CN113999528B - Polyorganosiloxane foam for heat preservation and insulation and preparation method thereof - Google Patents
Polyorganosiloxane foam for heat preservation and insulation and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a polyorganosiloxane foam for heat preservation and heat insulation and a preparation method thereof. The foam preparation raw materials comprise the following components in parts by mass: 100 parts of hydroxyl-terminated polysiloxane, 10-40 parts of vinyl polysiloxane, 10-20 parts of hydrogen-containing polysiloxane, 5-8 parts of MQ silicon resin, 2-10 parts of white carbon black, 2-10 parts of hollow glass beads, 1-5 parts of catalyst and 0.5-1 part of inhibitor; the vinyl polysiloxane and the hydrogen-containing silicone oil are subjected to a crosslinking reaction to provide mechanical properties for the foam silicone rubber, the hydroxyl-terminated polysiloxane and the hydrogen-containing silicone oil are subjected to a condensation dehydrogenation reaction to generate hydrogen to form micropores, the MQ silicone resin and the white carbon black are used as reinforcing agents to improve the mechanical properties, a large number of holes are provided by the unique closed-pore cavity structure of the hollow glass microsphere and the mechanical properties are enhanced at the same time, and the polyorganosiloxane foam has good mechanical properties and a low heat conductivity coefficient and can be applied to the field of heat preservation and insulation.
Description
Technical Field
The invention belongs to the field of high polymer materials, relates to the field of polyorganosiloxane foam materials, and particularly relates to polyorganosiloxane foam for heat preservation and heat insulation and a preparation method thereof.
Background
Polyorganosiloxane foam is a novel multifunctional material formed by adding a physical or chemical foaming agent or self-reaction foaming and the like during crosslinking of silicone rubber, combines the performance of silicone rubber materials with the characteristics of foam materials, and is also called silicone rubber foam. The polyorganosiloxane is a polymer with a main chain formed by silicon and oxygen atoms in an alternating way, two organic groups are usually connected on the silicon atoms, and compared with a common polymer material, the polyorganosiloxane has excellent performances of high and low temperature resistance, insulativity, weather resistance, chemical stability, biocompatibility and the like, and is widely applied to the fields of aerospace, buildings, electronics, flexible molds, automobiles, ships, biomedicine and the like. The foam material has the characteristics of light weight, heat insulation, sound absorption, shock absorption and the like due to the existence of a large number of gas micropores. The foam material can be divided into an open cell type, a closed cell type and a mixed type according to the types of micropores, the cells of the open cell foam material are mutually communicated and have excellent compressibility, heat preservation and heat insulation property, water stopping and water retaining property, sound absorption property and the like, the closed cell foam material has an independent cell structure, the inner cells are separated from the cells by wall membranes and are not mutually communicated, and the foam material has extremely excellent impact resistance, rebound, flexibility, sound insulation property, heat insulation property, waterproofness and the like.
At present, room temperature vulcanizing polyorganosiloxane foam is rapidly developed, and in the research on the influence factors of the generation of bubbles of dehydrogenated Room Temperature Vulcanizing (RTV) silicone rubber, although the obtained silicone rubber foam has good buffering performance and can be recycled, the rate is difficult to control when hydrogen is released, bubbles can be generated in a silicone rubber cured product, and more bubbles can influence the mechanical property of the silicone rubber. CN107434854A mixes hydrogen-containing organic polysiloxane, alkoxy silane and tris (pentafluorophenyl) borane uniformly at room temperature, and utilizes chemical foaming to prepare the organic silicon foam material. The patent C107434854A obtains the silicone rubber foam by utilizing the self-foaming reaction of the organic silicon, the method has strong practicability and is suitable for wide application, but the mechanical property of the obtained silicone rubber does not meet the requirement, and the cell structure is difficult to control. The patent CN107541070A utilizes thixotropic foam silicone rubber prepared by two components, the method reduces the cost and has good thixotropy, but the process is complex, and the heat insulation performance can not meet the industrial application. The open-cell liquid room-temperature vulcanized foam silicone rubber prepared in patent CN104312168A has the advantages of high open-cell rate, low density and the like, but the mechanical properties and heat insulation performance of the open-cell liquid room-temperature vulcanized foam silicone rubber hardly meet the requirements of heat insulation materials. The patent CN111234532A prepares the foaming flame-retardant liquid silicone rubber with excellent mechanical properties and good flame-retardant effect by using a small amount of flame-retardant additive, but the porosity density is too low, so that the thermal conductivity coefficient is too large, and the requirements of heat preservation and heat insulation cannot be met.
