CN115160604B - Ultrahigh molecular weight polysiloxane powder and preparation method thereof - Google Patents
Ultrahigh molecular weight polysiloxane powder and preparation method thereof Download PDFInfo
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- C08J2383/00—Characterised by the use 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; Derivatives of such polymers
- C08J2383/04—Polysiloxanes
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/005—Additives being defined by their particle size in general
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- C—CHEMISTRY; METALLURGY
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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
- C08K3/34—Silicon-containing compounds
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- 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
Abstract
The invention relates to a high molecular material, and provides an ultrahigh molecular weight polysiloxane powder and a preparation method thereof in order to prepare polysiloxane powder with wider applicability and better performance, wherein the preparation method comprises the following preparation steps: (1) Heating and mixing the silicon dioxide A and polysiloxane for 35-60min; (2) Adding silicon dioxide B into the mixture obtained in the step (1), continuously mixing uniformly, and kneading into powder for 35-90min. The ultrahigh molecular weight polysiloxane powder and the preparation method thereof are almost suitable for all thermoplastic resin processing, can improve the processing fluidity of the thermoplastic resin, and can improve the surface smoothness of products, reduce the surface friction coefficient and improve the wear resistance and scratch resistance.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to ultrahigh molecular weight polysiloxane powder and a preparation method thereof.
Background
The polysiloxane has the characteristics of smooth molecular chain, extremely low surface energy, excellent high temperature resistance and weather resistance, relatively low reactivity, inertia and the like due to the unique molecular structure, and the organic silicon additive is used as a processing additive of thermoplastic plastics and can achieve an obvious modification effect with a small addition amount.
The silicone master batch takes polysiloxane as an active ingredient and takes different resins as carriers, and the silicone master batch overcomes the defects that the traditional silicone plastic additive and plastic are difficult to uniformly mix and migrate to the surface of a product and is easy to add; however, different silicone masterbatches with different carriers are selected for different material systems, so that the application range of the silicone masterbatches is limited. Silicone powder, i.e., polysiloxane powder, is a powder prepared by using polysiloxane as an active ingredient in combination with silica or other inorganic fillers, and is almost suitable for various thermoplastic resins, regardless of the resin carrier used.
The polysiloxane powder, namely the silicone powder, is powder consisting of polysiloxane and silicon dioxide, in the preparation process of the polysiloxane powder, the larger the molecular weight of siloxane is, the higher the silicone content is, the larger the preparation difficulty is, the lower the molecular weight and the lower the content of common silicone powder on the market are, and when the polysiloxane powder is applied to thermoplastic resin, the silicone powder is easy to precipitate on the surface of a product, so that a series of problems are caused, and the application is limited. Lower silicone content results in the possible incorporation of excess silica and may also negatively impact article performance.
Disclosure of Invention
The invention aims to provide an ultrahigh molecular weight polysiloxane powder and a preparation method thereof, which are applicable to almost all thermoplastic resin processing, can improve the processing fluidity of the thermoplastic resin, and can improve the surface smoothness of products, reduce the surface friction coefficient and improve the wear resistance and scratch resistance.
The embodiment of the invention is realized by the following technical scheme: the preparation method of the ultrahigh molecular weight polysiloxane powder comprises the following preparation steps:
(1) Heating and mixing the silicon dioxide A and polysiloxane for 35-60min;
(2) Adding silicon dioxide B into the mixture obtained in the step (1), continuously mixing uniformly, and kneading into powder for 35-90min.
Further, the components in parts by weight are as follows: 30-70 parts of polysiloxane, 15-25 parts of silicon dioxide A and 25-55 parts of silicon dioxide B.
Further, in the step (1), the mixing temperature of the silicon dioxide A and the polysiloxane is 150-200 ℃, and the rotating speed of a mixer is 20-50rpm; the rotating speed of the mixer in the step (2) is 50-100rpm. Wherein the temperature of the mixer is increased to lower the viscosity of the ultra high molecular weight polysiloxane to facilitate dispersion; firstly, adding silicon dioxide with large median particle size to increase shearing with the ultra-high molecular weight polysiloxane, and then mixing at a low speed, wherein the raw materials are colloidal siloxane and powdery silicon dioxide, so that the low rotating speed can ensure that the siloxane enters the high-structure powdery silicon dioxide, and the large dust pollution is avoided; after the first step of uniform mixing, adding silicon dioxide with small median particle size for secondary dispersion so as to ensure that the ultrahigh molecular weight polysiloxane is uniformly and thoroughly dispersed in the silicon dioxide, and at the moment, high-speed mixing is needed to ensure that the mixture of the siloxane and the silicon dioxide in the step (1) and the silicon dioxide with small median particle size can be uniformly mixed by large shearing.
