Flexible hydrophobic aerogel heat insulation sheet with energy storage characteristic and preparation method thereof

文档序号:494880 发布日期:2022-01-07 浏览:28次 中文

阅读说明:本技术 一种具备储能特性的柔性疏水气凝胶隔热片及其制备方法 (Flexible hydrophobic aerogel heat insulation sheet with energy storage characteristic and preparation method thereof ) 是由 张祖琼 罗肖宁 杨浩 常稳 于 2021-08-25 设计创作,主要内容包括:本发明公开了一种具备储能特性的柔性疏水气凝胶隔热片及其制备方法,复合隔热片包括有机多孔泡沫材料、气凝胶材料和相变微胶囊;本发明针对现有有机多孔泡沫材料与气凝胶复合产品的冷面升温速度快的问题,通过提供带相变微胶囊的复合隔热产品,来推迟隔热产品冷面的升温速度;并通过制备方法改善偏厚有机多孔泡沫材料和气凝胶材料复合的隔热材料内部疏水改性不透的问题,并在一定程度上可以缩短有机多孔泡沫材料和气凝胶材料复合隔热产品的制备周期,进而减低成本;采用本制备方法所制得的隔热产品其不仅柔性好而且厚度范围广,可以制备厚度在0.1~0.5mm,最薄可以做到0.1mm,提高了产品的应用范围。(The invention discloses a flexible hydrophobic aerogel heat insulation sheet with energy storage characteristics and a preparation method thereof, wherein the composite heat insulation sheet comprises an organic porous foam material, an aerogel material and a phase change microcapsule; aiming at the problem that the temperature rising speed of the cold surface of the existing organic porous foam material and aerogel composite product is high, the invention delays the temperature rising speed of the cold surface of the heat insulation product by providing the composite heat insulation product with the phase change microcapsule; the preparation method solves the problem that the interior of the thermal insulation material compounded by thicker organic porous foam material and aerogel material is not permeable to hydrophobic modification, and can shorten the preparation period of the thermal insulation product compounded by organic porous foam material and aerogel material to a certain extent, thereby reducing the cost; the heat insulation product prepared by the preparation method is good in flexibility and wide in thickness range, the thickness can be 0.1-0.5 mm, the thinnest thickness can be 0.1mm, and the application range of the product is widened.)

1. A preparation method of a flexible hydrophobic aerogel heat insulation sheet with energy storage characteristics is characterized by comprising the following steps: the method comprises the following steps:

s1, preparing raw materials of the composite hydrolysate:

the raw materials of the composite hydrolysate comprise the following components: the phase change coating comprises absolute ethyl alcohol, deionized water, phase change microcapsules, a dispersing agent, a hydrophobic modifier and other components, wherein the other components are any one of a single metal alkoxide, a compound of two or more different metal alkoxides, a single silicon source, a compound of two or more different silicon sources, and a compound of at least one metal alkoxide and at least one silicon source;

and the preparation is carried out according to the following parts by weight: 500-1500 parts of absolute ethyl alcohol, 60-100 parts of deionized water, 10-100 parts of phase change microcapsules, 1-5 parts of a dispersing agent and 150-300 parts of other components, wherein the weight part of a hydrophobic modifier is not more than 3 times that of the other components, and preferably 0.4-1 time;

s2, preparing composite hydrolysate:

uniformly mixing the raw materials obtained in the step S1, and then adjusting the pH value to 1.5-3.5; hydrolyzing for 6-12 h at 20-50 ℃ to finish the preparation of the composite hydrolysate A;

s3, dipping and gelling;

firstly, adjusting the pH value of the composite hydrolysate A to be alkaline, and then soaking the organic porous foam material in the alkaline composite hydrolysate A for 30-120 min to prepare a wet gel product B of the organic porous foam material;

s4, aging;

removing redundant wet gel on the outer surface of a wet gel product B of the organic porous foam material, then soaking the wet gel product B into absolute ethyl alcohol, and standing the wet gel product B for 6-12 hours at 50-70 ℃ to prepare an aged composite product C;

s5, drying;

drying the aged composite product C, and removing the organic solvent to obtain a product D;

s6, cutting into rolls or sheets:

the product D is cut into rolls or sheets as needed.

