | Preparation method of high-insulation solvent-free silicone resin for composite insulator |
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Address after: No.3-3, Kaifeng Road, Yantai Economic and Technological Development Zone, Shandong Province 264006 Applicant after: Yantai Debang Technology Co.,Ltd. Address before: No.3-3 Kaifeng Road, Yantai Development Zone, Shandong Province Applicant before: DARBOND TECHNOLOGY Co.,Ltd. |
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Application publication date: 20190308 |