CN109749447B - Thermal decomposition material and preparation method thereof - Google Patents
Thermal decomposition material and preparation method thereof Download PDFInfo
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- CN109749447B CN109749447B CN201711067824.0A CN201711067824A CN109749447B CN 109749447 B CN109749447 B CN 109749447B CN 201711067824 A CN201711067824 A CN 201711067824A CN 109749447 B CN109749447 B CN 109749447B
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Abstract
The invention provides a thermal decomposition material and a preparation method thereof, the thermal decomposition material is prepared by compounding a thermal decomposition filler microcapsule, high-temperature resistant chopped fibers, a modified functional material, a high-temperature resistant silicon rubber adhesive and the like, and the convection heat transfer is greatly reduced, so that the thermal decomposition material has low heat conductivity, and the room-temperature heat conductivity coefficient is less than or equal to 0.085W/m.K; excellent heat absorption performance (the pyrolysis enthalpy value is more than or equal to 900J/g) and high temperature resistance (can resist the high temperature of 400 ℃).
Description
Technical Field
The invention relates to a thermal decomposition material and a preparation method thereof, belonging to the technical field of functional composite materials.
Background
With the development of the technology, a large number of equipment parts are arranged on a ship, and a large amount of heat is generated during working, so that the equipment cannot work normally, and therefore certain protection measures must be taken for the equipment parts.
At present, equipment parts are generally coated by adopting flexible cotton felts directly, but the method has limited effect and is limited by the structural size of the equipment parts, local parts are difficult to coat, the compactness is difficult to control, and the method is limited by the specification of the flexible cotton felts, so that the flexible cotton felts cannot meet the use requirements of the equipment parts.
Disclosure of Invention
The following presents a simplified summary of the invention in order to provide a basic understanding of some aspects of the invention. It should be understood that this summary is not an exhaustive overview of the invention. It is not intended to determine the key or critical elements of the present invention, nor is it intended to limit the scope of the present invention. Its sole purpose is to present some concepts in a simplified form as a prelude to the more detailed description that is discussed later.
In order to solve the problems, the invention provides a thermal decomposition material and a preparation method thereof, and the thermal decomposition material has the advantages of excellent heat insulation effect, capability of being used at 400 ℃, good shape following performance and simple preparation process.
The technical solution of the invention is as follows:
on one hand, the invention provides a thermal decomposition material, which comprises the following components in percentage by mass:
preferably, in the above mixture ratio, on the basis of the above content range, the higher the content of the thermally decomposed filler microcapsule is, the better the heat absorption effect of the thermally decomposed material is, and the higher the content of the modified functional material is, the better the heat insulation effect of the product is.
Further, the room temperature curing silicone rubber adhesive is a vulcanizable silicone rubber adhesive, and is selected from a single-component silicone rubber adhesive or a double-component silicone rubber adhesive; preferably a two-component silicone rubber adhesive;
preferably, the temperature-resistant grade of the room-temperature curing silicone rubber adhesive is 400 ℃ or above.
Furthermore, the thermal decomposition filler microcapsule is prepared from a thermal decomposition filler, the thermal decomposition filler is one or a mixture of any of magnesium hydroxide, aluminum hydroxide, ferric hydroxide and manganese hydroxide, but the thermal decomposition filler is not limited to magnesium hydroxide, aluminum hydroxide, ferric hydroxide and manganese hydroxide, and the thermal decomposition filler can absorb heat;
further, the chopped fibers are preferably high-temperature resistant chopped fibers, and specifically comprise: the fiber is composed of various chopped fibers or a mixture thereof with the temperature resistance grade of 600 ℃ or above, and can be selected from one or more of glass fiber, high silica fiber, quartz fiber and basalt rock wool fiber; other types of fibers may be used as long as they provide high temperature resistance and reinforcement;
preferably, the diameter of the chopped fiber is 1-15 μm, and the length of the chopped fiber is 1-10 mm.
If the range is larger than the upper limit value, the chopped fibers are not easy to fill and operate, and the reinforcing effect is influenced; if the range is less than the lower limit, the cost of the thermal decomposition material increases and the reinforcing effect is not significant.