2. The method for preparing a flexible hydrophobic aerogel thermal insulation sheet with energy storage characteristics as claimed in claim 1, further comprising a packaging process after step S6, wherein the packaging process comprises:

s7, packaging:

packaging a layer of packaging film material on each of two sides of the product obtained in the step S6; the packaging film material comprises a film material and an adhesive layer, wherein the film material is an organic film or a flexible fabric or a metal foil, and the adhesive layer comprises acrylic adhesive and epoxy adhesive.

3. The method for preparing the flexible hydrophobic aerogel heat insulation sheet with the energy storage property as claimed in claim 2, wherein the organic film is any one of a PET film, a PI film, a PC film, a PE film, a PVC film and a PTFE film; or the flexible fabric is any one of glass fiber cloth, high silica glass fiber cloth, ceramic fiber cloth and non-woven fabric; or the metal foil is any one of copper foil, aluminum foil, tin foil, gold foil and silver foil.

4. The method for preparing the flexible hydrophobic aerogel heat insulation sheet with the energy storage property as claimed in claim 1 or 2, wherein in the step S1, the weight part of the hydrophobic modifier is 0.4-1 times of the weight part of the other components.

5. The method for preparing the flexible hydrophobic aerogel heat insulation sheet with the energy storage property as claimed in claim 1 or 2, wherein the hydrophobic modifier is a compound containing hydrophobic organic groups; the shell material of the phase-change microcapsule is melamine resin or SiO2Polymethyl methacrylate, polyurea and polyurethane materials, phase-change microThe phase-change material of the capsule is any one of paraffin, polyethylene glycol, fatty acid and derivatives thereof, the phase-change temperature is 30-70 ℃, the enthalpy value of the phase-change material is required to be more than or equal to 100J/g, the content of the phase-change material is required to be more than or equal to 80%, and the average particle size D50 is 0.5-5 μm.

6. The method for preparing the flexible hydrophobic aerogel heat insulation sheet with the energy storage property as claimed in claim 1 or 2, wherein in step S3, the organic porous foam material is any one of melamine foam, EVA foam, polyimide foam, polyurethane foam, silicone rubber foam, ethylene propylene diene monomer foam, phenolic foam, CR foam, polymethacrylimide foam and sound absorption foam, and the grammage of the organic porous foam material is 5-50 kg/m3

7. The method for preparing the flexible hydrophobic aerogel thermal insulation sheet with the energy storage property as claimed in claim 1 or 2, wherein the drying method adopted by the aged composite product C in the step S5 is CO2Supercritical drying, ethanol supercritical drying, freeze drying, and drying under normal pressure.

8. The method for preparing a flexible hydrophobic aerogel thermal insulation sheet with energy storage property as claimed in claim 1 or 2, wherein in step S6, the thickness of the coiled material or the sheet material is in the range of 0.1-300 mm, preferably 0.1-10 mm.

9. The utility model provides a flexible hydrophobic aerogel heat insulating sheet that possesses energy storage characteristic which characterized in that: comprises a composite heat insulation sheet (1), wherein the composite heat insulation sheet (1) is prepared by the preparation method of claim 1, and the composite heat insulation sheet (1) comprises an organic porous foam material (101), an aerogel material (102) and phase-change microcapsules (103).

10. The flexible hydrophobic aerogel thermal insulation sheet with energy storage properties of claim 9, wherein: two end faces of the composite heat insulation sheet (1) are provided with packaging film materials (2); the packaging film material comprises a film material (201) and an adhesive layer (202), wherein the film material (201) is connected with the end face of the composite heat insulation sheet (1) through the adhesive layer (202); the film material is an organic film or a flexible fabric or a metal foil, and the adhesive layer comprises acrylic adhesive and epoxy adhesive.

Technical Field

The invention belongs to the field of heat insulation application of 3C industry and new energy industry, and particularly relates to a flexible hydrophobic aerogel heat insulation sheet with an energy storage characteristic and a preparation method thereof.

