CN107974087A - A kind of high-temperature resistant organic silicon resin - Google Patents
A kind of high-temperature resistant organic silicon resin Download PDFInfo
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- CN107974087A CN107974087A CN201711398674.1A CN201711398674A CN107974087A CN 107974087 A CN107974087 A CN 107974087A CN 201711398674 A CN201711398674 A CN 201711398674A CN 107974087 A CN107974087 A CN 107974087A
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- temperature resistant
- organic silicon
- resistant organic
- silicon resin
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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
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2312/00—Crosslinking
Abstract
The invention discloses a kind of high-temperature resistant organic silicon resin, is related to chemical technology field, and its preparation method comprises the following steps：（1）It is prepared by modifying agent；（2）It is prepared by solidfied material；（3）It is prepared by finished product；Organic siliconresin prepared by the present invention has good resistance to elevated temperatures, and after testing, organic siliconresin bending strength prepared by the present invention reaches 85.3MPa, and impact strength reaches 36.8kJ/m2.
Description
Technical field
The invention belongs to chemical technology field, and in particular to a kind of high-temperature resistant organic silicon resin.
Background technology
Organic siliconresin（HS）Inorganic material and the performance of organic material are had concurrently, there is electric insulation, resistance to ozone, resistance to
The excellent specific property such as radiation, fire retardant, hydrophobic, corrosion-resistant, nonpoisonous and tasteless and physiological inertia, therefore prepare mould using organic siliconresin
Plastic composite has the characteristics that the physical dimension stability of higher, high humidity complex environment, chemicals-resistant corrosion.It is but existing
Some organic siliconresin resistances to elevated temperatures are poor, can not meet the needs of market.
The content of the invention
The purpose of the present invention is for it is existing the problem of, there is provided a kind of high-temperature resistant organic silicon resin.
The present invention is achieved by the following technical solutions：
A kind of high-temperature resistant organic silicon resin, its preparation method comprise the following steps：
（1）It is prepared by modifying agent：Positive silicon ester resin monomer, 10-12g deionized waters and the 6- of 120-150g is added into reaction kettle
8g absolute ethyl alcohols, stir 10-15min with 1500r/min rotating speeds, then add positive silicon ester resin monomer mass 0.05-0.08%
Ammonium persulfate, be heated to 112 DEG C, continue stir 30-40min, then add positive silicon ester resin monomer mass 0.12- again
0.15% coupling agent, adjusts the temperature to 80 DEG C, when insulation 2 is small, the triethylamine of 0.5g is then instilled again, with 120r/min rotating speeds
2min, ultrasonication 3min are stirred, then cooled to room temperature, up to required modifying agent；
（2）It is prepared by solidfied material：Modifying agent and organic siliconresin are pressed 1:8-12 mass ratios uniformly mix, and are turned with 3500r/min
When speed stirring 2 is small, when then isothermal holding 1 is small at 80 DEG C, solidfied material is obtained；
（3）It is prepared by finished product：By solidfied material acetone solution, 40min is stirred with 2500r/min rotating speeds, then add solidfied material quality
2.5% activated bentonite, after stirring evenly, is added in batch mixing kneader and mediates 8-9min, and acetone is removed after discharging, prepares
Finished product.
Further, the step（1）Middle coupling agent is organo silane coupling agent.
Further, the step（1）Middle ultrasonic power is 1000W, frequency 50kHz.
Further, the step（3）Middle activated bentonite preparation method is：Bentonite is calcined at 800 DEG C
10min, then cooled to room temperature, then the bentonite after calcining is added to the Potassium Suceinate that mass fraction is 3.5% and is soaked
40min, is then filtered, and drying to constant weight, to obtain the final product
Further, the Potassium Suceinate solution soaking temperature is no more than 50 DEG C.
Further, the activated bentonite granularity is 1250 mesh.