Further, the diluent adopts an organic solvent;
preferably, the organic solvent may be selected from one or a combination of two or more of the following, gasoline, cyclohexane, pentane, heptane and the like, preferably cyclohexane, and other kinds of organic solvents may be selected as long as the whole system is not adversely affected;
further, the modified functional material is obtained by modifying functional material hollow microspheres or functional material aerogel through a modifier and the diluent;
preferably, the functional material cenospheres is one or a mixture of any more of aluminum silicate cenospheres, borate cenospheres, aluminum oxide cenospheres, silicon dioxide cenospheres, carbon cenospheres, ceramic cenospheres, zirconium oxide cenospheres, fly ash floating beads, polystyrene cenospheres, urea formaldehyde cenospheres or phenolic aldehyde cenospheres, but not limited thereto, as long as the function of preventing heat flow from transferring to the interior of the equipment can be achieved;
preferably, the particle size of the cenospheres is 0.1-500 μm, preferably 1-100 μm;
if be greater than the upper limit scope, difficult packing is closely knit, and thermal-insulated effect is not good, if be less than the lower limit scope, easily reunite in the operation process, difficult even stirring, the thermal-insulated effect of product also all can receive certain influence.
Preferably, the functional material aerogel is one or a mixture of any more of silica aerogel, alumina aerogel or zirconia aerogel;
preferably, the modifier is preferably silanes, aluminates or titanates, wherein the silanes are preferably one or more of KH550, KH560, KH570, KH792, KH580, DL602, DL171, KH-845-4, YDH553, YDH660, YDH791, YDH911, YDH910, YDH550, YDH320, YDH703, YDH704, YDH101, YDH102, YDH105, YDH109, YDH201, YDH401, KH551, A151 and A171;
the titanate is preferably one or more of TG-2 and TG-38S, TG-27;
the aluminate is preferably one or more of TG-10TG-200S, TG-5 and TG-4.
On the other hand, the invention also provides a preparation method of the thermal decomposition material, which is realized by the following steps:
firstly, preparing thermal decomposition filler microcapsules;
a1.1, mechanically crushing the thermal decomposition filler;
in this step, the thermally decomposable filler needs to be mechanically pulverized to 600 μm or less or to a desired particle size range, and the specific particle size is not particularly limited, and is, for example, 600 μm, 500 μm, 400 μm, 300 μm, 200 μm, 100 μm, 50 μm, 20 μm, 10 μm or 5 μm, etc., preferably less than 100 μm, more preferably 20 to 50 μm;
if the size of the thermal decomposition filler is too large, uniform coating or no coating is not easy to realize, and the subsequent use requirement is influenced; if the size is too small, the thickness of the coated microcapsule shell is easy to be too thick, and the heat absorption effect is influenced;
a1.2, adding the crushed thermal decomposition filler into toluene or xylene, and uniformly stirring to obtain a toluene or xylene system;
in the step, the mass percentage of the thermal decomposition filler in a dispersion medium (toluene or xylene) is generally 5-80%, and preferably 20-30%;
a1.3, adding a certain amount of maleic anhydride into the toluene or xylene system, and adding a certain amount of styrene or divinylbenzene after complete dissolution;
the step needs to be carried out in an oxygen-free environment, for example, a mode of introducing inert gas can be adopted, and the inert gas can be nitrogen;
in the step, the maleic anhydride is completely dissolved by adopting a mechanical stirring mode, wherein the stirring speed is 100-500 rpm during mechanical stirring.
In the step, the mass percentage of maleic anhydride in the thermal decomposition filler is 1-50%, and the mass percentage of styrene or divinyl benzene in the thermal decomposition filler is 1-50%; the proportion of the total monomer (maleic anhydride, styrene or divinylbenzene) to the thermally decomposable filler is preferably from 20% to 30%;
wherein, the mass percentage of the total monomer (maleic anhydride, styrene or divinyl benzene) in the thermal decomposition filler has important influence on the core-shell proportion of the microcapsule, when the total monomer content is low, the core material content of the microcapsule is high, the product absorbs more heat, but the leaching rate of the microcapsule is higher; on the contrary, when the total monomer content is high, the core material content of the microcapsule is low, the heat absorption of the product is less, but the leaching rate of the microcapsule is low, and the coating and packaging effect is good; therefore, in the practical application process, the proportion relation between the total monomer amount and the thermal decomposition filler is determined according to the requirement and the heat absorption amount and the leaching rate, and the proportion relation is preferably 20-30 percent generally;
a1.4, on the basis of the step A1.3, further adding a certain amount of azodiisobutyronitrile for reaction, and performing suction filtration after complete reaction to obtain the thermally decomposed filler microcapsule;
in the step, the mass percentage of the azobisisobutyronitrile in the thermal decomposition filler is 0.1-4%, preferably 0.5-3%;
the reaction time is also greatly influenced by the addition amount of the azobisisobutyronitrile, the reaction time can be properly reduced when the addition amount of the azobisisobutyronitrile is large, and the reaction time needs to be properly prolonged when the addition amount is small;