Background

In recent years, with the rapid development of science and technology, the types and the use amount of intelligent household appliances and new energy automobiles are more and more, the functions are more and more comprehensive, the performances are more and more powerful, and the problems of larger load capacity, higher heat generation quantity, easier thermal runaway and the like are brought. Overheating of the product may result in damage to components, reduced equipment life, and damage to human skin. Therefore, good thermal protection is one of the key points of enterprise development and management and control of the 3C industry and the new energy industry, and not only can the product be provided with a longer service life, but also safer protection can be provided for people.

Aerogel materials, as the solid materials with the minimum density in the world at present, have extremely high porosity and extremely low thermal conductivity, and are widely applied to the fields of aerospace, aviation, automobiles, new energy, clothing and the like. The phase-change material is always used as one of the preferred materials for thermal protection because of larger enthalpy value in the phase-change process and better energy storage capacity and regulation capacity for external temperature, and the phase-change microcapsule provides a good carrier for stable use of the phase-change material. The organic porous foam material has the advantages of small density, good flexibility, high porosity, processed and the like, so that the organic porous foam material can be used for noise isolation, insulation, heat insulation and the like. However, the heat insulation products developed in the market at present and made of organic porous foam materials, aerogel materials and phase-change materials have some problems, mainly the problems that the temperature rising speed of a cold surface is high, the ultrathin heat insulation sheet product with the thickness not more than 0.5mm is difficult to manufacture, and the interior of the heat insulation material compounded by the thicker organic porous foam materials and the aerogel materials is not permeable to hydrophobic modification in the preparation process.

Disclosure of Invention

In view of the above-described deficiencies in the prior art, the present invention provides a flexible hydrophobic aerogel thermal insulation sheet having energy storage characteristics and a method for preparing the same.

The technical scheme adopted by the invention is as follows:

a preparation method of a flexible hydrophobic aerogel heat insulation sheet with energy storage characteristics comprises the following steps:

s1, preparing raw materials of the composite hydrolysate:

the raw materials of the composite hydrolysate comprise the following components: the phase change coating comprises absolute ethyl alcohol, deionized water, phase change microcapsules, a dispersing agent, a hydrophobic modifier and other components, wherein the other components are any one of a single metal alkoxide, a compound of two or more different metal alkoxides, a single silicon source, a compound of two or more different silicon sources, and a compound of at least one metal alkoxide and at least one silicon source; the other components are raw materials for preparing the aerogel;

and the preparation is carried out according to the following parts by weight: 500-1500 parts of absolute ethyl alcohol, 60-100 parts of deionized water, 10-100 parts of phase change microcapsules, 1-5 parts of a dispersing agent, 150-300 parts of other components, and the weight part of a hydrophobic modifier is not more than 3 times, preferably 0.4-1 time of that of the other components.

S2, preparing composite hydrolysate:

uniformly mixing the raw materials obtained in the step S1, and then adjusting the pH value to 1.5-3.5 by using an acid catalyst; and hydrolyzing for 6-12 h at 20-50 ℃ to complete preparation of the composite hydrolysate A, wherein the composite hydrolysate A is the aerogel raw material hydrolysate.

S3, dipping and gelling;

firstly, adjusting the pH value of the composite hydrolysate A to be alkaline by using an alkali catalyst, and then soaking the organic porous foam material in the alkaline composite hydrolysate A for 30-120 min to prepare a wet gel product B of the organic porous foam material; in order to better perform the impregnation, the vacuum pumping mode is preferably adopted for assistance, so that the impregnation effect is improved.

S4, aging;

removing redundant wet gel on the outer surface of a wet gel product B of the organic porous foam material, then soaking the wet gel product B into absolute ethyl alcohol, and standing the wet gel product B for 6-12 hours at 50-70 ℃ to prepare an aged composite product C;

s5, drying;

drying the aged composite product C, and removing the organic solvent to obtain a product D; the drying method can use CO used in conventional aerogel preparation2Supercritical drying, ethanol supercritical drying, freeze drying and normal pressure drying.

