CN109486200A - Organosilicon resin composition and preparation method thereof containing tungsten oxide - Google Patents
Organosilicon resin composition and preparation method thereof containing tungsten oxide Download PDFInfo
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- CN109486200A CN109486200A CN201811618333.5A CN201811618333A CN109486200A CN 109486200 A CN109486200 A CN 109486200A CN 201811618333 A CN201811618333 A CN 201811618333A CN 109486200 A CN109486200 A CN 109486200A
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- tungsten oxide
- resin composition
- oxide
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- organosilicon resin
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- 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
- C08K3/22—Oxides; Hydroxides of metals
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- 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
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2244—Oxides; Hydroxides of metals of zirconium
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- 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
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2258—Oxides; Hydroxides of metals of tungsten
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The present invention relates to a kind of organosilicon resin composition and preparation method thereof containing tungsten oxide, belongs to medical ultrasound technical field.It includes 10-40 parts and organic siliconresin 60-90 parts of tungsten oxide, tungsten oxide is modified using silane coupling agent first, then it is sufficiently stirred again with organic siliconresin, the organosilicon resin composition containing tungsten oxide is obtained after deaeration, the method of the present invention prepares that the resulting organosilicon resin composition density containing tungsten oxide is suitable, average particle size particle size is suitable, viscosity is suitable, and decaying is few, easy deaeration, skin feel is good, can obtain good application in medical ultrasound field using the lens in the energy converter of the composition preparation.
Description
Technical field
The present invention relates to a kind of organosilicon resin composition and preparation method thereof containing tungsten oxide, and in particular to Yi Zhongyong
In the organosilicon resin composition and preparation method thereof containing tungsten oxide for preparing the lens in energy converter, belong to medical ultrasound skill
Art field.
Background technique
The acoustic impedance of the material of medical supersonic lens currently on the market, general organic siliconresin is lower, be 1-1.2 ×
106Pas/m, and the acoustic impedance between tissue is about 1.5 × 106Pas/m, in order to match between ultrasonic probe and human body
Impedance reduces energy loss when sound wave is passed to human body, inorganic filler is added in organic siliconresin, to improve acoustic impedance.
The inorganic filler type that can be added at present has very much, such as aluminium oxide, white carbon black, iron oxide, zinc oxide, density
It is distributed in 2~8g/cm3In range, filler particles size is all distributed from 5nm~1 μm.In the prior art substantially by following two
1. the opposite volume being added of low density filler is just relatively on the high side for problem, and high filler content can make silicone resin degradation, such as high viscous
Degree, it is highly attenuating, situations such as difficult deaeration；2. additive particles diameter reaches the filler of Nano grade, since quality is certain, filler
Particle size is smaller, and volume is more, can equally make silica gel degradation.And reach micron level even larger sized particle
Size will appear rough surface after being added into organic siliconresin, occur the symptoms such as discomfort after skin contact.
Need to find now it is a kind of can find density is suitable, the suitable certain mass ratio of average particle size particle size it is inorganic
Filler lacks to reach suitable viscosity and decay, and easy deaeration, skin feel is good at this time.
Summary of the invention
The object of the present invention is to provide a kind of organosilicon resin composition containing tungsten oxide, density is suitable, average
Particle size is suitable.
A further object of the invention is to provide the preparation method of the organosilicon resin composition containing tungsten oxide,
Preparation method is simple, and preparation resulting product skin feel is good.
Another of the invention is further objective is that provide a kind of system of organosilicon resin composition containing tungsten oxide
Product.
Technical solution of the present invention, the organosilicon resin composition containing tungsten oxide, comprising: 10-40 parts of tungsten oxide and
60-90 parts of organic siliconresin.
It further, by weight, further include 10-50 parts of metal composites.
Further, the tungsten oxide is by being modified.
Further, the tungsten oxide is nanoscale, and partial size is 5nm~1 μm
Further, the tungsten oxide is specially tungstic acid.
Further, the metal composites are specially one of oxide of iron, zinc, silicon, magnesium, titanium or zirconium or several
Kind.
Further, the metal composites are specially ferroso-ferric oxide, di-iron trioxide, zinc oxide, magnesia, dioxy
Change one or more of titanium or zirconium oxide.
