CN115895023B - Organic silicon foaming sheet and preparation method thereof - Google Patents
Organic silicon foaming sheet and preparation method thereof Download PDFInfo
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- CN115895023B CN115895023B CN202211254559.8A CN202211254559A CN115895023B CN 115895023 B CN115895023 B CN 115895023B CN 202211254559 A CN202211254559 A CN 202211254559A CN 115895023 B CN115895023 B CN 115895023B
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W90/00—Enabling technologies or technologies with a potential or indirect contribution to greenhouse gas [GHG] emissions mitigation
- Y02W90/10—Bio-packaging, e.g. packing containers made from renewable resources or bio-plastics
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Abstract
The invention discloses an organic silicon foaming sheet, which comprises the following components in parts by weight: 80-100 parts by weight of organic silicon resin composition and 40-50 parts by weight of modified chitosan sol solution. The preparation method of the organic silicon foaming sheet comprises the following steps: s1, coating an organic silicon resin composition on a lower polytetrafluoroethylene film on an automatic coating machine; s2, coating the modified chitosan sol solution on the organic silicon resin composition in the step S1; s3, covering an upper polytetrafluoroethylene film on the surface of the modified chitosan sol solution; s4, performing heat curing on the film layer in the step S3; s5, removing the lower polytetrafluoroethylene film and the upper polytetrafluoroethylene film after the heat curing in the step S4 to obtain a cured intermediate; and S6, uniformly coating the organic silicon resin composition on the surface of the cured intermediate, and performing heat curing to obtain the organic silicon foaming sheet. The organic silicon foaming sheet and the preparation method thereof have low communicated porosity and good mechanical properties.
Description
Technical Field
The invention relates to the field of foaming sheets, in particular to an organic silicon foaming sheet and a preparation method thereof.
Background
The foaming sheet material can still have higher impact absorption performance under the thinner condition, so the foaming sheet material is widely applied to electronic equipment such as smart phones, personal computers, electronic paper and the like, is configured between an electronic component and a frame structural member, and plays a role in buffering and sealing. For the existing polyolefin foaming sheet, the too high foaming temperature in the preparation process leads to too high aperture ratio, and meanwhile, the diameter of the foam cells is larger, so that the cushioning property of the foaming material is poor.
Disclosure of Invention
In view of the above, the present invention aims to provide an organosilicon foam sheet and a preparation method thereof, wherein the organosilicon foam sheet has low interconnected porosity and good mechanical properties.
In order to achieve the above purpose, the present invention provides the following technical solutions:
an organic silicon foaming sheet comprises the following components in parts by weight: comprises 80-100 parts by weight of organic silicon resin composition and 40-50 parts by weight of modified chitosan sol solution.
Preferably, the weight part ratio of the organic silicon resin composition to the modified chitosan sol solution is 2:1.
Preferably, the silicone resin composition comprises the following components in parts by weight: 40-60 parts of carbon hydroxyl modified organopolysiloxane, 40-60 parts of epoxy resin, 5-8 parts of polylactic acid, 10-30 parts of alkylphenol ethoxylates, 4-6 parts of sodium bicarbonate, 60-80 parts of water and 1-2 parts of zinc stearate.
Preferably, the molecular weight of the carbon hydroxyl modified organopolysiloxane is 2700 to 3800.
The preparation method of the organic silicon foaming sheet comprises the following steps:
s1, coating an organic silicon resin composition on a lower polytetrafluoroethylene film on an automatic coating machine;
s2, coating the modified chitosan sol solution on the organic silicon resin composition in the step S1;
s3, covering an upper polytetrafluoroethylene film on the surface of the modified chitosan sol solution;
s4, performing heat curing on the film layer in the step S3 for 1-2h;
s5, removing the lower polytetrafluoroethylene film and the upper polytetrafluoroethylene film after the heat curing in the step S4 to obtain a cured intermediate;
and S6, uniformly coating the organic silicon resin composition on the surface of the cured intermediate, and performing reheat curing for 2-4 hours to obtain the organic silicon foaming sheet.