S6, cutting into rolls or sheets:

cutting the product D into coiled materials or sheets according to the needs, and cutting the product D into coiled materials with the needed thickness by using a commercially available sponge rotary cutter when the coiled materials are needed to obtain a product E; and when the sheet is needed, cutting the product D into the sheet with the needed thickness by using a commercial sponge horizontal cutting machine to obtain a product F, wherein the thickness of the product E and the product F is 0.1-300 mm, and preferably 0.1-10 mm.

As a preferable aspect of the present invention, in order to encapsulate the web or sheet with a film material and avoid dusting and scratching during use, an encapsulation process is further provided after step S6, that is:

s7, packaging:

packaging a layer of packaging film material on each of two sides of the product obtained in the step S6; the packaging film material comprises a film material and an adhesive layer, wherein the film material is an organic film or a flexible fabric or a metal foil, and the adhesive layer comprises acrylic adhesive and epoxy adhesive. And during specific packaging, a hot press pressing mode, a manual bonding mode or a jig bonding mode can be selected to package a layer of packaging film material on each of two surfaces of the product E or the product F, and the product G is prepared.

As a preferable scheme of the present invention, the organic film is any one of a PET film, a PI film, a PC film, a PE film, a PVC film, and a PTFE film; or the flexible fabric is any one of glass fiber cloth, high silica glass fiber cloth, ceramic fiber cloth and non-woven fabric; or the metal foil is any one of copper foil, aluminum foil, tin foil, gold foil and silver foil.

As a preferred embodiment of the present invention, the single metal alkoxide includes a single metal alkoxide and a double metal alkoxide, preferably an aluminum alkoxide; the single silicon source comprises organic silicon alkoxide and water glass (Na)2O·nSiO2) And silica sol (nSiO)2·H2O), preferably Tetraethylorthosilicate (TEOS); the composite of two or more different metal alkoxide compounds, the composite of two or more different silicon sources, the composite of at least one metal alkoxide and at least one silicon source are preferably the composite of metal alkoxide and silicon source and the composite of multiple silicon sources.

As a preferable scheme of the invention, the hydrophobic modifier contains compounds with alkyl, alkoxy, chlorosilane and other hydrophobic organic groups, common silicon-based hydrophobic modifiers comprise methyltrimethoxysilane (MTMS), dimethyldimethoxysilane (DMDMS), Trimethylchlorosilane (TMCS), Trimethylethoxysilane (TMES) and Hexamethyldisilazane (HMDS), preferably Trimethylethoxysilane (TMES), and the modifier is added into hydrolysate to avoid the problem that the interior of a product with the thickness of more than 10mm cannot be subjected to hydrophobic modification when the surface of the product is subjected to hydrophobic modification after gel is adopted for producing the organic porous foam material and aerogel material composite heat insulation product at present.

In a preferred embodiment of the present invention, the shell material of the phase-change microcapsule is melamine resin or SiO2The phase-change microcapsule is prepared from any one of materials including polymethyl methacrylate (PMMA), polyurea and polyurethane, wherein the phase-change material of the phase-change microcapsule is any one of paraffin, polyethylene glycol (PEG), fatty acid and derivatives thereof, the phase-change temperature is 30-70 ℃, the enthalpy value of the phase-change material is required to be more than or equal to 100J/g, the content of the phase-change material is required to be more than or equal to 80%, and the average particle size D50 is 0.5-5 mu m.

As a preferable embodiment of the present invention, in step S3, the organic porous foam material is any one of melamine foam, EVA foam, polyimide foam, polyurethane foam (PU), silicone rubber foam, ethylene propylene diene monomer foam, phenol foam, CR foam, polymethacrylimide foam, and sound absorbing foam, and the grammage of the organic porous foam material is 5 to 50kg/m3

The invention also provides a flexible hydrophobic aerogel heat insulation sheet with the energy storage characteristic, which comprises a composite heat insulation sheet, wherein the composite heat insulation sheet is prepared by the preparation method, and the composite heat insulation sheet comprises an organic porous foam material, an aerogel material and a phase change microcapsule.

As a preferred scheme of the invention, the two end faces of the composite heat insulation sheet are provided with packaging film materials; the packaging film material comprises a film material and a glue layer, and the film material is connected with the end face of the composite heat insulation sheet through the glue layer; the film material is an organic film or a flexible fabric or a metal foil, and the adhesive layer comprises acrylic adhesive and epoxy adhesive.