Further, tungsten oxide is modified using silane coupling agent first, is then carried out again with organic siliconresin
It is sufficiently stirred, the organosilicon resin composition containing tungsten oxide is obtained after deaeration；
Preferably, the specific steps of which are as follows:
(1) configuration of modifying agent: taking 0.5-33 parts of silane coupling agent, is dissolved in 67-99.5 parts of solvents, obtains mixing and melts
It closes；
(2) modified: to take 10-40 parts of tungsten oxide, add the mixed solution of step (1) configuration wherein, be heated to 45-60
DEG C, it is stirred continuously in heating process, is sufficiently mixed 1-2h；It filters, dry 30min, cooling at 80-100 DEG C, was modified
Oxide-metal combinations filler；
(3) it mixes: taking oxide-metal combinations filler obtained by step (2) that blender is added with 60-90 parts of organic siliconresins
In with 2100-2300r/min revolving speed stir 2-4min, then the deaeration 4-6min within 130pa, obtains having containing tungsten oxide
Machine silicon resin composition；
Preferably, the solvent is isopropanol.
It further, further include metal composites；First using silane coupling agent to tungsten oxide and metal composites into
Row is modified；
Preferably, the specific steps are as follows:
(1) configuration of modifying agent: taking 0.5-33 parts of silane coupling agent, is dissolved in 67-99.5 parts of solvents, obtains mixing and melts
It closes；
(2) modified: to take 10-40 parts and metal composites 10-30 parts mixing of tungsten oxide, add step (1) wherein and match
The mixed solution set is heated to 45-60 DEG C, is stirred continuously in heating process, is sufficiently mixed 1-2h；It filters, is done at 80-100 DEG C
Dry 30min, cooling, the oxide-metal combinations filler being modified；
(3) it mixes: taking oxide-metal combinations filler obtained by step (2) that blender is added with 60-90 parts of organic siliconresins
In with 2100-2300r/min revolving speed stir 2-4min, then the deaeration 4-6min within 130pa, obtains having containing tungsten oxide
Machine silicon resin composition；
Preferably, the solvent is isopropanol.
The application of organosilicon resin composition containing tungsten oxide, including using the silicone resin composition containing tungsten oxide
Object prepares the lens in energy converter.
Beneficial effects of the present invention: the method for the present invention prepares the resulting organosilicon resin composition density containing tungsten oxide
Properly, average particle size particle size is suitable, viscosity is suitable, and it is few to decay, and easy deaeration, skin feel is good, using the composition preparation
Lens in energy converter can obtain good application in medical ultrasound field.
Specific embodiment
Embodiment 1
A kind of it can find that density is suitable, the inorganic material of the suitable certain mass ratio of average particle size particle size comes to find
Reach suitable viscosity and decaying is few, easy deaeration, skin feel is good at this time.According to the various characteristics of metal oxide, pick out
Nanoscale product nontoxic and with operability, as shown in table 1 below.
Table 1
As can be seen from Table 1, metal oxide Density Distribution is in 1.85~7.16g/cm3In range, using single metal
Oxide is screened, with the composition finished product density 1.4-1.5g/cm in organic siliconresin containing metal oxide3For mesh
Mark, 30 parts of metal oxides are added in 70 parts of organic siliconresins, and (buying is certainly by organic siliconresin model RTV630A
Momentive)。
Take said mixture by planetary mixer high-speed stirred (2200r/min) 3 minutes, and under vacuum (130pa with
It is interior) deaeration after five minutes, production sample and test performance, satisfactory only WO3One kind, other fillers are due to viscosity is too big
Failure.
Table 2
| Filler model | Chemical formula | Composition density g/cm3 | Acoustic velocity m/s | Impedance × 106Pas/m | Decay dB/mm under 3.5MHz |
| Tungstic acid | WO3 | 1.44 | 994 | 1.43 | 4.17 |
As can be seen from Table 2, after the nano-scale particle tungstic acid of single variety is added into organic siliconresin, contain tungsten oxide
Organosilicon resin composition impedance it is qualified, viscosity becomes larger, can flow reluctantly, mass production processes be difficult to control decay it is higher,
It needs further to be modified filler.