in the step, the temperature of a reaction system is 60-150 ℃, the reaction time is 10-100 hours, the reaction time is prolonged when the reaction temperature is lower, otherwise, the reaction time is short when the reaction temperature is higher, and the reaction temperature in the step is lower than the melting point of the thermal decomposition filler, so that the thermal decomposition filler is in a solid particle state in the reaction process;
secondly, stirring the functional material with a proper amount of diluent and modifier to uniformly mix the functional material with the diluent and the modifier so as to complete the surface modification of the functional material;
in the step, the addition amount of the diluent is preferably adjusted to be 5-200% of that of the functional material according to the actual situation, and the added functional material is more easily and uniformly dispersed after the diluent is added;
further, in the step, the mass ratio of the modifier to the diluent is 1: 1000-1: 5;
if the amount of the modifier is too large, the modifier is easy to remain in the thermally decomposed filler, which affects the use requirements, and if the amount of the modifier is too small, the modification of the functional material is affected, which affects the interfacial bonding between the functional material and other materials;
step three, uniformly mixing the room temperature curing silicone rubber adhesive with a proper amount of diluent;
in the step, the diluent is added to ensure that the thermal decomposition filler microcapsule, the high-temperature resistant chopped fiber and the functional material are more easily and uniformly dispersed in the room-temperature curing silicone rubber adhesive component when the thermal decomposition filler microcapsule, the high-temperature resistant chopped fiber and the functional material are added subsequently, the addition amount is adjusted according to the actual situation, and is preferably 5-200% of the room-temperature curing silicone rubber adhesive component;
fourthly, sequentially adding the thermal decomposition filler microcapsule, the high-temperature resistant chopped fiber and the modified functional material into the diluted room-temperature curing silicone rubber adhesive component according to the proportion, and uniformly stirring;
and fifthly, molding, curing, demolding and post-treating the mixture obtained in the fourth step.
In this step, the molding process may be performed by any one of other molding methods such as compression molding, injection molding, extrusion molding, calendering molding, etc.;
in the step, the mixed material matrix obtained by molding is cured for 8 to 168 hours at the temperature of 60 +/-5 ℃.
Further, the post-processing method comprises the following steps: and standing the demoulded product at 80 +/-5 ℃ for 12-100 h.
Compared with the prior art, the invention has the beneficial effects that:
the invention is prepared by compounding thermally decomposed filler microcapsules, high-temperature resistant chopped fibers, modified functional materials, high-temperature resistant silicon rubber adhesives and the like, wherein the thermally decomposed filler microcapsules are used for replacing the thermally decomposed filler, and the design principle is as follows: if the thermal decomposition filler is directly adopted, the thermal decomposition filler is heated to decompose, and a certain amount of micromolecules are released, so that the thermal decomposition material is deformed, and the use is influenced, therefore, the invention adopts a certain coating means to form the microcapsule; the release of small molecules can be slowly released after the microcapsules are encapsulated, so that the shape of the thermal decomposition material is ensured; in addition, the thermal decomposition filler microcapsule can slowly decompose and absorb heat emitted by equipment parts when being heated, and meanwhile, the modified functional material is adopted to prevent heat flow from further transmitting to the interior of the equipment, further, the high-temperature resistant chopped fibers are added in an auxiliary mode to provide high-temperature resistance and a reinforcing effect, and the high-temperature resistant silicon rubber adhesive is a room-temperature curing adhesive which can be used at the temperature of 400 ℃ or higher and is adopted to provide high-temperature resistance and an adhesive effect. The invention has the following advantages:
(1) according to the invention, by adding a certain proportion of the thermal decomposition filler microcapsule and the modified functional material for synergistic cooperation, the convection heat transfer is greatly reduced, so that the thermal decomposition material has low thermal conductivity, and the room temperature thermal conductivity is less than or equal to 0.085W/m.K; excellent heat absorption performance (the pyrolysis enthalpy value is more than or equal to 900J/g) and high temperature resistance (can resist the high temperature of 400 ℃).
(2) The invention fills a large amount of chopped fibers, is bonded by the silicon rubber adhesive, and is modified by the silane coupling agent and the like, and the prepared silicon rubber foam has the characteristics of high strength, small deformation and the like, and meets most of requirements on the mechanical property of the heat-insulating material.
(3) The method provided by the invention has simple preparation process and high encapsulation rate of the thermal decomposition filler, and the microcapsules prepared by other methods need melting and emulsifying processes of the thermal decomposition filler, and the proportion of each component and each process parameter must be strictly controlled to ensure the stability of the emulsion, so the process is more complex.