Currently, there are few reports of polyorganosiloxane foams for thermal insulation, especially room temperature vulcanized polyorganosiloxane foams for thermal insulation, and it can be seen from the above reported patents and documents that the currently applied room temperature vulcanized polyorganosiloxane foams have complicated process flow and high manufacturing cost, and when used for thermal insulation, mechanical properties, uniformity of micropores and thermal insulation cannot be combined, so that the application of polyorganosiloxane foams in thermal insulation is limited.
Therefore, it is very necessary to prepare a polyorganosiloxanecarbon foam having good mechanical properties, uniform pore size distribution and good thermal insulation properties.
Disclosure of Invention
The invention aims to solve the problems and the defects of the prior art and provides a polysiloxane foam for heat preservation and insulation and a preparation method thereof. The method has simple process and is suitable for popularization and application, and the prepared polysiloxane foam is mixed, has the performances of open-cell foam and closed-cell foam, has good compression performance, high flexibility, uniform pore distribution and low heat conductivity coefficient, and meets the application requirements of heat insulation materials.
The purpose of the invention is realized by at least one of the following technical solutions.
The invention provides a preparation method of polyorganosiloxane foam for heat preservation and heat insulation, which comprises the following steps: (1) Uniformly mixing n-butyl alcohol, a silane coupling agent and water to obtain a modified solution, then adding the hollow glass microspheres into the modified solution, uniformly stirring, filtering to obtain filter residues, and drying the filter residues to obtain modified hollow glass microspheres;
(2) Mixing hydroxyl-terminated polysiloxane, vinyl polysiloxane, white carbon black, the modified hollow glass microspheres in the step (1), MQ silicon resin, an inhibitor and hydrogen-containing polysiloxane, stirring, and performing ultrasonic treatment to obtain a mixed solution 1;
(3) Adding a catalyst into the mixed solution 1 obtained in the step (2), stirring to obtain a mixed solution 2, pouring the mixed solution 2 into a mold, and drying to obtain the polyorganosiloxane foam for heat preservation and insulation.
Furthermore, according to the mass portion,
further, the silane coupling agent in the step (1) is KH570; the mass ratio of the n-butanol to the silane coupling agent to the water is (5);
preferably, in the step (1), the mass ratio of the silane coupling agent to the water to the n-butanol is 5.
Further, the mass ratio of the hollow glass beads to the modification solution in the step (1) is 1.
Further, the density of the hollow glass microballoons in the step (1) is 0.18-0.22g/cm 3 The average particle size is 2-150 μm.
Further, the drying temperature in the step (1) is 120-140 ℃, and the drying time is 3-5 hours.
Preferably, the drying temperature in the step (1) is 120 ℃, and the drying time is 3 hours.
Further, the hydroxyl-terminated polysiloxane in the step (2) is alpha, omega-dihydroxy polysiloxane, and the viscosity of the alpha, omega-dihydroxy polysiloxane is 750-5000 mPa.S;
preferably, the hydroxyl-terminated polysiloxane of step (2) has a viscosity of 750 to 2000mPa · S.
Further, the vinyl polysiloxane in the step (2) is vinyl-terminated polydimethylsiloxane, and the viscosity of the vinyl-terminated polydimethylsiloxane is 500-5000mPa & S;
preferably, the viscosity of the vinyl polysiloxane of step (2) is 1000 to 3000 mPa.S;
further, the white carbon black in the step (2) is hydrophobic fumed silica, the particle size of the white carbon black is 10-30nm, and the specific surface area of the white carbon black is 120-140m 2 /g。
Preferably, the particle size of the white carbon black in the step (2) is 30nm, and the specific surface area of the white carbon black is 130m 2 /g。
Further, the hydrogenpolysiloxane in the step (2) is polymethylhydrosiloxane, and the hydrogen content of the hydrogenpolysiloxane is 1.58-1.62%; the ratio of MQ in the MQ resin in the step (2) is 0.8, the vinyl content is 1.5 percent, and the viscosity is 9000mPa & S; the inhibitor in the step (2) is 1-ethynyl-1-cyclohexanol.