Further, the polysiloxane in step (1) is of viscosity 10 5 ~5×10 7 Linear polysiloxanes of mPas have a weight-average molecular weight of 500000 to 1000000.
Further, the silica a in the step (1) and the silica B in the step (2) are obtained by modifying a general silica with a surface modifier.
Further, the surface modifier is one or more of chlorosilane, coupling agent, siloxane compound, alcohol ester, organic acid and organic salt.
More specifically, the coupling agent is one or more of a silane coupling agent, a titanate coupling agent and an aluminate coupling agent.
Further, the dosage of the surface modifier is 0.1-5% of the mass fraction of the common silicon dioxide.
More specifically, the median particle diameter of the silicon dioxide A in the step (1) is 25 to 50 μm, and the specific surface area is 100 to 200m 2 (ii) the bulk density is 0.2 to 0.4g/mL;
the median particle diameter of the silicon dioxide B in the step (2) is 1 to 5 mu m, and the specific surface area is 200 to 400m 2 (iii) the bulk density is 0.05 to 0.2g/mL.
The invention also provides the ultrahigh molecular weight polysiloxane powder prepared by the preparation method of the ultrahigh molecular weight polysiloxane powder.
The technical scheme of the embodiment of the invention at least has the following advantages and beneficial effects: the preparation method of the ultra-high molecular weight polysiloxane powder has the following advantages:
1. the surface of the common silicon dioxide contains a large number of polar groups such as hydroxyl groups and the like, so that the common silicon dioxide is easy to adsorb water molecules, has poor dispersibility, is easy to generate secondary aggregation and the like.
2. The viscosity of the ultra-high molecular weight polysiloxane is reduced by the matching of the process in the powder preparation process, such as increasing the temperature of a mixer, so that the ultra-high molecular weight polysiloxane is easier to disperse; firstly, adding silicon dioxide with large median particle size to increase shearing with the ultrahigh molecular weight polysiloxane, and then adding silicon dioxide with small median particle size to carry out secondary dispersion, thereby ensuring that the ultrahigh molecular weight polysiloxane is uniformly and thoroughly dispersed in the silicon dioxide.
3. The polysiloxane powder without organic carrier prepared by the preparation method is almost suitable for all thermoplastic resin processing, can improve the processing fluidity of the thermoplastic resin, and can improve the surface smoothness of products, reduce the surface friction coefficient, improve the wear resistance and scratch resistance and the like.
4. By the preparation method, the polysiloxane powder with ultrahigh molecular weight can be prepared, and simultaneously, siloxane powder products with different molecular weights and different median particle size distributions can be conveniently prepared according to specific application requirements.
Detailed Description
Example 1
The embodiment provides a preparation method of ultrahigh molecular weight polysiloxane powder, which comprises the following steps:
(1) The viscosity is 5X 10 7 60 parts of mPa s linear polysiloxane and 20 parts of silica A were mixed in a low-speed mixer at 150 ℃ for 40min (noted as mixing time in section A), the speed of the mixer being 20rpm. Wherein the dosage of the silane coupling agent in the silicon dioxide A is 0.1 percent of the dosage of the common silicon dioxide, the median particle diameter of the silicon dioxide A is 25 mu m, and the specific surface area is 150m 2 (ii)/g, bulk density 0.2g/mL;
(2) Adding 20 parts of silicon dioxide B into the mixture in the step (1), and continuously mixing in a low-speed mixer at 150 ℃ for 40min (recorded as mixing time of section B), wherein the rotating speed of the mixer is 50rpm; wherein the dosage of the alkane coupling agent in the silicon dioxide B is 0.1 percent of the dosage of the common silicon dioxide, the median particle diameter of the silicon dioxide B is 5 mu m, and the specific surface area is 250m 2 Per g, bulk density of0.05g/mL. The polysiloxane powder produced is designated SF-1.