Embodiment 2
Surface modification treatment is carried out to nano particle tungstic acid using silane coupling agent, is KH550 with silane coupling agent
For, it is that 0.5%~25% Silane coupling agent KH550 is configured to isopropyl alcohol mixture by mass ratio before modification, it is necessary
When can be properly added some acetic acid to adjust the pH value of solution.
Such as by the isopropyl alcohol mixture of 100g, wherein being 5g containing Silane coupling agent KH550 quality, by filler 20g
Tungstic acid is put into above-mentioned isopropyl alcohol mixture, is heated to 50 DEG C, is stirred continuously in heating process, and 1h is continued, using
Filter, the dry 30min at 80-100 DEG C after taking out cooling, will be modified tungstic acid and be added in 80g organic siliconresin, passed through
Planetary mixer high-speed stirred (2200r/min) 3 minutes, and deaeration after five minutes, makes oxygen-containing (within 130pa) under vacuum
Change the organosilicon resin composition sample and test performance of tungsten, as shown in table 3 below.
Wherein, tungstic acid and organic siliconresin intelligence connection coin are table 3
| Filler model | Chemical formula | Composition density g/cm3 | Acoustic velocity m/s | Impedance × 106Pas/m | Decay dB/mm under 3.5MHz |
| Tungstic acid | WO3 | 1.43 | 950 | 1.358 | 3.27 |
After carrying out tungstic acid surface modification treatment by silane coupling agent it can be seen from the data of table 3, organosilicon tree
The oil/fat composition velocity of sound reduces, and impedance decline, but the reduction that decays simultaneously, viscosity decline much compared with table 2, mobility with higher but
It is to decay at this time still higher, needs to adjust the composition and ratio of tungsten oxide, needs further progress improvement that can just meet technique
Demand.
Embodiment 3
In the present embodiment, the oxide-metal combinations filler comprising organic siliconresin and modified processing, such as oxygen are provided
Change tungsten, zirconium oxide composite filling, wherein the average particle size particle size of tungsten oxide is 5nm~1 μm, accounts for entire oxide-metal combinations and fills out
The mass fraction of material about 10%-70%.
Inorganic filler is surface-treated using silane coupling agent, by taking silane coupling agent is KH550 as an example, modification
Before, it is that 0.5%~25% Silane coupling agent KH550 is configured to isopropyl alcohol mixture by mass ratio, it may be necessary to suitably add
Add some acetic acid to adjust the pH value of solution.
Such as by the isopropyl alcohol mixture of 100g, wherein being 5g containing Silane coupling agent KH550 quality.By 40g metal
Combination of oxides filler is put into above-mentioned isopropyl alcohol mixture, is heated to 50 DEG C, is stirred continuously in heating process, and 1h is continued,
Using filter, after taking out cooling, 90g is added in the oxide-metal combinations filler being modified by the dry 30min at 80-100 DEG C
In organic siliconresin, by planetary mixer high-speed stirred (2200r/min) 3 minutes, and deaeration (within 130pa) under vacuum
After five minutes, the organosilicon resin composition sample and test performance of containing metal oxide composite filling are made, as shown in table 4 below:
Table 4
After being surface-treated it can be seen from the data of table 4 by silane coupling agent, the velocity of sound is reduced, impedance decline, but
Decaying is greatly lowered simultaneously, and viscosity reduces, and viscosity increase is unobvious, has operability, meets probe lens process requirement.
Claims (9)
1. the organosilicon resin composition containing tungsten oxide, by weight, comprising: 10-40 parts of tungsten oxide and organosilicon tree
60-90 parts of rouge.
2. as described in claim 1 containing the organosilicon resin composition of tungsten oxide, it is characterized in that: the tungsten oxide is by changing
Property.
3. as described in claim 1 containing the organosilicon resin composition of tungsten oxide, it is characterized in that: the tungsten oxide is nanometer
Grade, partial size are 5nm ~ 1 μm
As described in claim 1 containing the organosilicon resin composition of tungsten oxide, it is characterized in that: the tungsten oxide is specially three
Tungsten oxide.
4. further including metal composites by weight containing the organosilicon resin composition of tungsten oxide described in claim 1
10-50 parts.
