CN110092913A - A kind of MQ resin of the base containing Si-H and preparation method thereof - Google Patents
A kind of MQ resin of the base containing Si-H and preparation method thereof Download PDFInfo
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- CN110092913A CN110092913A CN201910104354.3A CN201910104354A CN110092913A CN 110092913 A CN110092913 A CN 110092913A CN 201910104354 A CN201910104354 A CN 201910104354A CN 110092913 A CN110092913 A CN 110092913A
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- 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
- C08G77/12—Polysiloxanes containing silicon bound to hydrogen
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- 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
- C08G77/42—Block-or graft-polymers containing polysiloxane sequences
- C08G77/44—Block-or graft-polymers containing polysiloxane sequences containing only polysiloxane sequences
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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- 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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- Silicon Polymers (AREA)
Abstract
The application discloses a kind of MQ resin of base containing Si-H, and the mass fraction of the Si-H of the MQ resin of the base containing Si-H is in the range of 0.07%-1.2%, MwIn the range of 4000g/mol-6000g/mol, softening point is in the range of 100 DEG C -400 DEG C.The preparation method of the MQ resin of the base containing Si-H is also disclosed in the application: the solution of MQ resin and Emathlite being mixed, are then refluxed for reacting, and the moisture that reaction generates is separated out；Radical siloxane containing Si-H and catalyst are added in solution after the reaction, the reaction was continued, obtains the MQ resin of the base containing Si-H.The crosslinking agent that Si―H addition reaction silicon sulfide ketone casting glue can be prepared with the MQ resin of the base containing Si-H has the characteristics that the compound viscosity of preparation is lesser, can be also used for the intermediate of modified MQ resin.
Description
Technical field
This application involves but be not limited to technical field of material chemistry, be particularly, but not limited to a kind of base containing Si-H MQ resin and
Preparation method, the application further relate to the sizing material of the MQ resin comprising the base containing Si-H.
Background technique
Methyl hydrogen silicon polyoxy alkane is the necessary crosslinking agent of hydrosilylation, generally with common end group (CH)3SiO1/2Chain
Methylhydrogenpolysi,oxane is connect, the toughness, intensity of product have very with adding compared with the MQ resin containing Si-H of molal weight after crosslinking
Big difference.Common methyl hydrogen siloxane is all alkaline process production, will cause dehydrogenation hinge, the product strength prepared, toughness, color
Deng all existing defects.The directly use of MQ resin can cause sizing material viscosity and increase, store unstable, and remaining Si-OH base will cause
Dehydrogenation reaction, hinge；If the partial size of product is big, with sizing material poor dispersion without spray drying.
No matter take sodium metasilicate method or esters of silicon acis method to prepare MQ resin, contains a certain amount of Si-OH base, Si-OH base
Dehydrogenation reaction occurs with Si-H base in equilibration reaction, influences the introduction volume of Si-H base.In the prior art, 1,1,3,3- tetra-
Tetramethyldisiloxane and positive esters of silicon acis are directly synthetically prepared the MQ resin of the base containing Si-H under concentrated hydrochloric acid, have largely comprising first
The waste water solution of alcohol, hydrochloric acid, subsequent processing is extremely difficult, pollutes environment.
Summary of the invention
It is the general introduction to the theme being described in detail herein below.This general introduction is not the protection model in order to limit claim
It encloses.
The application provides a kind of MQ resin of base containing Si-H, is first dehydrated Si-OH base MQ resin under Emathlite catalysis
Condensation, is not conformed to the MQ resin of Si-OH, then react with being balanced of siloxanes of Si-H base substantially, can quantitatively be introduced
Si-H base, prepares the MQ resin of the base containing Si-H, and the mass fraction of Si-H base can achieve 0.07%-1.2%.
Specifically, this application provides a kind of MQ resin of base containing Si-H, the Si-H's of the MQ resin of the base containing Si-H
Mass fraction is in the range of 0.07%-1.2%, MWIn the range of 4000g/mol-6000g/mol, softening point 100 DEG C-
In the range of 400 DEG C.