Aiming at the problem that the temperature rising speed of the cold surface of the existing organic porous foam material and aerogel composite product is high, the invention delays the temperature rising speed of the cold surface of the heat insulation product by providing the composite heat insulation product with the phase change microcapsule; the preparation method solves the problem that the interior of the thermal insulation material compounded by thicker organic porous foam material and aerogel material is not permeable to hydrophobic modification, and can shorten the preparation period of the thermal insulation product compounded by organic porous foam material and aerogel material to a certain extent, thereby reducing the cost; the heat insulation product prepared by the preparation method is good in flexibility and wide in thickness range, the thickness can be 0.1-0.5 mm, the thinnest thickness can be 0.1mm, and the application range of the product is widened.

According to the invention, the phase-change microcapsule, the aerogel material and the organic porous foam material are compounded to prepare the flexible heat insulation sheet with a good energy storage function, the flexible heat insulation sheet can be directly used, can also be packaged by a membrane material for use, can be applied to various scenes such as the heat protection field of 3C products and new energy industries, and provides a better choice for the heat protection design.

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 schematic structural diagram of a packaged flexible hydrophobic aerogel thermal insulation sheet with energy storage characteristics.

Fig. 2 is a schematic structural diagram of an unpackaged flexible hydrophobic aerogel thermal insulation sheet with energy storage characteristics.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without inventive effort based on the embodiments of the present invention, are within the scope of the present invention.

Example 1:

1) preparing materials: selecting a phase change microcapsule (selecting a shell material as melamine, a phase change material as paraffin, the phase change temperature of 50 ℃, D50=2 μm, and the mass content of the phase change material is 79%), tetraethoxysilane (selecting silicon 40), a hydrophobic modifier (selecting TMES), absolute ethyl alcohol (selecting the purity of 95%), a dispersing agent (selecting PEG 1500), and all the components are commercially available;

2) preparing a composite hydrolysate: the preparation method comprises the following steps of proportioning 500 parts by mass of absolute ethyl alcohol, 100 parts by mass of deionized water, 150 parts by mass of tetraethoxysilane, 40 parts by mass of phase change microcapsules, 80 parts by mass of hydrophobic modifier and 2 parts by mass of dispersant, uniformly stirring and mixing (rotating speed 500 revolutions for 5 min), adjusting the pH of the hydrolysate to 1.5-3.5 by using HCl with the concentration of 36wt% as a catalyst, and carrying out hydrolysis reaction at 50 ℃ for 10 hours to complete the preparation of the composite hydrolysate A.

3) Impregnation and gelling: firstly, alkaline catalyst NaHCO is used3And (3) adjusting the pH value of the composite hydrolysate A to 9, and then soaking the organic porous foam material in hydrolysis for 80min to prepare a wet gel product B of the organic porous foam material.

4) Aging: and removing the redundant wet gel on the outer surface of the wet gel product B of the organic porous foam material, then soaking the wet gel product B into absolute ethyl alcohol, and standing the wet gel product B for 12 hours at the temperature of 50 ℃ to prepare an aged composite product C.

5) And (3) drying: by using CO2Supercritical drying the composite product C to remove organic solvent to obtain product D, wherein CO is2The reference parameters of supercritical drying are temperature of 45 ℃, pressure of 8MPa and time of 6-12 h.

6) Cutting into sheets: and cutting the product D into sheets with required thickness by using a commercially available sponge horizontal cutting machine (removing materials with the surface being 6mm, and taking a product made of the product D as a test product) to obtain a product F, wherein the thickness of the product F is 0.1mm and 2mm, and the cutting parameters are that the cutting speed is 10-30/min and the motor power is 4-5 KW.

7) Packaging: the step is an alternative process, is carried out when packaging is needed, and is carried out by packaging a layer of film material on each of two surfaces of a product F with the thickness of 2mm by a manual laminating method to prepare the product G, wherein the thickness of PET in the film material is 50 mu m, and the thickness of acrylic glue is 25 mu m.