Preferably, the preparation method of the modified chitosan sol solution in the step S2 comprises the following steps:
adding chitosan into graphene oxide-nano silica sol solution, and mixing solution of acetic acid and hydrogen peroxide, and stirring for 4-6h at 60-70 ℃ to obtain modified chitosan sol solution.
Preferably, the weight part ratio of the chitosan, the graphene oxide-nano silica sol solution, the acetic acid and the hydrogen peroxide is 1:1:3:1.
Preferably, the preparation method of the graphene oxide-nano silica sol solution comprises the following steps: mixing tetraethoxysilane, graphene oxide, ethanol solution with the volume fraction of 75% and nitric acid solution with the volume fraction of 55%, regulating the pH value to 3-4, and stirring for 12-14h to obtain graphene oxide-silicon dioxide sol.
Preferably, the weight part ratio of the tetraethoxysilane to the graphene oxide to the ethanol solution to the nitric acid solution is 2:1:6:3.
Preferably, the temperature of the thermal curing in step S2 is 40-60 ℃.
The graphene oxide surface in the modified chitosan sol solution contains a large number of polar functional groups, has a larger specific surface area, increases the bonding strength of each component, and further improves the interfacial bonding capability between the modified chitosan sol solution and the organic silicon resin composition, so that the interfacial property of the sheet can be improved, the mechanical modulus of the sheet is improved, and the tensile property and the compression property of the sheet are increased.
In addition, the graphene oxide-nano silicon oxide nanostructure has more stable bonding tension and dimensional stability, can ensure that the steric hindrance of foam molding is more compact and uniform, and further repairs the defects on the surface of the cells, so that the density of the cells is uniform.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention. In addition, the raw materials and the equipment according to the present invention are commercially available, and are not specifically exemplified, and the raw materials according to the present invention are commercially available and are well known to those skilled in the art.
Example 1:
an organic silicon foaming sheet comprises the following components in parts by weight: comprises 100 parts by weight of a silicone resin composition and 50 parts of a modified chitosan sol solution.
Wherein the weight ratio of the organic silicon resin composition to the modified chitosan sol solution is 2:1.
The organic silicon resin composition comprises the following components in parts by weight: 60 parts of carbon hydroxyl modified organopolysiloxane with molecular weight of 2700-3800, 60 parts of epoxy resin, 8 parts of polylactic acid, 30 parts of alkylphenol ethoxylate, 6 parts of sodium bicarbonate, 80 parts of water and 2 parts of zinc stearate.
The preparation method of the organic silicon foaming sheet comprises the following steps:
s1, coating the organic silicon resin composition on a lower polytetrafluoroethylene film on an automatic coating machine;
s2, coating the modified chitosan sol solution on the organic silicon resin composition in the step S1;
s3, covering the surface of the modified chitosan sol solution coated on the organic silicon resin composition in the step S1 with an upper polytetrafluoroethylene film to obtain a two-component coating film layer;
s4, performing heat curing on the film layer obtained in the step S3 for 2 hours at 60 ℃;
s5, removing the lower polytetrafluoroethylene film and the upper polytetrafluoroethylene film after the heat curing in the step S4 to obtain a cured intermediate;
and S6, uniformly coating the organosilicon resin composition on the surface of the curing intermediate, and thermally curing for 4 hours at 60 ℃ to obtain the organosilicon foaming sheet.
The preparation method of the modified chitosan sol solution in the step S2 comprises the following steps:
adding chitosan into a graphene oxide-nano silica sol solution and a mixed solution of acetic acid and hydrogen peroxide, and stirring for 6 hours at 70 ℃ to obtain a modified chitosan sol solution, wherein the weight ratio of the chitosan to the graphene oxide-nano silica sol solution to the acetic acid to the hydrogen peroxide is 1:1:3:1.
The preparation method of the graphene oxide-nano silica sol solution comprises the following steps: mixing ethyl orthosilicate, graphene oxide, an ethanol solution with the volume fraction of 75% and a nitric acid solution with the volume fraction of 55%, adjusting the pH value to 3-4, and stirring for 14h to obtain graphene oxide-silicon dioxide sol, wherein the weight ratio of the ethyl orthosilicate to the graphene oxide to the ethanol solution to the nitric acid solution is 2:1:6:3.