The application also provides the preparation method of the MQ resin of the base containing Si-H, and the preparation method includes:
(1) solution of MQ resin and Emathlite are mixed, are then refluxed for reacting by Si-OH base Seal treatment, and will
The moisture that reaction generates separates out；
(2) silicon of base containing Si-H oxygen is added in the solution after step (1) separation water outlet in the preparation of the MQ resin of the base containing Si-H
Alkane and catalyst, the reaction was continued, then neutralizes, cooling, stands, and filtering steams solvent under decompression, obtains containing the Si-H base
MQ resin.
In this application, the solution of the MQ resin can for the toluene solution of the MQ resin, xylene solution, just oneself
Any one of alkane solution, n-heptane solution or more.
In this application, the siloxanes containing Si-H is hydrogeneous double seal head or structural formula is MeSiO (MeHSiO)nSiM3
Or (MeHSiO)n M2The silicone oil of SiO.
In this application, the catalyst can be trifluoromethayl sulfonic acid or Emathlite.
In this application, the solid content of the solution of the MQ resin can be 60%-70%,
The mass ratio of the MQ resin and Emathlite are as follows: 80-120: 1,
The mass ratio of the MQ resin and the radical siloxane containing Si-H are as follows: 10-20: 1.
In this application, in step (1), back flow reaction can continue -6 hours 5 hours.
In this application, in step (1), infrared spectrum analysis (infrared spectra can be passed through
Analysis, FT-IR analysis) 3700cm in Indicator Reaction solution-1, 3500cm-1Absorption peak disappears, and confirmation reaction reaches terminal.
It in this application, can the reaction was continued at 70 DEG C -90 DEG C in step (2)
In this application, in step (2), 6-8 hours can be continued so that the reaction was continued
In this application, in step (2), can at 70 DEG C -90 DEG C, the reaction was continued continue 6-8 hours
It in this application, can be in the ammonium hydrogen carbonate for being 0.2% with mass concentration and 2 hours -4 small in step (2)
When.
The application also provides a kind of sizing material, the MQ resin comprising the base containing Si-H.
In the embodiment of the application, by MQ resin, toluene is added there-necked flask, after mixed dissolution, is added acid
Carclazyte, after being uniformly mixed, back flow reaction 6 hours, and the water that condensation generates is separated and gathered up by steam-water separator
Come.3700cm in Indicator Reaction solution is analyzed by FT-IR-1, 3500cm-1Absorption peak disappears, and confirmation reaction reaches terminal.?
In above-mentioned reaction solution, hydrogeneous double seal head is added, trifluoromethayl sulfonic acid continues to be stirred to react 8 hours at 70 DEG C.Then it uses
It is cooling in 0.2% part of ammonium hydrogen carbonate and 2 hours, static filtering, depressurize it is lower flow out toluene, obtain the MQ tree of the base containing Si-H
Rouge.
In another embodiment herein, by MQ resin, toluene is added there-necked flask, and after mixed dissolution, acid is added
Property carclazyte, after being uniformly mixed, back flow reaction 6 hours, and the water that condensation generates is separated and collected by steam-water separator
Get up.3700cm in Indicator Reaction solution is analyzed by FT-IR-1, 3500cm-1Absorption peak disappears, and confirmation reaction reaches terminal.
In above-mentioned reaction solution, viscosity (25 degree) 20mm is added2/ s, structural formula are MeSiO (MeHSiO)nSiM3Silicone oil and acidity
Carclazyte continues to be stirred to react 6-8 hours at 80-90 DEG C.Then in 0.2% part of ammonium hydrogen carbonate and 2 hours, cooling, static mistake
Filter depressurizes lower outflow toluene, obtains the MQ resin of the base containing Si-H.
In another embodiment herein, by MQ resin, toluene is added there-necked flask, and after mixed dissolution, acid is added
Property carclazyte, after being uniformly mixed, back flow reaction 6 hours, and the water that condensation generates is separated and collected by steam-water separator
Get up.3700cm in Indicator Reaction solution is analyzed by FT-IR-1, 3500cm-1Absorption peak disappears, and confirmation reaction reaches terminal.