Further, the catalyst in the step (3) is a complex of platinum ions and vinyl methyl siloxane, and the effective platinum content is 3000-5000PPM.
Preferably, the catalyst in the step (3) is a complex of platinum ions and vinyl methyl siloxane, and the effective platinum content is 3000PPM.
Further, the stirring treatment time of the step (2) is 40-60 minutes;
further, the ultrasonic treatment time in the step (2) is 15-20 minutes;
further, the stirring treatment time in the step (3) is 15-30 minutes;
further, the drying temperature in the step (3) is 150-160 ℃, and the drying time is 30-60 minutes.
Preferably, the drying temperature in the step (3) is 150 ℃, and the drying time is 30 minutes.
The invention provides the polyorganosiloxane foam for heat preservation and insulation prepared by the preparation method.
In the preparation method provided by the invention, vinyl polysiloxane and hydrogen-containing silicone oil are subjected to a crosslinking reaction to provide mechanical properties for foam silicone rubber, hydroxyl-terminated polysiloxane and hydrogen-containing silicone oil are subjected to a condensation dehydrogenation reaction to generate hydrogen to form micropores, MQ silicone resin and white carbon black are used as reinforcing agents to improve the mechanical properties, and the unique closed-cell cavity structure of the hollow glass microsphere provides a large number of holes and enhances the mechanical properties.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) In the preparation method provided by the invention, hydrogen-containing polysiloxane is selected as a cross-linking agent and a foaming agent, and simultaneously, the cross-linking reaction with vinyl polysiloxane and the condensation foaming reaction with hydroxyl-terminated polysiloxane occur, so that the proportion and the hydrogen content of the hydrogen-containing polysiloxane can directly influence the mechanical property, the density, the structure of foam cells and the heat conductivity coefficient of the polyorganosiloxane foam; with the increase of the proportion and the hydrogen content of the hydrogen-containing polysiloxane, the activity of the hydrogen-containing polysiloxane is increased, the reaction speed of foaming and crosslinking reaction is accelerated, the key of the comprehensive performance of the polyorganosiloxane foam lies in the matching degree of the two reactions, when the foaming reaction is faster than the crosslinking reaction, the reaction sizing material can not wrap the generated hydrogen at the initial stage, the fixing speed of the cell wall is slowed down, the phenomena of hole merging and hole breaking are increased, and a large-hole and through-hole structure is easier to form; when the foaming reaction is slower than the crosslinking reaction, the generated hydrogen is difficult to overflow in time and is fixed in the crosslinking network, so that the cell nucleus is difficult to grow, and uneven small holes and closed holes are easy to form, and the selection of the proportion and the hydrogen content of the hydrogenpolysiloxane is a key factor influencing the quality of the product. The invention selects the proportion and the hydrogen content of the hydrogen-containing polysiloxane, so that the prepared heat-insulating polysiloxane has the advantages of uniform foam holes, high compression modulus, low heat conductivity coefficient and the like;
(2) According to the preparation method provided by the invention, the hollow glass beads and the white carbon black are selected as fillers, the hollow glass beads are better compatible with the polyorganosiloxane after being modified, the hydrophobic fumed silica is a novel reinforcing filler, the combination of the hollow glass beads and the hydrophobic fumed silica is favorable for enhancing the mechanical property of the polyorganosiloxane, and the unique closed-cell cavity structure of the hollow glass beads can block heat conduction and heat convection, so that the heat preservation and heat insulation properties of the polyorganosiloxane are improved;
(3) In the preparation method provided by the invention, the polysiloxane foam is obtained by utilizing the special cavity structure of the air holes generated by the reaction of the hydrogen-containing polysiloxane and the hydroxyl-terminated polysiloxane and the hollow glass beads, and the proportion of the air holes generated by the hydrogen-containing polysiloxane and the hydroxyl-terminated polysiloxane is reasonably matched, so that the aperture and the type of the polysiloxane foam holes are controllable.