Example 2:

1) preparing materials: the phase-change microcapsule (melamine is selected as a shell material, paraffin is selected as a phase-change material, the phase-change temperature is 50 ℃, D50=2 μm, and the mass content of the phase-change material is 79%), ethyl orthosilicate (silicon 40 is selected), aluminum sec-butoxide, a hydrophobic modifier (TMES is selected), absolute ethyl alcohol (purity 95% is selected), a dispersing agent (PEG 1500 is selected), and all the components are commercially available.

2) Preparing a composite hydrolysate: the preparation method comprises the following steps of proportioning 500 parts of absolute ethyl alcohol, 100 parts of deionized water, 150 parts of various compounds (comprising 100 parts of ethyl orthosilicate and 50 parts of aluminum sec-butoxide), 40 parts of phase-change microcapsules, 80 parts of hydrophobic modifier and 2 parts of dispersing agent by mass, uniformly stirring and mixing (rotating speed is 500 revolutions for 5 min), adjusting the pH of the hydrolysate to 1.5-3.5 by using HCl with concentration of 36wt% as a catalyst, and carrying out hydrolysis reaction at 50 ℃ for 10 hours to complete the preparation of the composite hydrolysate A.

3) Impregnation and gelling: firstly, alkaline catalyst NaHCO is used3And (3) adjusting the pH value of the composite hydrolysate A to 9, and then soaking the organic porous foam material in hydrolysis for 100min to prepare a wet gel product B of the organic porous foam material.

4) Aging: and removing the redundant wet gel on the outer surface of the wet gel product B of the organic porous foam material, then soaking the wet gel product B into absolute ethyl alcohol, and standing the wet gel product B for 12 hours at the temperature of 50 ℃ to prepare an aged composite product C.

5) And (3) drying: and (3) performing supercritical drying on the composite product C by adopting an ethanol supercritical drying process, and removing the organic solvent to obtain a product D, wherein the reference parameters of the ethanol supercritical drying are 280 ℃, 8MPa and 6-12 h.

6) Cutting into sheets: and cutting the product D into sheets with required thickness by using a commercially available sponge horizontal cutting machine (removing materials with the surface being 6mm, and taking a product made of the product D as a test product) to obtain a product F, wherein the thickness of the product F is 0.1mm and 2mm, and the cutting parameters are that the cutting speed is 10-30/min and the motor power is 4-5 KW.

7) And (3) packaging: the step is an alternative process, is carried out when packaging is needed, and is carried out by packaging a layer of film material on each of two surfaces of a product F with the thickness of 2mm by adopting a manual laminating method to prepare the product G, wherein the thickness of PET in the film material is 50 mu m, and the thickness of acrylic adhesive is 25 mu m.

Example 3:

1) preparing materials: selecting phase-change microcapsule (selecting shell material as SiO)2The phase-change material is polyethylene glycol 6000, the phase-change temperature is 60 ℃, D50=2 μm, the mass content of the phase-change material is 68 percent), tetraethoxysilane (silicon 40 is selected), a hydrophobic modifier (TMES is selected), absolute ethyl alcohol (the purity is 95 percent) and a dispersant (PEG 1500 is selected) are all sold in the market;

2) preparing a composite hydrolysate: the preparation method comprises the following steps of proportioning 500 parts by mass of absolute ethyl alcohol, 100 parts by mass of deionized water, 150 parts by mass of tetraethoxysilane, 40 parts by mass of phase change microcapsules, 80 parts by mass of hydrophobic modifier and 2 parts by mass of dispersant, uniformly stirring and mixing (rotating speed 500 revolutions for 5 min), adjusting the pH of the hydrolysate to 1.5-3.5 by using HCl with the concentration of 36wt% as a catalyst, and carrying out hydrolysis reaction at 50 ℃ for 10 hours to complete the preparation of the composite hydrolysate A.

3) Impregnation and gelling: firstly, alkaline catalyst NaHCO is used3And (3) adjusting the pH value of the composite hydrolysate A to 9, and then soaking the organic porous foam material in hydrolysis for 80min to prepare a wet gel product B of the organic porous foam material.