Example 2
This example provides a process for the preparation of an ultra-high molecular weight polysiloxane powder, which differs from example 1 in that: the mixing time of the section A is 35min, and the rotating speed of a mixer is 50rpm; the mixing time of the section B is 35min, and the rotating speed of the mixer is 100rpm. The polysiloxane powder produced is designated SF-2.
Example 3
This example provides a process for the preparation of an ultra-high molecular weight polysiloxane powder, which differs from example 1 in that: mixing time for section A is 60min. The polysiloxane powder produced is noted SF-3.
Example 4
This example provides a process for the preparation of an ultra-high molecular weight polysiloxane powder, which differs from example 1 in that: and mixing for 50min in the section B, and marking the prepared polysiloxane powder as SF-4.
Example 5
This example provides a method for preparing an ultra-high molecular weight polysiloxane powder, which differs from example 1 in that: the mixing time of the A section is 60min, the mixing time of the B section is 90min, and the prepared polysiloxane powder is marked as SF-5.
Example 6
The embodiment provides a preparation method of ultrahigh molecular weight polysiloxane powder, which comprises the following steps:
(1) The viscosity is 5X 10 7 30 parts of mPa & s linear polysiloxane and 15 parts of silicon dioxide A are mixed in a low-speed mixer at 150 ℃ for 40min (recorded as mixing time of A section); wherein the dosage of the silane coupling agent in the silicon dioxide A is 2.5 percent of the dosage of the common silicon dioxide, the median particle diameter of the silicon dioxide A is 30 mu m, and the specific surface area is 100m 2 (ii)/g, bulk density 0.3g/mL;
(2) To the mixture in step (1) was added 25 parts of silica B and mixing was continued in a low speed mixer at 150 ℃ for 40min (noted as B-stage mixing time). Wherein the dosage of the alkane coupling agent in the silicon dioxide B is 2.5 percent of the dosage of the common silicon dioxide, the median particle diameter of the silicon dioxide B is 1 mu m, and the specific surface areaProduct of 400m 2 (ii)/g, bulk density 0.2g/mL.
Example 7
The embodiment provides a preparation method of ultrahigh molecular weight polysiloxane powder, which comprises the following steps:
(1) The viscosity is 5X 10 7 70 parts of mPa & s linear polysiloxane and 25 parts of silicon dioxide A are mixed in a low-speed mixer at 150 ℃ for 40min (recorded as mixing time in the stage A); wherein the dosage of the silane coupling agent in the silicon dioxide A is 5 percent of the dosage of the common silicon dioxide, the median particle diameter of the silicon dioxide A is 50 mu m, and the specific surface area is 200m 2 (iv)/g, bulk density of 0.4g/mL;
(2) 55 parts of silica B are added to the mixture from step (1) and mixing is continued in a low-speed mixer at 150 ℃ for 40min (noted as B-stage mixing time). Wherein the dosage of the alkane coupling agent in the silicon dioxide B is 5 percent of the dosage of the common silicon dioxide, the median particle diameter of the silicon dioxide B is 3 mu m, and the specific surface area is 200m 2 (ii)/g, bulk density 0.05g/mL.
Example 8
This example provides a process for the preparation of an ultra-high molecular weight polysiloxane powder, which differs from example 1 in that: the temperature in the low speed mixer is 200 ℃, the mixing time of the A section is 35min, and the mixing time of the B section is 35min. The polysiloxane powder prepared is noted SF-8
Example 9
This example provides a method for preparing an ultra-high molecular weight polysiloxane powder, which differs from example 1 in that: the viscosity of the linear polysiloxane was 10 5 mPa·s。
Comparative example 1
This comparative example provides a process for the preparation of an ultra-high molecular weight polysiloxane powder, which differs from example 8 in that: the temperature of the low-speed mixer is room temperature and is not heated; the polysiloxane powder produced is denoted SK-1.
Comparative example 2
This comparative example provides a process for the preparation of an ultra-high molecular weight polysiloxane powder which differs from example 1 in that: the viscosity of the polysiloxane was 5X 10 4 mPa · s. System for makingThe polysiloxane powder prepared was designated SK-2.
Comparative example 3
This comparative example provides a process for the preparation of an ultra-high molecular weight polysiloxane powder which differs from example 1 in that: firstly adding the silicon dioxide B and then adding the silicon dioxide A, wherein the mixing speed and the mixing time are unchanged. The polysiloxane powder produced was noted SK-3.