The present invention has the following advantages compared with prior art：Organic siliconresin prepared by the present invention has good high temperature resistant
Performance, after testing, organic siliconresin bending strength prepared by the present invention reach 85.3MPa, and impact strength reaches 36.8kJ/m2；
The present invention is modified organic siliconresin processing by using the modifying agent of preparation so that modified organic siliconresin has
The structure of high degree of symmetry, containing rigid radicals such as substantial amounts of phenyl ring, its C ≡ C key contained can be handed in the curing process
Connection reaction.The addition of activated bentonite increases the crosslink density of system at the same time, improves toughness, mechanical strength also gradually increases
By force, therefore by the modification to organic siliconresin, system rigidity and crosslink density all strengthen, the mechanical property of prepared product
Also strengthen therewith, especially resistance to elevated temperatures, which is greatly enhanced, is, greatly expands its application range.
Embodiment
Embodiment 1
A kind of high-temperature resistant organic silicon resin, its preparation method comprise the following steps：
（1）It is prepared by modifying agent：Positive silicon ester resin monomer, 10g deionized waters and the anhydrous second of 6g of 120g is added into reaction kettle
Alcohol, 10min is stirred with 1500r/min rotating speeds, then adds the ammonium persulfate of positive silicon ester resin monomer mass 0.05%, heating
To 112 DEG C, continue to stir 30min, then add the coupling agent of positive silicon ester resin monomer mass 0.12% again, adjust the temperature to
80 DEG C, when insulation 2 is small, the triethylamine of 0.5g is then instilled again, and 2min, ultrasonication 3min are stirred with 120r/min rotating speeds,
Then cooled to room temperature, up to required modifying agent；
（2）It is prepared by solidfied material：Modifying agent and organic siliconresin are pressed 1:8 mass ratios uniformly mix, and are stirred with 3500r/min rotating speeds
Mix 2 it is small when, when then isothermal holding 1 is small at 80 DEG C, obtain solidfied material；
（3）It is prepared by finished product：By solidfied material acetone solution, 40min is stirred with 2500r/min rotating speeds, then add solidfied material quality
2.5% activated bentonite, after stirring evenly, is added in batch mixing kneader and mediates 8min, remove acetone after discharging, be prepared into
Product.
Further, the step（1）Middle coupling agent is organo silane coupling agent.
Further, the step（1）Middle ultrasonic power is 1000W, frequency 50kHz.
Further, the step（3）Middle activated bentonite preparation method is：Bentonite is calcined at 800 DEG C
10min, then cooled to room temperature, then the bentonite after calcining is added to the Potassium Suceinate that mass fraction is 3.5% and is soaked
40min, is then filtered, and drying to constant weight, to obtain the final product
Further, the Potassium Suceinate solution soaking temperature is no more than 50 DEG C.
Further, the activated bentonite granularity is 1250 mesh.
Embodiment 2
A kind of high-temperature resistant organic silicon resin, its preparation method comprise the following steps：
（1）It is prepared by modifying agent：Positive silicon ester resin monomer, 12g deionized waters and the anhydrous second of 8g of 150g is added into reaction kettle
Alcohol, 15min is stirred with 1500r/min rotating speeds, then adds the ammonium persulfate of positive silicon ester resin monomer mass 0.08%, heating
To 112 DEG C, continue to stir 40min, then add the coupling agent of positive silicon ester resin monomer mass 0.15% again, adjust the temperature to
80 DEG C, when insulation 2 is small, the triethylamine of 0.5g is then instilled again, and 2min, ultrasonication 3min are stirred with 120r/min rotating speeds,
Then cooled to room temperature, up to required modifying agent；
（2）It is prepared by solidfied material：Modifying agent and organic siliconresin are pressed 1:12 mass ratios uniformly mix, with 3500r/min rotating speeds
Stir 2 it is small when, when then isothermal holding 1 is small at 80 DEG C, obtain solidfied material；
（3）It is prepared by finished product：By solidfied material acetone solution, 40min is stirred with 2500r/min rotating speeds, then add solidfied material quality
2.5% activated bentonite, after stirring evenly, is added in batch mixing kneader and mediates 9min, remove acetone after discharging, be prepared into
Product.
Further, the step（1）Middle coupling agent is organo silane coupling agent.
Further, the step（1）Middle ultrasonic power is 1000W, frequency 50kHz.
Further, the step（3）Middle activated bentonite preparation method is：Bentonite is calcined at 800 DEG C
10min, then cooled to room temperature, then the bentonite after calcining is added to the Potassium Suceinate that mass fraction is 3.5% and is soaked
40min, is then filtered, and drying to constant weight, to obtain the final product
Further, the Potassium Suceinate solution soaking temperature is no more than 50 DEG C.