4) Aging: and removing the redundant wet gel on the outer surface of the wet gel product B of the organic porous foam material, then soaking the wet gel product B into absolute ethyl alcohol, and standing the wet gel product B for 12 hours at the temperature of 50 ℃ to prepare an aged composite product C.

5) And (3) drying: and (3) performing supercritical drying on the composite product C by adopting an ethanol supercritical drying process, and removing the organic solvent to obtain a product D, wherein the reference parameters of the ethanol supercritical drying are 280 ℃, 8MPa and 6-12 h.

6) Cutting into sheets: and cutting the product D into sheets with required thickness by using a commercially available sponge horizontal cutting machine (removing materials with the surface being 6mm, and taking a product made of the product D as a test product) to obtain a product F, wherein the thickness of the product F is 0.1mm and 2mm, and the cutting parameters are that the cutting speed is 10-30/min and the motor power is 4-5 KW.

7) And (3) packaging: the step is an alternative process, is carried out when packaging is needed, and is carried out by packaging a layer of film material on each of two surfaces of a product F with the thickness of 2mm by adopting a manual laminating method to prepare the product G, wherein the thickness of PET in the film material is 50 mu m, and the thickness of acrylic adhesive is 25 mu m.

Comparative example 1:

corresponding to example 1, the difference is that no phase-change microcapsule is added in comparative example 1, and the specific steps are as follows:

1) preparing materials: the selected tetraethoxysilane (selected from silicon 40), hydrophobic modifier (selected from TMES), absolute ethyl alcohol (selected from 95% purity) and dispersant (selected from PEG 1500) are all sold in the market.

2) Preparing a composite hydrolysate: the preparation method comprises the following steps of proportioning 500 parts by mass of absolute ethyl alcohol, 100 parts by mass of deionized water, 150 parts by mass of tetraethoxysilane, 80 parts by mass of hydrophobic modifier and 2 parts by mass of dispersant, uniformly stirring and mixing (rotating speed is 500 revolutions, time is 5 min), adjusting the pH of the hydrolysate to 1.5-3.5 by using HCl with concentration of 36wt% as a catalyst, and carrying out hydrolysis reaction at 50 ℃ for 10 hours to complete preparation of the composite hydrolysate A.

3) Impregnation and gelling: firstly, alkaline catalyst NaHCO is used3And (3) adjusting the pH value of the composite hydrolysate A to 9, and then soaking the organic porous foam material in hydrolysis for 80min to prepare a wet gel product B of the organic porous foam material.

4) Aging: and removing the redundant wet gel on the outer surface of the wet gel product B of the organic porous foam material, then soaking the wet gel product B into absolute ethyl alcohol, and standing the wet gel product B for 12 hours at the temperature of 50 ℃ to prepare an aged composite product C.

5) And (3) drying: by using CO2Supercritical drying the composite product C to remove organic solvent to obtain product D, wherein CO is2The reference parameters of supercritical drying are temperature of 45 ℃, pressure of 8MPa and time of 6-12 h.

6) Cutting into sheets: and cutting the product D into sheets with required thickness by using a commercially available sponge horizontal cutting machine (removing materials with the surface being 6mm, and taking a product made of the product D as a test product) to obtain a product F, wherein the thickness of the product F is 0.1mm and 2mm, and the cutting parameters are that the cutting speed is 10-30/min and the motor power is 4-5 KW.

7) And (3) packaging: and (3) respectively packaging a layer of film material on each of two sides of a product F with the thickness of 2mm by adopting a manual laminating method to prepare a product G, wherein the thickness of PET in the film material is 50 mu m, and the thickness of acrylic glue is 25 mu m.

Comparative example 2:

the difference is that in comparative example 2, the hydrolysis liquid is not added with hydrophobic modifier in step 2, and the conventional surface hydrophobic modification treatment after supercritical drying is selected, and the specific steps are as follows:

1) preparing materials: in the case, the selected tetraethoxysilane (selected from silicon 40), the hydrophobic modifier (selected from TMCS), the absolute ethyl alcohol (selected from 95% purity) and the dispersing agent (selected from PEG 1500) are all sold in the market.