Example 2:
an organic silicon foaming sheet comprises the following components in parts by weight: comprises 80 parts by weight of organic silicon resin composition and 40 parts by weight of modified chitosan sol solution.
Wherein the weight ratio of the organic silicon resin composition to the modified chitosan sol solution is 2:1.
The organic silicon resin composition comprises the following components in parts by weight: 40 parts of carbon hydroxyl modified organopolysiloxane with molecular weight of 2700-3800, 40 parts of epoxy resin, 5 parts of polylactic acid, 10 parts of alkylphenol ethoxylate, 4 parts of sodium bicarbonate, 60 parts of water and 1 part of zinc stearate.
The preparation method of the organic silicon foaming sheet comprises the following steps:
s1, coating the organic silicon resin composition on a lower polytetrafluoroethylene film on an automatic coating machine;
s2, coating the modified chitosan sol solution on the organic silicon resin composition in the step S1;
s3, covering the surface of the modified chitosan sol solution coated on the organic silicon resin composition in the step S1 with an upper polytetrafluoroethylene film to obtain a two-component coating film layer;
s4, performing heat curing on the film layer obtained in the step S3 for 1h at the temperature of 40 ℃;
s5, removing the lower polytetrafluoroethylene film and the upper polytetrafluoroethylene film after the heat curing in the step S4 to obtain a cured intermediate;
and S6, uniformly coating the organosilicon resin composition on the surface of the curing intermediate, and thermally curing for 2 hours at 40 ℃ to obtain the organosilicon foaming sheet.
The preparation method of the modified chitosan sol solution in the step S2 comprises the following steps:
adding chitosan into a graphene oxide-nano silica sol solution and a mixed solution of acetic acid and hydrogen peroxide, and stirring for 4 hours at 60 ℃ to obtain a modified chitosan sol solution, wherein the weight ratio of the chitosan to the graphene oxide-nano silica sol solution to the acetic acid to the hydrogen peroxide is 1:1:3:1.
The preparation method of the graphene oxide-nano silica sol solution comprises the following steps: mixing ethyl orthosilicate, graphene oxide, an ethanol solution with the volume fraction of 75% and a nitric acid solution with the volume fraction of 55%, adjusting the pH value to 3-4, and stirring for 12 hours to obtain graphene oxide-silicon dioxide sol, wherein the weight ratio of the ethyl orthosilicate to the graphene oxide to the ethanol solution to the nitric acid solution is 2:1:6:3.
Example 3:
an organic silicon foaming sheet comprises the following components in parts by weight: comprises 90 parts by weight of organic silicon resin composition and 45 parts by weight of modified chitosan sol solution.
Wherein the weight ratio of the organic silicon resin composition to the modified chitosan sol solution is 2:1.
The organic silicon resin composition comprises the following components in parts by weight: 50 parts of carbon hydroxyl modified organopolysiloxane with molecular weight of 2700-3800, 50 parts of epoxy resin, 6 parts of polylactic acid, 20 parts of alkylphenol ethoxylates, 5 parts of sodium bicarbonate, 70 parts of water and 1.5 parts of zinc stearate.
The preparation method of the organic silicon foaming sheet comprises the following steps:
s1, coating the organic silicon resin composition on a lower polytetrafluoroethylene film on an automatic coating machine;
s2, coating the modified chitosan sol solution on the organic silicon resin composition in the step S1;
s3, covering the surface of the modified chitosan sol solution coated on the organic silicon resin composition in the step S1 with an upper polytetrafluoroethylene film to obtain a two-component coating film layer;
s4, performing heat curing on the film layer obtained in the step S3 at 50 ℃ for 1.5 hours;
s5, removing the lower polytetrafluoroethylene film and the upper polytetrafluoroethylene film after the heat curing in the step S4 to obtain a cured intermediate;
and S6, uniformly coating the organosilicon resin composition on the surface of the curing intermediate, and thermally curing at 50 ℃ for 3 hours to obtain the organosilicon foaming sheet.
The preparation method of the modified chitosan sol solution in the step S2 comprises the following steps:
adding chitosan into a graphene oxide-nano silica sol solution and a mixed solution of acetic acid and hydrogen peroxide, and stirring for 5 hours at 65 ℃ to obtain a modified chitosan sol solution, wherein the weight ratio of the chitosan to the graphene oxide-nano silica sol solution to the acetic acid to the hydrogen peroxide is 1:1:3:1.