Further, the activated bentonite granularity is 1250 mesh.
Embodiment 3
A kind of high-temperature resistant organic silicon resin, its preparation method comprise the following steps：
（1）It is prepared by modifying agent：Positive silicon ester resin monomer, 11g deionized waters and the anhydrous second of 7g of 130g is added into reaction kettle
Alcohol, stirs 12min with 1500r/min rotating speeds, then adds the ammonium persulfate of positive silicon ester resin monomer mass 0.05-0.08%,
112 DEG C are heated to, continues to stir 35min, then adds the coupling agent of positive silicon ester resin monomer mass 0.14% again, adjust temperature
Degree is to 80 DEG C, when insulation 2 is small, then instills the triethylamine of 0.5g again, and 2min, ultrasonication are stirred with 120r/min rotating speeds
3min, then cooled to room temperature, up to required modifying agent；
（2）It is prepared by solidfied material：Modifying agent and organic siliconresin are pressed 1:10 mass ratios uniformly mix, with 3500r/min rotating speeds
Stir 2 it is small when, when then isothermal holding 1 is small at 80 DEG C, obtain solidfied material；
（3）It is prepared by finished product：By solidfied material acetone solution, 40min is stirred with 2500r/min rotating speeds, then add solidfied material quality
2.5% activated bentonite, after stirring evenly, is added in batch mixing kneader and mediates 8.5min, and acetone is removed after discharging, prepares
Finished product.
Further, the step（1）Middle coupling agent is organo silane coupling agent.
Further, the step（1）Middle ultrasonic power is 1000W, frequency 50kHz.
Further, the step（3）Middle activated bentonite preparation method is：Bentonite is calcined at 800 DEG C
10min, then cooled to room temperature, then the bentonite after calcining is added to the Potassium Suceinate that mass fraction is 3.5% and is soaked
40min, is then filtered, and drying to constant weight, to obtain the final product
Further, the Potassium Suceinate solution soaking temperature is no more than 50 DEG C.
Further, the activated bentonite granularity is 1250 mesh.
Comparative example 1：Differed only in embodiment 1 in step（1）In do not add coupling agent.
Comparative example 2：Step is differed only in embodiment 1（3）In do not add activated bentonite.
Comparative example 3：Step is differed only in embodiment 1（3）Middle activated bentonite replaces with common bentonite.
Experiment：
Performance detection is carried out to the organic siliconresin prepared in embodiment and comparative example；
Table 1
| Bending strength conservation rate % at 200 DEG C | |
| Embodiment 1 | 83.6 |
| Embodiment 2 | 82.9 |
| Embodiment 3 | 83.5 |
| Comparative example 1 | 80.1 |
| Comparative example 2 | 72.8 |
| Comparative example 3 | 76.5 |
As can be seen from Table 1, the silicone resin material resistance to elevated temperatures that prepared by the present invention is superior.
Claims (6)
1. a kind of high-temperature resistant organic silicon resin, it is characterised in that its preparation method comprises the following steps：
（1）It is prepared by modifying agent：Positive silicon ester resin monomer, 10-12g deionized waters and the 6- of 120-150g is added into reaction kettle
8g absolute ethyl alcohols, stir 10-15min with 1500r/min rotating speeds, then add positive silicon ester resin monomer mass 0.05-0.08%
Ammonium persulfate, be heated to 112 DEG C, continue stir 30-40min, then add positive silicon ester resin monomer mass 0.12- again
0.15% coupling agent, adjusts the temperature to 80 DEG C, when insulation 2 is small, the triethylamine of 0.5g is then instilled again, with 120r/min rotating speeds
2min, ultrasonication 3min are stirred, then cooled to room temperature, up to required modifying agent；
（2）It is prepared by solidfied material：Modifying agent and organic siliconresin are pressed 1:8-12 mass ratios uniformly mix, and are turned with 3500r/min
When speed stirring 2 is small, when then isothermal holding 1 is small at 80 DEG C, solidfied material is obtained；
（3）It is prepared by finished product：By solidfied material acetone solution, 40min is stirred with 2500r/min rotating speeds, then add solidfied material quality
2.5% activated bentonite, after stirring evenly, is added in batch mixing kneader and mediates 8-9min, and acetone is removed after discharging, prepares
Finished product.