In above-mentioned reaction solution, it is (MeHSiO) that structural formula, which is added,nM2The silicone oil and Emathlite of SiO continues to stir at 80-90 DEG C
Reaction 6-8 hours.Then in 0.2% part of ammonium hydrogen carbonate and 2 hours, cooling, static filtering, depressurize it is lower flow out toluene, obtain
The MQ resin of the base containing Si-H.
The application introduces Si-H base on Si atom, obtains the MQ resin of the base containing Si-H.Compared to common end group (CH)3SiO1/2After methylhydrogenpolysi,oxane is linked as crosslinking, it is prepared into sizing material, the glue prepared with the MQ resin of the base containing Si-H
Expect that viscosity is smaller, process operability is good, convenient for the small component in some gaps of encapsulating；Sizing material is easy to be mixed, the gas of generation
Bubble is easy abjection, and product properties is preferable.
Other features and advantage will illustrate in the following description, also, partly become from specification
It obtains it is clear that being understood and implementing the application.The purpose of the application and other advantages can by specification and
Specifically noted structure is achieved and obtained in claims.
Specific embodiment
It, hereinafter will be to embodiments herein for the purposes, technical schemes and advantages of the application are more clearly understood
It is described in detail.It should be noted that in the absence of conflict, the features in the embodiments and the embodiments of the present application can
With mutual any combination.
Reagent used in the embodiment of the present application unless otherwise stated, is otherwise commercially available.
Embodiment 1
By 140 grams of MQ resin, 60 grams of toluene are added there-necked flasks, after mixed dissolution, 1.6 grams of Emathlites are added, stir
After mixing, it then starts to warm up back flow reaction 6 hours, and the water that condensation generates is separated and gathered up by steam-water separator
Come, separates 1.3 grams of water.3700cm in Indicator Reaction solution is analyzed by FT-IR-1, 3500cm-1Absorption peak disappears, confirmation reaction
Reach terminal.
In above-mentioned reaction solution, 8 grams of hydrogeneous double seal heads are added, the trifluoromethayl sulfonic acid of 10ppm are added, at 70-80 DEG C
Continue to be stirred to react 8 hours.Then in 0.2% ammonium hydrogen carbonate and 2 hours, cooling, static filtering, depressurize it is lower flow out toluene,
White powder, 350 DEG C of softening point, GPC (gel permeation chromatography, Gel Permeation Chromatography) Mw=
4900g/mol, Si-H base 0.12% (mass parts).
Embodiment 2
By 140 grams of MQ resin, 60 grams of toluene are added there-necked flasks, after mixed dissolution, 1.2 grams of Emathlites are added, stir
After mixing, it then starts to warm up back flow reaction 6 hours, and the water that condensation generates is separated and gathered up by steam-water separator
Come, separates 0.9 gram of water.3700cm in Indicator Reaction solution is analyzed by FT-IR-1, 3500cm-1Absorption peak disappears, confirmation reaction
Reach terminal.Then viscosity (25 degree) 20mm is added thereto2/ s, structural formula are MeSiO (MeHSiO)nSiM310 grams of silicone oil
With the Emathlite of 10ppm, at 80-90 DEG C, the reaction was continued 6-8 hours, then in 0.2% ammonium hydrogen carbonate and 2 hours, cooling,
Filtering, distills out toluene, obtains white solid powder, 200 DEG C of softening point, GPC tests Mw=5000gmol, base containing Si-H 0.12%
The methyl MQ resin of (mass parts).