Detailed Description
The following examples are presented to further illustrate the practice of the invention, but the practice and protection of the invention is not limited thereto. It is noted that the following processes, if not described in particular detail, are all realizable or understandable by those skilled in the art with reference to the prior art. The reagents or apparatus used are not indicated to the manufacturer and are considered to be conventional products available by commercial purchase.
The parts by weight (mass) used in the following examples and comparative examples may be given by way of example in the form of grams, kilograms, etc., or may be any other amount commonly used in the art.
Example 1
A heat-insulating polyorganosiloxane foam comprises the following raw materials in parts by weight:
the preparation process comprises the following steps:
(1) Uniformly mixing n-butanol, KH570 and deionized water in a mass ratio of 5;
(2) Mixing hydroxyl-terminated polysiloxane, vinyl polysiloxane, white carbon black, the modified hollow glass microspheres in the step (1), MQ silicon resin, an inhibitor and hydrogen-containing polysiloxane, stirring for 60 minutes, and then carrying out ultrasonic treatment for 15 minutes to obtain a mixed solution 1;
(3) Adding a catalyst into the mixed solution 1 obtained in the step (2), stirring for 30 minutes to obtain a mixed solution 2, pouring the mixed solution 2 into a mold, and drying for 30 minutes at 150 ℃ to obtain the polyorganosiloxane foam for heat preservation and insulation, wherein the test performance of the product is shown in Table 1.
Example 2
A heat preservation and insulation polysiloxane foam comprises the following preparation raw materials in parts by weight:
the preparation method comprises the following specific steps:
(1) Uniformly mixing n-butanol, KH570 and deionized water in a mass ratio of 5;
(2) Mixing hydroxyl-terminated polysiloxane, vinyl polysiloxane, white carbon black, the modified hollow glass microspheres in the step (1), MQ silicon resin, an inhibitor and hydrogen-containing polysiloxane, stirring for 60 minutes, and then carrying out ultrasonic treatment for 15 minutes to obtain a mixed solution 1;
(3) Adding a catalyst into the mixed solution 1 obtained in the step (2), stirring for 30 minutes to obtain a mixed solution 2, pouring the mixed solution 2 into a mold, and drying at 150 ℃ for 60 minutes to obtain the polyorganosiloxane foam for heat preservation and insulation, wherein the test performance of the product is shown in Table 1.
Example 3
A heat-insulating polyorganosiloxane foam comprises the following raw materials in parts by weight:
the preparation process comprises the following steps:
(1) Uniformly mixing n-butanol, KH570 and deionized water in a mass ratio of 5;
(2) Mixing hydroxyl-terminated polysiloxane, vinyl polysiloxane, white carbon black, the modified hollow glass microspheres in the step (1), MQ silicon resin, an inhibitor and hydrogen-containing polysiloxane, stirring for 60 minutes, and then carrying out ultrasonic treatment for 15 minutes to obtain a mixed solution 1;
(3) Adding a catalyst into the mixed solution 1 obtained in the step (2), stirring for 30 minutes to obtain a mixed solution 2, pouring the mixed solution 2 into a mold, and drying for 30 minutes at 150 ℃ to obtain the polyorganosiloxane foam for heat preservation and insulation, wherein the test performance of the product is shown in Table 1.
Example 4
A heat preservation and insulation polysiloxane foam comprises the following preparation raw materials in parts by weight:
the preparation process comprises the following steps:
(1) Uniformly mixing n-butanol, KH570 and deionized water in a mass ratio of 5;
(2) Mixing hydroxyl-terminated polysiloxane, vinyl polysiloxane, white carbon black, the modified hollow glass microspheres in the step (1), MQ silicon resin, an inhibitor and hydrogen-containing polysiloxane, stirring for 45 minutes, and then carrying out ultrasonic treatment for 20 minutes to obtain a mixed solution 1;
(3) Adding a catalyst into the mixed solution 1 obtained in the step (2), stirring for 20 minutes to obtain a mixed solution 2, pouring the mixed solution 2 into a mold, and drying for 30 minutes at 160 ℃ to obtain the polyorganosiloxane foam for heat preservation and insulation, wherein the test performance of the product is shown in table 1.