A kind of 2. high-temperature resistant organic silicon resin as claimed in claim 1, it is characterised in that the step（1）Middle coupling agent is
Organo silane coupling agent.
A kind of 3. high-temperature resistant organic silicon resin as claimed in claim 1, it is characterised in that the step（1）Middle ultrasonic wave work(
Rate is 1000W, frequency 50kHz.
A kind of 4. high-temperature resistant organic silicon resin as claimed in claim 1, it is characterised in that the step（3）Middle activation swelling
Native preparation method is：Bentonite is calcined into 10min at 800 DEG C, then cooled to room temperature, then by the bentonite after calcining
Be added to the Potassium Suceinate that mass fraction is 3.5% and soak 40min, then filtered, drying to constant weight, to obtain the final product.
A kind of 5. high-temperature resistant organic silicon resin as claimed in claim 4, it is characterised in that the Potassium Suceinate solution immersion temperature
Degree is no more than 50 DEG C.
6. a kind of high-temperature resistant organic silicon resin as claimed in claim 4, it is characterised in that the activated bentonite granularity is
1250 mesh.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711398674.1A CN107974087A (en) | 2017-12-22 | 2017-12-22 | A kind of high-temperature resistant organic silicon resin |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711398674.1A CN107974087A (en) | 2017-12-22 | 2017-12-22 | A kind of high-temperature resistant organic silicon resin |
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| Publication Number | Publication Date |
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| CN107974087A true CN107974087A (en) | 2018-05-01 |
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| CN201711398674.1A Withdrawn CN107974087A (en) | 2017-12-22 | 2017-12-22 | A kind of high-temperature resistant organic silicon resin |
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Citations (9)
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|---|---|---|---|---|
| CN101012363A (en) * | 2007-01-25 | 2007-08-08 | 四川大学 | Filling rubber for preparing high-strength transparence room-temperature curing silicon rubber |
| CN101177595A (en) * | 2007-12-13 | 2008-05-14 | 同济大学 | Nano MQ silicon resin reinforced moisture curing organic pressure-sensitive gel and preparation method thereof |
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| CN103265702A (en) * | 2013-05-28 | 2013-08-28 | 哈尔滨工业大学 | Preparation method of ultraviolet-resistant and high-temperature-resistant methyl silicone resin |
| CN103342816A (en) * | 2013-06-19 | 2013-10-09 | 广州慧谷化学有限公司 | Organic silicone resin, curable organopolysiloxane composition and application |
| CN104478476A (en) * | 2014-11-20 | 2015-04-01 | 济南大学 | Modifier for cement concrete and method for improving performance of cement concrete |
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-
2017
- 2017-12-22 CN CN201711398674.1A patent/CN107974087A/en not_active Withdrawn
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|---|---|---|---|---|
| CN101012363A (en) * | 2007-01-25 | 2007-08-08 | 四川大学 | Filling rubber for preparing high-strength transparence room-temperature curing silicon rubber |
| CN101177595A (en) * | 2007-12-13 | 2008-05-14 | 同济大学 | Nano MQ silicon resin reinforced moisture curing organic pressure-sensitive gel and preparation method thereof |
| CN102675643A (en) * | 2012-05-23 | 2012-09-19 | 沈阳化工大学 | Synthesizing method for organic silicon micro-balls with performances of super hydrophobicity and high temperature resistant |
| CN103265702A (en) * | 2013-05-28 | 2013-08-28 | 哈尔滨工业大学 | Preparation method of ultraviolet-resistant and high-temperature-resistant methyl silicone resin |
| CN103342816A (en) * | 2013-06-19 | 2013-10-09 | 广州慧谷化学有限公司 | Organic silicone resin, curable organopolysiloxane composition and application |
| CN104478476A (en) * | 2014-11-20 | 2015-04-01 | 济南大学 | Modifier for cement concrete and method for improving performance of cement concrete |
| CN104532226A (en) * | 2014-12-18 | 2015-04-22 | 青岛乐化科技有限公司 | Environment-friendly organic-inorganic hybrid aluminum alloy primer and preparation method thereof |
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Application publication date: 20180501 |