Embodiment 3
By 140 grams of MQ resin, 60 grams of toluene are added there-necked flasks, after mixed dissolution, 1.2 grams of Emathlites are added, stir
After mixing, it then starts to warm up back flow reaction 6 hours, and the water that condensation generates is separated and gathered up by steam-water separator
Come, separates 0.9 gram of water.3700cm in Indicator Reaction solution is analyzed by FT-IR-1, 3500cm-1Absorption peak disappears, confirmation reaction
Reach terminal.Then 12 grams are added thereto, structural formula is (MeHSiO)nM2The silicone oil of SiO and the Emathlite of 10ppm,
80-90 DEG C the reaction was continued 6-8 hours, and then in 0.2% ammonium hydrogen carbonate and 2 hours, cooling, filtering distills out toluene, obtains white
Color solid powder, 190 DEG C of softening point, GPC tests Mw=5100g/mol, the methyl MQ tree of base containing Si-H 0.07% (mass parts)
Rouge
The measuring method of Si-H content in embodiment 1-3
Reagent and its preparation method
1. the bromo- acetic acid solution of 0.2mol
The pure bromine of 1mL chemistry is pipetted with pipette to be dissolved in 100mL glacial acetic acid, is shaken up.
10% potassium iodide 2. (KI) solution
10 grams of KI are dissolved in 90 grams of water.
3. 0.1N sodium thiosulfate (Na2S2O3) standard solution
1)0.1N Na2S2O3The preparation of standard solution
Weigh the pure Na of analysis2S2O3·5H2O25g is dissolved in 1 liter of distilled water for newly boiling and cooling down, Na is added2CO3About 0.2
It gram stores in brown bottle, opens in dark place, its concentration is demarcated after 24 hours.
2) calibration of sodium thiosulfate titer
Weigh the primary standard reagent potassium bichromate (K dried 2 hours and cooled down at 120 DEG C2Cr2O7)0.1200-0.1400g
25mL water is added in (being accurate to 0.0001g)；2g potassium iodide and 5mL6N sulfuric acid are added, is placed in dark place 10 minutes, takes out and adds water
70mL, with 0.1N Na2S2O3Titer titration when nearly terminal, adds 3mL0.5% starch indicator, continues titration solution by purple
Becoming sapphirine is terminal.
N=G/0.04903V
In formula: N Na2S2O3Concentration of standard solution；G is K2Cr2O7It weighs (g)；V is consumption Na2S2O3Titer volume
(mL)。
4. 0.5% starch solution
0.5g grams of soluble starch is taken, adds a small amount of water-wet to moisten, adds 100mL, the distilled water boiled stirs evenly.
Measuring method:
1. accurately weighing sample size 1.2890 (being accurate to 0.0001g), it is placed in 250mL iodine flask, adds carbon tetrachloride
(CCl4) 20mL, then dissolved samples are added bromo- acetic acid solution 10mL (accurately being added with pipette), then plus 0.5mL water shake up,
Dark place is placed in react 15 minutes.
2. 10%KI solution 15mL after the reaction was completed, which is added, uses 0.1N with deionized water or distilled water flushing bottleneck
Na2S2O3Titer titration, starch is indicator, and being dropped to colourless by blue is terminal, while making blank test.
3. calculation method:
H%=N (V0-V1) × 0.5 × 1.008 × 100/1000G%
In formula: N Na2S2O3The equivalent concentration of titer；V0Na is consumed for blank2S2O3Titer volume (mL)；V1For examination
Sample consumes Na2S2O3Titer volume (mL)；G is sample weight (g).
Application Example 1
100 parts by weight of dimethyl silicone polymer of both ends vinyl is linked, average degree of polymerization about 20, embodiment 1 are made
Standby 150 parts by weight of Si-H content MQ resin, butynol and ethynylcyclohexanol mixture 500ppm, mixing are made into sizing material A.
Application Example 2
100 parts by weight of dimethyl silicone polymer of both ends vinyl is linked, average degree of polymerization about 20, the platinum of 25ppm
The platinum chelate 0.1% of gold content is uniformly mixed and is made into sizing material B
Comparative example 1
100 parts by weight of dimethyl silicone polymer of both ends vinyl is linked, average degree of polymerization about 20 are added hydrogeneous
0.09% ordinary hydrogen silicon entreats 150 parts of alkane (containing hydrogen silicone oil), and butynol and ethynylcyclohexanol mixture 500ppm, mixing are made into ratio
Compared with material A.
