CN115926243B - Flame-retardant heat-insulating foam aerogel and preparation method thereof - Google Patents
Flame-retardant heat-insulating foam aerogel and preparation method thereof Download PDFInfo
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- CN115926243B CN115926243B CN202210989251.1A CN202210989251A CN115926243B CN 115926243 B CN115926243 B CN 115926243B CN 202210989251 A CN202210989251 A CN 202210989251A CN 115926243 B CN115926243 B CN 115926243B
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- 239000006260 foam Substances 0.000 title claims abstract description 57
- 239000004964 aerogel Substances 0.000 title claims abstract description 38
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract description 14
- 239000003063 flame retardant Substances 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000002904 solvent Substances 0.000 claims abstract description 33
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 31
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 23
- 239000010703 silicon Substances 0.000 claims abstract description 23
- 229920005830 Polyurethane Foam Polymers 0.000 claims abstract description 22
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000004088 foaming agent Substances 0.000 claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 239000011863 silicon-based powder Substances 0.000 claims abstract description 8
- 229920002943 EPDM rubber Polymers 0.000 claims abstract description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 13
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 12
- 230000002378 acidificating effect Effects 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 10
- 238000005187 foaming Methods 0.000 claims description 9
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical group CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 9
- 238000002791 soaking Methods 0.000 claims description 9
- 239000004305 biphenyl Substances 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 8
- 239000000377 silicon dioxide Substances 0.000 claims description 8
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 7
- 239000012467 final product Substances 0.000 claims 1
- 238000009413 insulation Methods 0.000 abstract description 11
- 239000011148 porous material Substances 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 5
- 239000000499 gel Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 239000013078 crystal Substances 0.000 description 4
- 238000000352 supercritical drying Methods 0.000 description 4
- 239000002937 thermal insulation foam Substances 0.000 description 4
- 150000001335 aliphatic alkanes Chemical class 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000007654 immersion Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 239000012744 reinforcing agent Substances 0.000 description 2
- 239000000741 silica gel Substances 0.000 description 2
- 229910002027 silica gel Inorganic materials 0.000 description 2
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 1
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 description 1
- 239000004156 Azodicarbonamide Substances 0.000 description 1
- MWRWFPQBGSZWNV-UHFFFAOYSA-N Dinitrosopentamethylenetetramine Chemical compound C1N2CN(N=O)CN1CN(N=O)C2 MWRWFPQBGSZWNV-UHFFFAOYSA-N 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 235000012538 ammonium bicarbonate Nutrition 0.000 description 1
- 239000001099 ammonium carbonate Substances 0.000 description 1
- XOZUGNYVDXMRKW-AATRIKPKSA-N azodicarbonamide Chemical compound NC(=O)\N=N\C(N)=O XOZUGNYVDXMRKW-AATRIKPKSA-N 0.000 description 1
- 235000019399 azodicarbonamide Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003139 buffering effect Effects 0.000 description 1
- 239000000701 coagulant Substances 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000006261 foam material Substances 0.000 description 1
- 238000001879 gelation Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002106 nanomesh Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 239000004945 silicone rubber Substances 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Silicon Compounds (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
Abstract
The invention discloses a flame-retardant heat-insulating foam aerogel and a preparation method thereof, wherein the foam aerogel comprises the following raw materials: the porous foam is selected from one of porous PU foam, porous PE foam, porous EPDM foam and porous EVA foam, and the silicon-containing solvent comprises the following components in parts by mass: 5-10 parts of silicon powder, 5-15 parts of silica sol, 15-30 parts of solvent and 1-5 parts of foaming agent. The foam aerogel prepared by the invention has excellent heat insulation performance and can be applied to precise modern instruments and equipment such as notebooks and the like.
Description
Technical Field
The invention relates to the technical field of G03F, in particular to a flame-retardant heat-insulating foam aerogel and a preparation method thereof.
Background
Along with the development of technology, consumer electronic products are continuously intelligent, light and thin, which means that the requirements on heat conduction, heat insulation, soaking and the like of the electronic products are also higher and higher, and especially the requirements on heat insulation, buffering and flame retardance of materials are higher and higher.
CN109651821a discloses an organosilicon foam, which comprises resin, cross-linking agent, reinforcing agent, flame retardant and other components, and the obtained organosilicon foam has the properties of high toughness, high ductility, high elasticity and the like, and has good flame retardance, but has poor heat insulation performance, and the preparation raw materials and the preparation process are complex.