The preparation method of the graphene oxide-nano silica sol solution comprises the following steps: mixing ethyl orthosilicate, graphene oxide, an ethanol solution with the volume fraction of 75% and a nitric acid solution with the volume fraction of 55%, adjusting the pH value to 3-4, and stirring for 13h to obtain graphene oxide-silicon dioxide sol, wherein the weight ratio of the ethyl orthosilicate to the graphene oxide to the ethanol solution to the nitric acid solution is 2:1:6:3.
Comparative example 1:
comparative example 1 was prepared in substantially the same manner as in example 1, except that no modified chitosan sol solution was used, specifically:
an organic silicon foaming sheet comprises the following components in parts by weight: comprises 100 parts by weight of a silicone resin composition.
The organic silicon resin composition comprises the following components in parts by weight: 60 parts of carbon hydroxyl modified organopolysiloxane with molecular weight of 2700-3800, 60 parts of epoxy resin, 8 parts of polylactic acid, 30 parts of alkylphenol ethoxylate, 6 parts of sodium bicarbonate, 80 parts of water and 2 parts of zinc stearate.
The preparation method of the organic silicon foaming sheet comprises the following steps:
s1, coating the organic silicon resin composition on a lower polytetrafluoroethylene film on an automatic coating machine;
s2, covering the surface of the organic silicon resin composition coated in the step S1 with an upper polytetrafluoroethylene film to obtain a coating film layer;
s3, performing heat curing on the film layer obtained in the step S2 for 2 hours at 60 ℃;
s4, removing the lower polytetrafluoroethylene film and the upper polytetrafluoroethylene film after the heat curing in the step S4 to obtain a cured intermediate;
and S5, uniformly coating the organosilicon resin composition on the surface of the curing intermediate, and thermally curing for 4 hours at 60 ℃ to obtain the organosilicon foaming sheet.
The silicone foam cushions of examples 1 to 3, commercially available Shanghai Xiangcheng specialty rubber products Co., ltd., and the silicone foam sheet obtained in comparative example 1 were each tested for closed cell ratio, open cell ratio, compressive strength, tensile strength and elongation at break.
Determination of closed cell content:
the closed cell ratio F1 and the closed cell ratio F2 of the sample are calculated according to ASTM D2856 (1998) standard:
the aperture ratio F1 (%) =100× (W2-W1)/V2
Closed cell content F2 (%) =100-F1
Measurement of the interconnected porosity: measured using an Xradia 520 Versa type X-ray tomography scanner.
Determination of compressive Strength: according to ISO3386-1, a material having a thickness of 10mm or less was laminated to a thickness of 10mm or more, and the compression rate was set as close as possible to 50% of the material thickness per minute, and the compression stress at 25% deformation was measured.
Tensile strength measurement: the test was carried out according to GB/T6344-2008 "determination of tensile Strength and elongation at break of Soft foam Polymer Material".
As can be seen from the above table, examples 1 to 3 have improved closed cell ratio, compressive strength and tensile strength as compared with those of the foamed sheet of comparative example 1 and the commercially available foamed sheet, indicating that the foamed sheet of the present invention has high closed cell ratio, low open cell ratio and good mechanical properties.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (8)
1. An organosilicon foaming sheet material is characterized in that: comprises the following components in parts by weight: 80-100 parts by weight of organic silicon resin composition and 40-50 parts by weight of modified chitosan sol solution, wherein the weight ratio of the organic silicon resin composition to the modified chitosan sol solution is 2:1, and the organic silicon resin composition comprises the following components in parts by weight: 40-60 parts of carbon hydroxyl modified organopolysiloxane, 40-60 parts of epoxy resin, 5-8 parts of polylactic acid, 10-30 parts of alkylphenol ethoxylates, 4-6 parts of sodium bicarbonate, 60-80 parts of water and 1-2 parts of zinc stearate;
the preparation method of the modified chitosan sol solution comprises the following steps:
adding chitosan into graphene oxide-nano silica sol solution, and mixing solution of acetic acid and hydrogen peroxide, and stirring for 4-6h at 60-70 ℃ to obtain modified chitosan sol solution.