Example 5
A heat-insulating polyorganosiloxane foam comprises the following raw materials in parts by weight:
the preparation process comprises the following steps:
(1) Uniformly mixing n-butyl alcohol, KH570 and deionized water in a mass ratio of 10;
(2) Mixing hydroxyl-terminated polysiloxane, vinyl polysiloxane, white carbon black, the modified hollow glass microspheres in the step (1), MQ silicon resin, an inhibitor and hydrogen-containing polysiloxane, stirring for 45 minutes, and then carrying out ultrasonic treatment for 20 minutes to obtain a mixed solution 1;
(3) Adding a catalyst into the mixed solution 1 obtained in the step (2), stirring for 30 minutes to obtain a mixed solution 2, pouring the mixed solution 2 into a mold, and drying at 155 ℃ for 40 minutes to obtain the polyorganosiloxane foam for heat preservation and insulation, wherein the test performance of the product is shown in Table 1.
Example 6
A heat-insulating polyorganosiloxane foam comprises the following raw materials in percentage by mass:
the preparation process comprises the following steps:
(1) Uniformly mixing n-butyl alcohol, KH570 and deionized water in a mass ratio of 10;
(2) Mixing hydroxyl-terminated polysiloxane, vinyl polysiloxane, white carbon black, the modified hollow glass microspheres in the step (1), MQ silicon resin, an inhibitor and hydrogen-containing polysiloxane, stirring for 40 minutes, and then carrying out ultrasonic treatment for 20 minutes to obtain a mixed solution 1;
(3) Adding a catalyst into the mixed solution 1 obtained in the step (2), stirring for 30 minutes to obtain a mixed solution 2, pouring the mixed solution 2 into a mold, and drying for 45 minutes at 150 ℃ to obtain the polyorganosiloxane foam for heat preservation and insulation, wherein the test performance of the product is shown in Table 1.
Example 7
A heat-insulating polyorganosiloxane foam comprises the following raw materials in percentage by mass:
the preparation process comprises the following steps:
(1) Uniformly mixing n-butanol, KH570 and deionized water in a mass ratio of 5;
(2) Mixing hydroxyl-terminated polysiloxane, vinyl polysiloxane, white carbon black, the modified hollow glass microspheres in the step (1), MQ silicon resin, an inhibitor and hydrogen-containing polysiloxane, stirring for 60 minutes, and then carrying out ultrasonic treatment for 15 minutes to obtain a mixed solution 1;
(3) Adding a catalyst into the mixed solution 1 obtained in the step (2), stirring for 30 minutes to obtain a mixed solution 2, pouring the mixed solution 2 into a mold, and drying for 30 minutes at 150 ℃ to obtain the polyorganosiloxane foam for heat preservation and insulation, wherein the test performance of the product is shown in Table 1.
Example 8
A heat-insulating polyorganosiloxane foam comprises the following raw materials in percentage by mass:
the preparation process comprises the following steps:
(1) Uniformly mixing n-butanol, KH570 and deionized water in a mass ratio of 10;
(2) Mixing hydroxyl-terminated polysiloxane, vinyl polysiloxane, white carbon black, the modified hollow glass microspheres in the step (1), MQ silicon resin, an inhibitor and hydrogen-containing polysiloxane, stirring for 50 minutes, and then carrying out ultrasonic treatment for 15 minutes to obtain a mixed solution 1;
(3) Adding a catalyst into the mixed solution 1 obtained in the step (2), stirring for 15 minutes to obtain a mixed solution 2, pouring the mixed solution 2 into a mold, and drying at 150 ℃ for 60 minutes to obtain the polyorganosiloxane foam for heat preservation and insulation, wherein the test performance of the product is shown in Table 1.
TABLE 1 Properties of the polyorganosiloxane foams
Table 1 the apparent densities were tested according to GB/T6343-1995; the compression modulus was tested according to GB/T8813-2020; the compression set was tested according to GBT 6669-2008 using the formula
Calculating, wherein A is the initial height (mm), B is the height after compression (mm), and C is the rebound height (mm); shore A hardness is tested according to GB/T531-1992; the sample was cut into pieces of 10 cm. Times.10 cm, and weighed m 1 After the sample was completely immersed in deionized water for 24 hours, it was weighed m 2 Based on the formula->
Calculating the water absorption rate; reference study of the Effect of the molecular weight of Silicone rubber on the Properties of silicon foams according to the formula>
Calculating porosity where f Is the apparent density of the polyorganosiloxane foam, rho f Corresponding to the apparent density of the solid polyorganosiloxane; the thermal conductivity was tested according to GB/T10294-2008.