CN107141808A discloses a heat-conducting and temperature-resistant foam material, and the preparation raw materials comprise components such as silicone rubber, silicone resin, reinforcing agent and the like, and although the heat-conducting property is good, the flame retardance is poor, and the preparation process is complex.
Disclosure of Invention
In view of the above problems, in one aspect, the present invention provides a flame retardant and heat insulation foam aerogel, wherein the foam aerogel comprises the following raw materials: open-pore sponge, silicon-containing solvent, volume ratio is 1: (5-10).
In one embodiment, the open-cell foam is selected from one of open-cell PU foam, open-cell PE foam, open-cell EPDM foam, and open-cell EVA foam.
Preferably, the open-cell foam is selected from open-cell PU foam.
Preferably, the open-cell PU foam has PPI of 30-60.
Further preferred, the open-celled PU foam has a PPI of 50.
The open-cell PU foam is commercially available.
The inventor creatively discovers in the experimental process that the foam aerogel prepared by adopting open-cell PU foam, especially the foam aerogel prepared by PPI of 30-60 has good toughness, good softness and good heat insulation effect. The inventors believe that the possible reasons are: the porosity of the open-pore sponge has an important influence on the immersion speed of the solvent, when the PPI of the open-pore sponge is smaller than 30, the porosity is lower, the resistance in the immersion process of the solvent is large, the immersion speed is lower, and part of functional suspended substances in the solvent cannot be uniformly distributed in the foam, and the foam is unevenly foamed, so that the final heat insulation effect of the foam air coagulant is influenced; when the PPI is more than 60, the hardness of the inside of the sponge is insufficient in the foaming process, so that the inside of the sponge is easily damaged, the toughness of the foam aerogel is affected, and the mechanical strength is poor.
In one embodiment, the silicon-containing solvent comprises, in parts by mass: 5-10 parts of silicon powder, 5-15 parts of silica sol, 15-30 parts of solvent and 1-5 parts of foaming agent.
Preferably, the silicon-containing solvent comprises, in parts by mass: 7 parts of silicon powder, 10 parts of silica sol, 20 parts of solvent and 3.5 parts of foaming agent.
In one embodiment, the silicon powder is ultrafine silicon powder.
Preferably, the average particle size of the superfine silica powder is 1-50 μm.
Further preferably, the ultrafine silica powder has an average particle diameter of 10. Mu.m.
The superfine silicon micropowder is purchased from Jiangsu long crystal novel material limited company, the model is 1250, and the particle size is 10 mu m.
In one embodiment, the silica sol is an acidic silica sol.
Preferably, the average particle size of the silicon dioxide in the acidic silica sol is 30-70nm.
The acidic silica sol is purchased from Kaohan silicon products Co., ltd in Linyi, and the model is KHAS-5030.
In one embodiment, the solvent is selected from one of water, alcohols, alkanes.
Preferably, the solvent is selected from alkanes.
Further preferably, the solvent is n-hexane.
In one embodiment, the foaming agent is selected from one or more of sodium bicarbonate, ammonium bicarbonate, dinitroso pentamethylene tetramine, p-diphenyl sulfonyl hydrazide, azodicarbonamide.
Preferably, the foaming agent is selected from p-diphenyl sulfonyl hydrazine and sodium bicarbonate, and the mass ratio is (2-5): 1.
further preferably, the mass ratio of the p-diphenyl sulfonyl hydrazine to the sodium bicarbonate is 3:1.
the invention also provides a preparation method of the foam aerogel, which comprises the following preparation steps:
s1: soaking in a solvent;
s2: secondary foaming;
s3: and (5) drying the gel to obtain the product.
In one embodiment, the step S1 specifically includes: the PU foam is soaked in the silicon-containing solvent for 10-30min at 20-35 ℃.
Preferably, the soaking time is 15min, and the soaking temperature is 25 ℃.
In one embodiment, the step S2 specifically includes: the pH of the solution was adjusted to 4-6 with sulfuric acid and the temperature was controlled at 110-140 ℃.
Preferably, the sulfuric acid adjusts the pH of the solution to 5 and the temperature to 125 ℃.
In one embodiment, the step S3 specifically includes: and (5) performing aerogel drying by adopting a supercritical drying mode.
The foam aerogel obtained by secondarily foaming and modifying the open-pore foam has strong flame retardant capability and excellent heat insulation performance. The reason the inventors consider is: in the secondary foaming process, the pH is regulated to 4-6, the gelation process of the acidic silica gel is aggravated, the acidic silica gel is quickly coagulated in the foam, superfine silica powder is stably wrapped in the gel, the flame retardance of the foam is improved, the foaming agent generates gas at the temperature of 110-140 ℃, alkane is evaporated, a large number of micropore structures are generated in the aerogel, a nano-mesh structure is formed in the open-pore foam after drying, the specific surface area is large, and the heat insulation performance and the flame retardance are greatly improved.