5. as claimed in claim 4 containing the organosilicon resin composition of tungsten oxide, it is characterized in that: the metal composites are specific
For one or more of the oxide of iron, zinc, silicon, magnesium, titanium or zirconium.
6. as claimed in claim 5 containing the organosilicon resin composition of tungsten oxide, it is characterized in that: the metal composites are specific
For one or more of ferroso-ferric oxide, di-iron trioxide, zinc oxide, magnesia, titanium dioxide or zirconium oxide.
7. the preparation method of the organosilicon resin composition containing tungsten oxide includes the following steps: first using silane coupling agent
Tungsten oxide is modified, is then sufficiently stirred again with organic siliconresin, is obtained after deaeration containing the organic of tungsten oxide
Silicon resin composition；
Preferably, the specific steps of which are as follows:
(1) configuration of modifying agent: taking 0.5-33 parts of silane coupling agent, is dissolved in 67-99.5 parts of solvents, obtains mixing fusion；
(2) modified: 10-40 parts of tungsten oxide are taken, the mixed solution of step (1) configuration is added wherein, is heated to 45-60 DEG C,
It is stirred continuously in heating process, is sufficiently mixed 1-2h；It filters, dry 30min, cooling at 80-100 DEG C, the gold being modified
Belong to combination of oxides filler；
(3) mix: take oxide-metal combinations filler obtained by step (2) in 60-90 part organic siliconresins addition blenders with
2100-2300r/min revolving speed stirs 2-4min, and then the deaeration 4-6min within 130pa, obtains the organosilicon containing tungsten oxide
Resin combination；
Preferably, the solvent is isopropanol.
8. the preparation method of the organosilicon resin composition containing tungsten oxide as claimed in claim 8, it is characterized in that: further including gold
Belong to composition；Tungsten oxide and metal composites are modified using silane coupling agent first；
Preferably, the specific steps are as follows:
(1) configuration of modifying agent: taking 0.5-33 parts of silane coupling agent, is dissolved in 67-99.5 parts of solvents, obtains mixing fusion；
(2) modified: to take 10-40 parts and metal composites 10-30 parts mixing of tungsten oxide, add step (1) configuration wherein
Mixed solution is heated to 45-60 DEG C, is stirred continuously in heating process, is sufficiently mixed 1-2h；It filters, it is dry at 80-100 DEG C
30min, cooling, the oxide-metal combinations filler being modified；
(3) mix: take oxide-metal combinations filler obtained by step (2) in 60-90 part organic siliconresins addition blenders with
2100-2300r/min revolving speed stirs 2-4min, and then the deaeration 4-6min within 130pa, obtains the organosilicon containing tungsten oxide
Resin combination；
Preferably, the solvent is isopropanol.
9. the application of the organosilicon resin composition containing tungsten oxide, including using the organosilicon resin composition containing tungsten oxide
Prepare the lens in energy converter.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112111154A (en) * | 2020-09-27 | 2020-12-22 | 北京瑞祥宏远科技有限公司 | Ultrasonic coupling agent for nondestructive testing and preparation method thereof |
| JPWO2021131430A1 (en) * | 2019-12-24 | 2021-07-01 | ||
| CN116554686A (en) * | 2023-04-27 | 2023-08-08 | 深圳鲲为科技有限公司 | Ultrasonic probe acoustic lens material, ultrasonic probe acoustic lens and preparation method of ultrasonic probe acoustic lens material |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JPWO2021131430A1 (en) * | 2019-12-24 | 2021-07-01 | ||
| JP7351929B2 (en) | 2019-12-24 | 2023-09-27 | 富士フイルム株式会社 | Composition for acoustic lenses, acoustic lenses, acoustic wave probes, ultrasound probes, acoustic wave measurement devices, ultrasound diagnostic devices, photoacoustic wave measurement devices, ultrasound endoscopes, and methods for producing acoustic wave probes |
| CN112111154A (en) * | 2020-09-27 | 2020-12-22 | 北京瑞祥宏远科技有限公司 | Ultrasonic coupling agent for nondestructive testing and preparation method thereof |
| CN116554686A (en) * | 2023-04-27 | 2023-08-08 | 深圳鲲为科技有限公司 | Ultrasonic probe acoustic lens material, ultrasonic probe acoustic lens and preparation method of ultrasonic probe acoustic lens material |
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