(4) The invention has the advantages of simple process, simple and convenient operation, good shape following property, strong practicability and the like, and can meet the requirements of aviation, aerospace, precise instruments, equipment parts, civil industry and the like, thereby having wide application prospect.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a flow chart showing one embodiment of a method for producing a thermally decomposable material provided by the present invention;
Detailed Description
Specific embodiments of the present invention will be described in detail below with reference to the accompanying drawings.
Example 1
Referring to fig. 1, the preparation method of the thermal decomposition material provided in this example is as follows:
firstly, preparing thermal decomposition filler microcapsules;
a1.1, mechanically crushing magnesium hydroxide to 50 μm;
a1.2, adding the crushed magnesium hydroxide into xylene, and mechanically and uniformly stirring to obtain a xylene system; the mass percentage of the magnesium hydroxide in the dimethylbenzene is 25 percent.
A1.3, adding a certain amount of maleic anhydride into a xylene system, mechanically stirring until the maleic anhydride is completely dissolved, and introducing nitrogen to remove oxygen; and after complete dissolution, adding a certain amount of styrene, and continuously introducing nitrogen, wherein the stirring speed is 100-500 rpm during mechanical stirring.
The mass percentage of maleic anhydride in the magnesium hydroxide is 15%, and the mass percentage of styrene in the magnesium hydroxide is 10%.
A1.4, adding a certain amount of azobisisobutyronitrile into a xylene system, and reacting at 85 ℃ for 60 hours, wherein the mass percentage of the azobisisobutyronitrile in the magnesium hydroxide is 2%.
And A1.5, carrying out suction filtration to obtain the microcapsule of the thermal decomposition filler.
Secondly, soaking the phenolic aldehyde hollow microspheres in a mixed solvent of KH550 and cyclohexane for modification; the functional material, the modifier and the diluent are in the following mass ratio: phenolic aldehyde hollow microspheres: KH 550: cyclohexane 100: 15: 150.
and step three, uniformly mixing the double-component KH-CL-RTV silicon rubber adhesive with cyclohexane, wherein the mass ratio of the KH-CL-RTV silicon rubber adhesive is as follows: KH-CL-RTV curing agent: cyclohexane is 100:6: 150.
Fourthly, adding magnesium hydroxide microcapsules, short glass fibers and modified phenolic aldehyde hollow microspheres into the diluted KH-CL-RTV silicone rubber adhesive, and uniformly stirring; the mass ratio is as follows: KH-CL-RTV silicone rubber: magnesium hydroxide microcapsules: short glass fiber: modified phenolic cenospheres are 100: 120: 35: 35.
and fifthly, filling the mixture obtained in the fourth step into a corresponding mould for compression molding.
Sixthly, placing the formed mixed material matrix at 60 ℃ for 50 hours of curing.
And seventhly, demolding the material, and then standing the demolded material at 80 ℃ for 50 hours for post-treatment to obtain the thermal decomposition material prefabricated block.
A flat plate of a thermally decomposable material was prepared in accordance with the proportions of the thermally decomposable materials in examples, the length and width of the sample were 200mm, the thickness was 15mm, and the apparent density was 0.66g/cm3And carrying out performance test on the sample prepared by the method, wherein: enthalpy of pyrolysis: 920J/g (GB/T19466.3-2004); thermal conductivity at room temperature: 0.081W/m.K (GB/T10295-.
Examples 2 to 15
The raw materials and the preparation ratio thereof for preparing the thermal decomposition material microcapsules of examples 2 to 15 are shown in table 1; the thermal decomposition materials prepared in the examples 2-15 and the performance test thereof are shown in the table 2, and the other contents are the same as the example 1, wherein:
the thermal decomposition material prepared by the mixture ratio of the embodiment 2-15 is as follows: the length and width of the sample piece are both 200mm, the thickness is 15mm, and the apparent density: less than or equal to 0.66g/cm3The enthalpy of pyrolysis: not less than 900J/g; thermal conductivity at room temperature: less than or equal to 0.085W/m.K.
TABLE 1
TABLE 2
Features that are described and/or illustrated above with respect to one embodiment may be used in the same way or in a similar way in one or more other embodiments and/or in combination with or instead of the features of the other embodiments.
It should be emphasized that the term "comprises/comprising" when used herein, is taken to specify the presence of stated features, integers, steps or components but does not preclude the presence or addition of one or more other features, integers, steps, components or groups thereof.