The beneficial effects are that:
1. the foam aerogel prepared by adopting the open-pore foam and selecting the PPI of 30-60 has good toughness, good softness and good heat insulation effect.
2. The foam aerogel obtained by secondarily foaming and modifying the open-pore foam has strong flame retardant capability and excellent heat insulation performance.
3. The foam aerogel prepared by the invention has excellent heat insulation performance and can be applied to precise modern instruments and equipment such as notebooks and the like.
Detailed Description
Example 1
In one aspect, this embodiment 1 provides a flame retardant and heat insulation foam aerogel, wherein the foam aerogel is prepared from the following raw materials: the volume ratio of the open-cell PU foam to the silicon-containing solvent is 1:5.
the open-cell PU foam has PPI of 30.
The open-cell PU foam is commercially available.
The silicon-containing solvent comprises the following components in parts by mass: 5 parts of superfine silica powder, 15 parts of acidic silica sol, 30 parts of normal hexane and 5 parts of foaming agent.
The foaming agent is p-diphenyl sulfonyl hydrazine and sodium bicarbonate, and the mass ratio is 2:1.
the superfine silicon micropowder is purchased from Jiangsu long crystal novel material limited company, the model is 1250, and the particle size is 10 mu m.
The acidic silica sol is purchased from Kaohan silicon products Co., ltd in Linyi, and the model is KHAS-5030.
In another aspect, the embodiment 1 provides a method for preparing the foam aerogel, which comprises the following preparation steps:
s1: soaking in a solvent: the PU foam is soaked in a siliceous solvent for 10min at 35 ℃.
S2: secondary foaming: the solution was adjusted to pH 4 using sulfuric acid and the temperature was controlled at 140 ℃.
S3: gel drying: and (5) performing aerogel drying by adopting a supercritical drying mode to obtain the product.
Example 2
In one aspect, this embodiment 2 provides a flame retardant and heat insulation foam aerogel, wherein the foam aerogel is prepared from the following raw materials: the volume ratio of the open-cell PU foam to the silicon-containing solvent is 1:10.
the open-cell PU foam has PPI of 60.
The open-cell PU foam is commercially available.
The silicon-containing solvent comprises the following components in parts by mass: 10 parts of superfine silica powder, 5 parts of acidic silica sol, 15 parts of normal hexane and 1 part of foaming agent.
The foaming agent is p-diphenyl sulfonyl hydrazine and sodium bicarbonate, and the mass ratio is 5:1.
the superfine silicon micropowder is purchased from Jiangsu long crystal novel material limited company, the model is 1250, and the particle size is 10 mu m.
The acidic silica sol is purchased from Kaohan silicon products Co., ltd in Linyi, and the model is KHAS-5030.
In another aspect, the embodiment 2 provides a method for preparing the foam aerogel, which comprises the following preparation steps:
s1: soaking in a solvent: the PU foam is soaked in a siliceous solvent for 30min at 20 ℃.
S2: secondary foaming: the solution was adjusted to pH 6 using sulfuric acid and the temperature was controlled at 110 ℃.
S3: gel drying: and (5) performing aerogel drying by adopting a supercritical drying mode to obtain the product.
Example 3
In one aspect, this embodiment 3 provides a flame retardant and heat insulation foam aerogel, wherein the foam aerogel is prepared from the following raw materials: the volume ratio of the open-cell PU foam to the silicon-containing solvent is 1:7.
the open-cell PU foam has PPI of 50.
The open-cell PU foam is commercially available.
The silicon-containing solvent comprises the following components in parts by mass: 7 parts of superfine silica powder, 10 parts of acidic silica sol, 20 parts of normal hexane and 3.5 parts of foaming agent.
The foaming agent is p-diphenyl sulfonyl hydrazine oxide and sodium bicarbonate, and the mass ratio is 3:1.
the superfine silicon micropowder is purchased from Jiangsu long crystal novel material limited company, the model is 1250, and the particle size is 10 mu m.
The acidic silica sol is purchased from Kaohan silicon products Co., ltd in Linyi, and the model is KHAS-5030.
In another aspect, this embodiment 3 provides a method for preparing the foam aerogel, which comprises the following steps:
s1: soaking in a solvent: the PU foam is soaked in a siliceous solvent for 15min at 25 ℃.