Comparative example 4
This comparative example provides a process for the preparation of an ultra-high molecular weight polysiloxane powder which differs from example 1 in that: adding the silicon dioxide A and the silicon dioxide B together, firstly mixing at the rotating speed of 20rpm for 40min, and then mixing at the rotating speed of 50rpm for 40min. The polysiloxane powder produced with the mixing speed is denoted as SK-4.
Experimental example 1
Powdering property
The powder morphology of the ultra-high molecular weight polysiloxane powders marked SF-1, SF-2, SF-3, SF-4, SF-5, SF-8, SK-1, SK-2, SK-3, SK-4 obtained in examples 1-5, 8 and comparative examples 1-4 was observed, respectively. The results are shown in table 1 below.
TABLE 1 summary of the times and morphology for the preparation of the polysiloxane powders of examples 1-5, 8 and comparative examples 1-4
From the results of examples 1 to 5 and the results of comparative examples 1 to 4, it can be seen that: by adopting the method, part of the silicon dioxide A with the specific surface area lower than that of the silicon dioxide A is added to increase the shearing between the silicon dioxide A and the polysiloxane, so that the silicon dioxide A is pre-dispersed, and then the silicon dioxide B with the specific surface area higher than that of the silicon dioxide A is added according to the requirement to further disperse, and the polysiloxane powder product with uniform median particle size can be prepared. The common silicon dioxide is modified, silanol groups on the surface of the common silicon dioxide can be reduced, hydrogen bonds among silicon dioxide particles are further reduced, the silicon dioxide is easy to disperse, and the time for mixing the silicon dioxide into uniform powder is shorter, in the comparative example 3, after the adding sequence of the silicon dioxide A and the silicon dioxide B is changed, the silicon dioxide B which is added first and has a large specific surface area cannot be well dispersed with polysiloxane in the same time, and the final powder has a large number of large particles. Comparative example 4 was added all at once and mixed, and it was not possible to mix silica and polysiloxane uniformly, resulting in a large number of large particles in the final powder. Comparative example 1 the mixing temperature was lowered compared to example 8, resulting in large particles in the final powder and non-uniform particle size.
In the preparation process, by adjusting the process conditions, compared with the example 1, in the example 2, the powdering time can also be shortened after the rotating speed is increased and the shearing is increased; example 8 compares to example 1 by increasing the temperature of the mixer and thereby decreasing the viscosity of the ultra high molecular weight polysiloxane, making it easier to disperse and shorter time to mix into a uniform powder.
Experimental example 2
Rheological Properties, gloss and Friction coefficient measurements
The experimental example is provided with 10 groups, the raw materials of each experimental group are weighed according to the proportion (weight parts, the same below) of the following table 2 except for the selection of the polysiloxane powder, the raw materials are mixed and granulated by a double screw, and then the mixture is added into a capillary extrusion device of a torque rheometer, and the extrusion die is a sheet die to test the rheological property. The particles were injection molded into a light panel to test the coefficient of friction against PE film. The selection of polysiloxane particles for each experimental group is shown in Table 3 below (where SF-1, SF-2, SF-3, SF-4, SF-5 were obtained by examples 1-5, respectively, and SK-1, SK-2, SK-3, SK-4 were obtained by comparative examples 1-4). The results of the rheological property measurements for each experimental group are shown in table 4. The results of the friction coefficient for each experimental group are shown in table 5.