The many features and advantages of these embodiments are apparent from the detailed specification, and thus, it is intended by the appended claims to cover all such features and advantages of these embodiments which fall within the true spirit and scope thereof. Further, since numerous modifications and changes will readily occur to those skilled in the art, it is not desired to limit the embodiments of the invention to the exact construction and operation illustrated and described, and accordingly, all suitable modifications and equivalents may be resorted to, falling within the scope thereof.
The invention has not been described in detail and is in part known to those of skill in the art.
Claims (9)
1. A preparation method of a thermal decomposition material is characterized by comprising the following steps:
firstly, preparing thermal decomposition filler microcapsules;
a1.1, mechanically crushing a thermal decomposition filler, wherein the thermal decomposition filler is one or a mixture of any more of magnesium hydroxide, aluminum hydroxide, ferric hydroxide and manganese hydroxide;
a1.2, adding the crushed thermal decomposition filler into toluene or xylene, and uniformly stirring to obtain a toluene or xylene system;
a1.3, adding a certain amount of maleic anhydride into the toluene or xylene system, and adding a certain amount of styrene or divinylbenzene after complete dissolution;
a1.4, on the basis of the step A1.3, further adding a certain amount of azodiisobutyronitrile for reaction, and performing suction filtration after complete reaction to obtain the thermally decomposed filler microcapsule;
wherein, the mass percentage of the maleic anhydride in the thermal decomposition filler is 1-50%, and the mass percentage of the styrene or the divinylbenzene in the thermal decomposition filler is 1-50%;
secondly, stirring the functional material hollow microspheres or the functional material aerogel with a proper amount of diluent and modifier to uniformly mix the functional material hollow microspheres or the functional material aerogel and the diluent and the modifier, and finishing the surface modification of the functional material to obtain a modified functional material;
step three, uniformly mixing the room temperature curing silicone rubber adhesive with a proper amount of diluent;
step four, adding the thermal decomposition filler microcapsule, the high-temperature resistant chopped fiber and the modified functional material into the room-temperature curing silicone rubber adhesive component obtained in the step three in sequence according to the proportion, and uniformly stirring;
and fifthly, molding, curing, demolding and post-treating the mixture obtained in the fourth step.
2. The method for producing a thermally decomposable material as claimed in claim 1, wherein: in the first step, the proportion of the total amount of maleic anhydride, styrene or divinyl benzene and the thermal decomposition filler is 20-30%.
3. The method for producing a thermally decomposable material as claimed in claim 1, wherein: in the second step, the mass ratio of the modifier to the diluent is 1: 1000-1: 5.
4. a thermal decomposition material prepared by the method according to any one of claims 1 to 3, wherein the thermal decomposition material comprises the following components in parts by mass:
room temperature curing silicone rubber adhesive 100
50-200 of thermally decomposed filler microcapsule
5 to 50% of short fibers
5-100 modified functional material
And an appropriate amount of diluent.
5. The thermally decomposable material as claimed in claim 4, wherein the chopped fibers are composed of chopped fibers having a temperature resistance level of 600 ℃ or higher or a mixture thereof.
6. The thermally decomposable material as claimed in claim 5, wherein the chopped fibers have a diameter of 1 to 15 μm and a length of 1 to 10 mm.
7. A thermally decomposable material as claimed in claim 4, wherein the diluent is an organic solvent.
8. The thermally decomposable material as claimed in claim 4, wherein the cenospheres have a particle size of 0.1 to 500 μm.
9. The thermally decomposable material as claimed in claim 8, wherein the cenospheres have a particle size of 1 μm to 100 μm.
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| CN103130454A (en) * | 2011-11-29 | 2013-06-05 | 航天特种材料及工艺技术研究所 | Low heat conductance silicon rubber foam material and manufacture method thereof |
| CN104072691A (en) * | 2014-06-26 | 2014-10-01 | 衢州市中通化工有限公司 | Preparation method for flame retardant expanded polystyrene with core-shell structure |
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| CN101531885A (en) * | 2009-04-17 | 2009-09-16 | 清华大学深圳研究生院 | Environment-friendly inflaming retarding smoke-inhibiting shaping phase-changing energy storage material and preparing method thereof |
| CN103130454A (en) * | 2011-11-29 | 2013-06-05 | 航天特种材料及工艺技术研究所 | Low heat conductance silicon rubber foam material and manufacture method thereof |
| CN104072691A (en) * | 2014-06-26 | 2014-10-01 | 衢州市中通化工有限公司 | Preparation method for flame retardant expanded polystyrene with core-shell structure |
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