According to the analysis of the experimental data (table 1) obtained in different embodiments, it can be seen that the density of the obtained polyorganosiloxanecoates is moderate, which is between medium foaming and low foaming, but the foams maintain lower thermal conductivity, better mechanical properties, higher porosity and lower water absorption, and all the properties meet the requirements of thermal insulation materials.
The above examples are only preferred embodiments of the present invention, which are intended to be illustrative and not limiting, and those skilled in the art should understand that they can make various changes, substitutions and alterations without departing from the spirit and scope of the invention.
Claims (7)
1. A preparation method of polyorganosiloxane foam for heat preservation and heat insulation is characterized by comprising the following steps:
(1) Uniformly mixing n-butyl alcohol, a silane coupling agent and water to obtain a modified solution, then adding the hollow glass beads into the modified solution, uniformly stirring, filtering to obtain filter residues, and drying the filter residues to obtain modified hollow glass beads;
(2) Mixing hydroxyl-terminated polysiloxane, vinyl polysiloxane, white carbon black, the modified hollow glass microspheres in the step (1), MQ silicon resin, an inhibitor and hydrogen-containing polysiloxane, stirring, and performing ultrasonic treatment to obtain a mixed solution 1;
(3) Adding a catalyst into the mixed solution 1 obtained in the step (2), stirring to obtain a mixed solution 2, pouring the mixed solution 2 into a mold, and drying to obtain the polyorganosiloxane foam for heat preservation and heat insulation;
the mass ratio of the n-butanol to the silane coupling agent to the water in the step (1) is 5; the mass ratio of the hollow glass beads to the modified solution in the step (1) is 1; the density of the hollow glass microballoons in the step (1) is 0.18-0.22g/cm 3 The average grain diameter is 2-150 mu m; the hydrogenpolysiloxane in the step (2) is polymethylhydrosiloxane, and the hydrogen content of the hydrogenpolysiloxane is 1.58-1.62%; the hydroxyl-terminated polysiloxane in the step (2) is alpha, omega-dihydroxy polysiloxane, and the viscosity of the hydroxyl-terminated polysiloxane is 750-5000mPa & S; the vinyl polysiloxane in the step (2) is vinyl-terminated polydimethylsiloxane, and the viscosity of the vinyl-terminated polydimethylsiloxane is 500-5000mPa & S; the white carbon black in the step (2) is hydrophobic fumed silica, the particle size of the white carbon black is 10-30nm, and the specific surface area of the white carbon black is 120-140m 2 (ii)/g; the ratio of MQ in the MQ silicon resin in the step (2) is 0.8, the vinyl content is 1.5 percent, and the viscosity is 9000mPa & S;
according to the mass portion of the raw materials,
2. the method for preparing polyorganosiloxane foam for heat preservation and insulation according to claim 1, wherein the silane coupling agent in step (1) is KH570.
3. The method for preparing the polyorganosiloxane foam for heat preservation and insulation according to claim 1, wherein the drying temperature in the step (1) is 120-140 ℃ and the drying time is 3-5 hours.
4. The method for preparing polyorganosiloxane foam for heat preservation and insulation according to claim 1, wherein the inhibitor in the step (2) is 1-ethynyl-1-cyclohexanol.
5. The method for preparing polyorganosiloxane foam for heat preservation and insulation according to claim 1, wherein the catalyst in the step (3) is a complex of platinum ions and vinyl methyl siloxane, and the effective platinum content is 3000-5000PPM.
6. The method for preparing polyorganosiloxane foam for heat preservation and insulation according to claim 1, wherein the stirring treatment time of step (2) is 40-60 minutes, and the ultrasonic treatment time of step (2) is 15-20 minutes; the stirring treatment time in the step (3) is 15-30 minutes, the drying temperature in the step (3) is 150-160 ℃, and the drying time is 30-60 minutes.
7. A polyorganosiloxane foam for thermal insulation produced by the production method according to any one of claims 1 to 6.
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