TABLE 2 proportions of the raw materials added to the twin-screw granulator
| Raw materials | PC | ABS | MBS | Antioxidant agent | Black masterbatch | Polysiloxane particles |
| Proportioning | 67.5 | 25 | 5 | 0.6 | 1.5 | Is free of |
Table 3 selection of polysiloxane particles for each experimental group
| Experimental groups | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 |
| Polysiloxane particles | Is free of | SF-1 | SF-2 | SF-3 | SF-4 | SF-5 | SK-1 | SK-2 | SK-3 | SK-4 |
| Addition of Silicone particles | Is composed of | 2 | 2 | 2 | 2 | 2 | 2 | 2 | 2 | 2 |
TABLE 4 evaluation of rheological Properties of the test groups
| Experimental groups | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 |
| Polysiloxane particles | Is free of | SF-1 | SF-2 | SF-3 | SF-4 | SF-5 | SK-1 | SK-2 | SK-3 | SK-4 |
| Extrusion Torque (Nm) | 56-59 | 48-51 | 49-52 | 48-51 | 49-52 | 48-51 | 48-59 | 47-51 | 49-60 | 48-59 |
| Extrusion pressure (MPa) | 45-47 | 40-42 | 40-42 | 40-42 | 40-42 | 40-42 | 40-47 | 38-40 | 40-47 | 39-48 |
TABLE 5 evaluation of Friction coefficient of each test group
| Experimental groups | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 |
| Polysiloxane particles | Is free of | SF-1 | SF-2 | SF-3 | SF-4 | SF-5 | SK-1 | SK-2 | SK-3 | SK-4 |
| Coefficient of static friction | 0.400 | 0.275 | 0.280 | 0.270 | 0.279 | 0.281 | 0.356 | 0.250 | 0.348 | 0.339 |
| Coefficient of dynamic friction | 0.356 | 0.230 | 0.234 | 0.231 | 0.240 | 0.230 | 0.278 | 0.215 | 0.267 | 0.261 |
From the experimental results of table 4, it can be seen that:
by comparing the results of experimental group 1 with those of experimental groups 2 to 6, it can be understood that: the ultra-high molecular weight polysiloxane prepared by the method of the invention is used as a lubricant to be added into thermoplastic resin, so that the torque and pressure in the processing process can be effectively reduced, and the energy consumption in the actual production process can be reduced.
As can be seen from the comparison of the results of experimental groups 2 to 6 and 7, the ultra-high molecular weight polysiloxane powder prepared by the method of the present invention is excellent, while the polysiloxane powder of experimental groups 8,9 and 10 is prepared by a method which causes non-uniform dispersion and finally does not have good effect in application in thermoplastic resins, and the torque pressure fluctuates greatly.
As can be seen by comparing the results of experimental groups 2 to 6 with the results of experimental group 8, experimental group 8 was found to have lower torque pressure than the ultra-high molecular weight polysiloxane due to the low molecular weight polysiloxane used, and the above results were in accordance with the theoretical values.
From the experimental results of table 5, it can be seen that:
by comparing the results of experimental group 1 with those of experimental groups 2 to 8, it can be understood that: the coefficient of friction of the substrate decreases after the addition of the silicone powder. Experimental groups 7,9, 10 did not show a significant decrease in the friction coefficient because the polysiloxane powder itself was not well dispersed, resulting in poor dispersion in the thermoplastic resin, and experimental group 8 had a lower friction coefficient because it was not an ultra-high molecular weight polysiloxane, which was in line with the theoretical results.
Experimental example 3
In this example, 10 groups (the raw materials are the same as those in example 2) were set, polysiloxane powders marked as SF-1, SF-2, SF-3, SF-4, SF-5, SK-1, SK-2, SK-3, and SK-4 were added to a PP/POE/talc powder (weight ratio 71, 8) system, and injection molded into a 2mm thick plate for scratch resistance (popular PV3952, the smaller the Δ L value, the better the scratch resistance) and migration test (PV 1306,6 cycles, 96 h/cycle), and the results are shown in Table 6 below.
TABLE 6 scratch resistance and migration test results for each experimental group
| Experimental groups | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 |
| Polysiloxane particles | Is free of | SF-1 | SF-2 | SF-3 | SF-4 | SF-5 | SK-1 | SK-2 | SK-3 | SK-4 |
| △L | 3.52 | 1.35 | 1.40 | 1.34 | 1.45 | 1.38 | 2.52 | 3.01 | 2.63 | 2.56 |
| Stickiness on the surface | > 6 cycles | > 6 cycles | > 6 cycles | > 6 cycles | > 6 cycles | Greater than 6 cycles | 5 period(s) | 3 period of | 5 period(s) | 5 period(s) |
From the experimental results of table 6, it can be seen that:
the polysiloxane powder of experimental groups 2-6 has better scratch resistance and migration resistance, and no stickiness phenomenon occurs in the whole stickiness test; while the scratch resistance was not exhibited because the polysiloxane powder itself was not well dispersed in the thermoplastic resin in experimental groups 7,9 and 10, and the scratch resistance was poor and liable to bleed out because the polysiloxane powder was not ultra-high molecular weight.