S2: secondary foaming: the solution was adjusted to pH 5 using sulfuric acid and the temperature was controlled at 125 ℃.
S3: gel drying: and (5) performing aerogel drying by adopting a supercritical drying mode to obtain the product.
Comparative example 1
The open cell foam was open cell PU foam, PPI 80, and the remainder was as in example 3.
Comparative example 2
The procedure of example 3 was repeated except that ethanol was used instead of n-hexane.
Comparative example 3
The foaming agent is p-diphenyl sulfonyl hydrazine and sodium bicarbonate, and the mass ratio is 10:1 and the rest are the same as in example 3.
Performance test:
1. flame retardant performance test: the foam aerogels of examples 1-3 and comparative examples 1-3 were tested for flame retardant properties using a vertical flame box, and were rated as acceptable for UL 94HBF and unacceptable for UL 94HBF, and the results are shown in the following table.
2. Thermal conductivity coefficient: the foam aerogels of examples 1 to 3 and comparative examples 1 to 3 were subjected to thermal conductivity measurement using a thermal conductivity tester, and the results are shown in the following table.
Claims (5)
1. A preparation method of flame-retardant heat-insulating foam aerogel is characterized in that,
at least comprises the following preparation steps:
s1: soaking in a silicon-containing solvent;
s2: secondary foaming;
s3: drying the gel to obtain the final product;
the step S1 specifically comprises the following steps: soaking the open-cell foam in a silicon-containing solvent;
the step S2 specifically comprises the following steps: adjusting the pH of the solution to 4-6 by sulfuric acid, and controlling the temperature to 110-140 ℃;
the foam aerogel is prepared from the following raw materials: the volume ratio of the open-cell foam to the silicon-containing solvent is 1: (5-10);
the open-cell foam is selected from one of open-cell PU foam, open-cell PE foam, open-cell EPDM foam and open-cell EVA foam;
the open-cell foam has PPI of 30-60;
the silicon-containing solvent comprises the following components in parts by mass: 5-10 parts of silicon powder, 5-15 parts of silica sol, 15-30 parts of solvent and 1-5 parts of foaming agent;
the foaming agent is selected from 4,4' -diphenyl sulfonyl hydrazine and sodium bicarbonate, and the mass ratio is (2-5): 1, a step of;
the solvent is n-hexane.
2. The method for preparing foam aerogel according to claim 1, wherein the silicon powder is ultrafine silicon powder.
3. The method for preparing foam aerogel according to claim 2, wherein the average particle size of the ultrafine silica powder is 1-50 μm.
4. The method of claim 1, wherein the silica sol is an acidic silica sol.
5. A foam aerogel prepared by the method of preparing a foam aerogel according to any one of claims 1 to 4.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210989251.1A CN115926243B (en) | 2022-08-17 | 2022-08-17 | Flame-retardant heat-insulating foam aerogel and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210989251.1A CN115926243B (en) | 2022-08-17 | 2022-08-17 | Flame-retardant heat-insulating foam aerogel and preparation method thereof |
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| Publication Number | Publication Date |
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| CN115926243A CN115926243A (en) | 2023-04-07 |
| CN115926243B true CN115926243B (en) | 2024-04-05 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102516770A (en) * | 2011-12-13 | 2012-06-27 | 西北橡胶塑料研究设计院 | Environmentally-friendly flame-retardant silicone rubber sponge and preparation method thereof |
| CN105585725A (en) * | 2015-11-13 | 2016-05-18 | 杭州师范大学 | Preparation method and application of heat insulating and inflaming retarding foam material and |
| CN110918008A (en) * | 2019-11-28 | 2020-03-27 | 航天海鹰(镇江)特种材料有限公司 | Foam-reinforced SiO2-TiO2Preparation method of composite aerogel |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007146945A2 (en) * | 2006-06-12 | 2007-12-21 | Aspen Aerogels, Inc. | Aerogel-foam composites |
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- 2022-08-17 CN CN202210989251.1A patent/CN115926243B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102516770A (en) * | 2011-12-13 | 2012-06-27 | 西北橡胶塑料研究设计院 | Environmentally-friendly flame-retardant silicone rubber sponge and preparation method thereof |
| CN105585725A (en) * | 2015-11-13 | 2016-05-18 | 杭州师范大学 | Preparation method and application of heat insulating and inflaming retarding foam material and |
| CN110918008A (en) * | 2019-11-28 | 2020-03-27 | 航天海鹰(镇江)特种材料有限公司 | Foam-reinforced SiO2-TiO2Preparation method of composite aerogel |
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