2) Preparing a composite hydrolysate: the preparation method comprises the following steps of proportioning 500 parts by mass of absolute ethyl alcohol, 100 parts by mass of deionized water, 150 parts by mass of tetraethoxysilane, 80 parts by mass of hydrophobic modifier and 2 parts by mass of dispersant, uniformly stirring and mixing (rotating speed is 500 revolutions, time is 5 min), adjusting the pH of the hydrolysate to 1.5-3.5 by using HCl with concentration of 36wt% as a catalyst, and carrying out hydrolysis reaction at 50 ℃ for 10 hours to complete preparation of the composite hydrolysate A.

3) Impregnation and gelling: firstly, alkaline catalyst NaHCO is used3And (3) adjusting the pH value of the composite hydrolysate A to 9, and then soaking the organic porous foam material in hydrolysis for 80min to prepare a wet gel product B of the organic porous foam material.

4) Aging: and removing the redundant wet gel on the outer surface of the wet gel product B of the organic porous foam material, then soaking the wet gel product B into absolute ethyl alcohol, and standing the wet gel product B for 12 hours at the temperature of 50 ℃ to prepare an aged composite product C.

5) And (3) drying: by using CO2Supercritical drying the composite product C to remove organic solvent to obtain product D, wherein CO is2The reference parameters of supercritical drying are temperature of 45 ℃, pressure of 8MPa and time of 6-12 h.

6) Surface hydrophobic modification: firstly, mixing a hydrophobic modifier with absolute ethyl alcohol according to a mass ratio of 5:100, uniformly stirring, then immersing the composite product D in the mixture, and standing at 70 ℃ for 8 hours to obtain a composite product H subjected to hydrophobic modification.

7) Cutting into sheets: and cutting the product H into sheets with required thickness by using a commercially available sponge horizontal cutting machine (products made of materials with the thickness of 6mm on the outer surface of the product D are marked as a test product 1, products made of materials at other parts are marked as a test product 2), and obtaining a product F, wherein the thickness of the product F is 0.1mm and 2mm, and the cutting parameters are cutting speed of 10-30/min and motor power of 4-5 KW.

7) And (3) packaging: and (3) respectively packaging a layer of film material on each of two sides of a product F with the thickness of 2mm by adopting a manual laminating method to prepare a product G, wherein the thickness of PET in the film material is 50 mu m, and the thickness of acrylic glue is 25 mu m.

The examples and comparative examples were tested for hydrophobicity and thermal insulation, as follows:

hydrophobicity test method:

the hydrophobicity of the product is expressed by a static surface contact angle theta, the larger the value of the theta is, the better the hydrophobicity is, the contact angle theta of the sample to water is measured by an optical contact angle measuring instrument of OCA20 model of Germany Dataphysics company, a flat plane of the sample is selected, water drops are dropped on the flat plane, and after the liquid drops are stabilized, the size of the contact angle theta is calculated by instrument software by using a tangent method.

The heat insulation performance test method comprises the following steps:

1) selecting a heating table and a contact type thermocouple thermodetector, and calibrating;

2) setting the temperature of a heater to be 200 ℃, and starting heating;

3) after the temperature of the heater is stabilized at 200 ℃, quickly placing the heat insulation pad bonded with the thermocouple temperature measuring wire on a heating table, and starting timing and temperature measurement;

4) and (3) reading data once every 2min, respectively reading the cold surface temperature of the sample at 2min, 4min, 6min, 8min, 10min, 12min, 14min and 16min, and recording.

The experimental comparison results of the examples and comparative examples are as follows:

according to the results of examples 1-3 and comparative example 1 in the table, the product of the invention can effectively slow down the temperature rise speed of the cold surface of the sample, and meanwhile, the data comparison between the example 1 and the comparative example 2 shows that the product of the invention can ensure the internal hydrophobicity of the product. Further, according to the processes of example 1 and comparative example 2, it was found that the time for the process of preparing the heat insulating material in which the organic porous foam material is combined with the aerogel composite according to the present invention is shorter because the process of hydrophobically modifying the surface after gelation in one step, which takes a longer time, is omitted.

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