In conclusion, the ultrahigh molecular weight polysiloxane powder prepared by the preparation method disclosed by the invention has uniform median particle size, and when the ultrahigh molecular weight polysiloxane powder is applied to a resin processing process, the rheological property, the wear resistance, the scratch resistance and the like of resin are obviously improved, and the ultrahigh molecular weight polysiloxane powder is not easy to precipitate to meet the actual use performance.
The present invention has been described in terms of the preferred embodiment, and it is not intended to be limited to the embodiment. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. A preparation method of ultrahigh molecular weight polysiloxane powder is characterized by comprising the following preparation steps:
(1) Heating and mixing the silicon dioxide A and polysiloxane for 35-60min;
(2) Adding silicon dioxide B into the mixture obtained in the step (1), continuously mixing uniformly, and kneading into powder for 35-90min;
the polysiloxane in the step (1) has the viscosity of 10 5 ~5×10 7 Linear polysiloxane of mPa.s, the weight-average molecular weight is 500000 to 1000000;
the median particle diameter of the silicon dioxide A in the step (1) is 25-50 μm, and the specific surface area is 100-200 m 2 (ii) the bulk density is 0.2 to 0.4g/mL;
the median particle diameter of the silicon dioxide B in the step (2) is 1-5 mu m, and the specific surface area is 200-400 m 2 (iii) the bulk density is 0.05 to 0.2g/mL.
2. The method for preparing ultra-high molecular weight polysiloxane powder according to claim 1, wherein the mass parts of the components are as follows: 30-70 parts of polysiloxane, 15-25 parts of silicon dioxide A and 25-55 parts of silicon dioxide B.
3. The method for preparing ultra-high molecular weight polysiloxane powder according to claim 1, wherein the mixing temperature of silicon dioxide A and polysiloxane in step (1) is 150-200 ℃, and the rotation speed of the mixer is 20-50rpm; the rotating speed of the mixer in the step (2) is 50-100rpm.
4. The method for producing an ultra-high molecular weight polysiloxane powder according to claim 1, wherein the silica A in step (1) and the silica B in step (2) are obtained by modifying ordinary silica with a surface modifier.
5. The method of claim 4, wherein the surface modifier is one or more of chlorosilanes, coupling agents, silicone compounds, alcohol esters, organic acids, and organic salts.
6. The method of claim 5, wherein the coupling agent is one or more of a silane coupling agent, a titanate coupling agent, and an aluminate coupling agent.
7. The method for preparing ultra-high molecular weight polysiloxane powder according to claim 4, wherein the amount of the surface modifier is 0.1-5% of the mass fraction of the common silicon dioxide.
8. An ultra-high molecular weight polysiloxane powder obtained by the method for preparing an ultra-high molecular weight polysiloxane powder according to any one of claims 1 to 7.
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| JP3464527B2 (en) * | 1994-05-27 | 2003-11-10 | 東レ・ダウコーニング・シリコーン株式会社 | Curable resin composition and cured resin |
| JPH11116693A (en) * | 1997-10-17 | 1999-04-27 | Dow Corning Toray Silicone Co Ltd | Continuous production of silicone rubber base |
| DE10330287A1 (en) * | 2003-07-04 | 2004-02-26 | Wacker-Chemie Gmbh | Filler-containing organopolysiloxane granules useful as additives for thermoplastics have a defined particle size |
| JP2009191155A (en) * | 2008-02-14 | 2009-08-27 | Shin Etsu Chem Co Ltd | Method for producing liquid silicone rubber base and method for producing addition curing type liquid silicone rubber composition |
| JP5687920B2 (en) * | 2010-03-03 | 2015-03-25 | 日本エイアンドエル株式会社 | Thermoplastic resin composition |
| CN102337031B (en) * | 2011-06-29 | 2013-02-13 | 南京四新科技应用研究所有限公司 | Organosilicon composition with low viscosity and preparation method thereof |
| JP6227700B2 (en) * | 2016-04-18 | 2017-11-08 | 株式会社トウペ | Silicone resin composition and painted product |
| JP6973307B2 (en) * | 2018-06-26 | 2021-11-24 | 信越化学工業株式会社 | Silicone adhesive grease composition and its manufacturing method |
| CN112029296B (en) * | 2020-09-17 | 2022-05-24 | 成都思立可科技有限公司 | Organic carrier-free polysiloxane particles and preparation method thereof |
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