Comparative example 2
100 parts by weight of dimethyl silicone polymer of both ends vinyl is linked, average degree of polymerization about 20, the platinum of 25ppm
The platinum chelate 0.1% of gold content is uniformly mixed to be made into and compares sizing material B
Sizing material viscosity is prepared using plum Teller rotational viscometer testing example and comparative example, as a result as shown in table 1.
The viscosity for the sizing material prepared in 1 embodiment of table and comparative example
| Sizing material | Viscosity/mpa.s (25 DEG C) |
| Application Example 1 | 15800 |
| Application Example 2 | 37000 |
| Comparative example 1 | 98000 |
| Comparative example 2 | 390000 |
From table 1 it follows that the viscosity for the sizing material that Application Example 1-2 is prepared is than being prepared with common containing hydrogen silicone oil
Sizing material is small, and process operability is good, convenient for the small component in some gaps of encapsulating；A, two kinds of components of B are easy to be mixed, generation
Bubble is easy abjection, and product properties is preferable.
Although embodiment disclosed by the application is as above, the content only for ease of understanding the application and use
Embodiment is not limited to the application.Technical staff in any the application fields, is taken off not departing from the application
Under the premise of the spirit and scope of dew, any modification and variation, but the application can be carried out in the form and details of implementation
Scope of patent protection, still should be subject to the scope of the claims as defined in the appended claims.
Claims (11)
1. a kind of MQ resin of base containing Si-H, the mass fraction of the Si-H of the MQ resin of the base containing Si-H is in 0.07%-1.2%
In the range of, MwIn the range of 4000g/mol-6000g/mol, softening point is in the range of 100 DEG C -400 DEG C.
2. the preparation method of the MQ resin of the base described in claim 1 containing Si-H, the preparation method include:
(1) solution of MQ resin and Emathlite are mixed, are then refluxed for reacting by Si-OH base Seal treatment, and will reaction
The moisture of generation separates out；
(2) preparation of the MQ resin of the base containing Si-H separates in the solution after being discharged in step (1) and radical siloxane containing Si-H is added
And catalyst, the reaction was continued, then neutralizes, and it is cooling, it stands, filtering steams solvent under decompression, obtain the MQ of the base containing Si-H
Resin.
3. preparation method according to claim 2, wherein the solution of the MQ resin is that the toluene of the MQ resin is molten
Any one of liquid, xylene solution, hexane solution, n-heptane solution or more.
4. preparation method according to claim 2, wherein the radical siloxane containing Si-H is hydrogeneous double seal head or structural formula
For MeSiO (MeHSiO)nSiM3Or (MeHSiO)nM2The silicone oil of SiO,
The catalyst is trifluoromethayl sulfonic acid or Emathlite.
5. preparation method according to claim 2, wherein the solid content of the solution of the MQ resin is 60%-70%,
The mass ratio of the MQ resin and Emathlite are as follows: 80-120: 1,
The mass ratio of the MQ resin and the radical siloxane containing Si-H are as follows: 10-20: 1.
6. preparation method according to claim 2, wherein in step (1), back flow reaction continues -6 hours 5 hours.
7. preparation method according to claim 2, wherein molten by infrared spectrum analysis Indicator Reaction in step (1)
3700cm in liquid-1, 3500cm-1Absorption peak disappears, and confirmation reaction reaches terminal.
8. preparation method according to claim 2, wherein in step (2), at 70 DEG C -90 DEG C, the reaction was continued.
9. preparation method according to claim 2, wherein in step (2), the reaction was continued continues 6-8 hours.
10. preparation method according to claim 2, wherein in step (2), the bicarbonate for being 0.2% with mass concentration
In ammonium and -4 hours 2 hours.
11. a kind of sizing material, the MQ resin comprising the base according to claim 1 containing Si-H.
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Application publication date: 20190806 |