2. The silicone foam sheet according to claim 1, wherein: the molecular weight of the carbon hydroxyl modified organopolysiloxane is 2700-3800.
3. A method for producing the silicone foamed sheet according to claim 1, wherein: the method comprises the following steps:
s1, coating an organic silicon resin composition on a lower polytetrafluoroethylene film on an automatic coating machine;
s2, coating the modified chitosan sol solution on the organic silicon resin composition in the step S1;
s3, covering an upper polytetrafluoroethylene film on the surface of the modified chitosan sol solution;
s4, performing heat curing on the film layer in the step S3 for 1-2h;
s5, removing the lower polytetrafluoroethylene film and the upper polytetrafluoroethylene film after the heat curing in the step S4 to obtain a cured intermediate;
and S6, uniformly coating the organic silicon resin composition on the surface of the cured intermediate, and performing reheat curing for 2-4 hours to obtain the organic silicon foaming sheet.
4. A method for producing the silicone foamed sheet according to claim 3, wherein: the preparation method of the modified chitosan sol solution in the step S2 comprises the following steps:
adding chitosan into graphene oxide-nano silica sol solution, and mixing solution of acetic acid and hydrogen peroxide, and stirring for 4-6h at 60-70 ℃ to obtain modified chitosan sol solution.
5. The method for preparing the organic silicon foaming sheet according to claim 4, wherein the weight ratio of the chitosan, the graphene oxide-nano silica sol solution, the acetic acid and the hydrogen peroxide is 1:1:3:1.
6. The method for preparing the organic silicon foaming sheet according to claim 5, wherein the method for preparing the graphene oxide-nano silica sol solution comprises the following steps: mixing tetraethoxysilane, graphene oxide, ethanol solution with the volume fraction of 75% and nitric acid solution with the volume fraction of 55%, regulating the pH value to 3-4, and stirring for 12-14h to obtain graphene oxide-silicon dioxide sol.
7. The method for preparing the organic silicon foaming sheet according to claim 6, wherein the weight ratio of the tetraethoxysilane to the graphene oxide to the ethanol solution to the nitric acid solution is 2:1:6:3.
8. The method for producing a silicone foamed sheet according to claim 7, wherein the heat curing temperature is 40 to 60 ℃.
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| CN106433139A (en) * | 2016-09-29 | 2017-02-22 | 中国工程物理研究院核物理与化学研究所 | Low-density and high-porosity silicone rubber foam material and preparation method thereof |
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| CN113462166A (en) * | 2021-07-08 | 2021-10-01 | 湖北祥源新材科技股份有限公司 | Organic silicon foamed sheet for electronic products and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| AU2014315160B2 (en) * | 2013-09-04 | 2018-02-15 | Ghassan Dehni | Flexible polyurethane and polyurethane/polyorganosiloxane foam materials that absorb impact energy |
| JP6622178B2 (en) * | 2016-12-05 | 2019-12-18 | 信越化学工業株式会社 | Condensation curable silicone resin composition sheet, method for producing condensation curable silicone resin composition sheet, and method for producing light emitting device |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108431107A (en) * | 2015-12-25 | 2018-08-21 | 日东电工株式会社 | Organosilicon foam sheet and its manufacturing method |
| CN106433139A (en) * | 2016-09-29 | 2017-02-22 | 中国工程物理研究院核物理与化学研究所 | Low-density and high-porosity silicone rubber foam material and preparation method thereof |
| EP3653576A2 (en) * | 2018-11-16 | 2020-05-20 | National Chung-Shan Institute of Science and Technology | Anode material of nano-silicon having multilayer-graphene as carrier and coated with silicon suboxide and with amorphous carbon layer and method for fabricating the same |
| GB202014224D0 (en) * | 2019-06-06 | 2020-10-28 | Univ Qingdao Technology | Graphene oxide-tetraethyl orthosilicate/silane composite gel material |
| CN113462166A (en) * | 2021-07-08 | 2021-10-01 | 湖北祥源新材科技股份有限公司 | Organic silicon foamed sheet for electronic products and preparation method thereof |
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