CN111660649B - Method for manufacturing high-strength laminated heat-insulation composite material - Google Patents
Method for manufacturing high-strength laminated heat-insulation composite material Download PDFInfo
- Publication number
- CN111660649B CN111660649B CN202010549682.7A CN202010549682A CN111660649B CN 111660649 B CN111660649 B CN 111660649B CN 202010549682 A CN202010549682 A CN 202010549682A CN 111660649 B CN111660649 B CN 111660649B
- Authority
- CN
- China
- Prior art keywords
- prepreg
- pressing
- composite material
- base material
- thickness
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/10—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/38—Layered products comprising a layer of synthetic resin comprising epoxy resins
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
- C08L63/04—Epoxynovolacs
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/30—Properties of the layers or laminate having particular thermal properties
- B32B2307/304—Insulating
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
Landscapes
- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Fluid Mechanics (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Reinforced Plastic Materials (AREA)
- Laminated Bodies (AREA)
Abstract
The invention relates to a method for manufacturing a high-strength laminated heat-insulating composite material, which takes high-temperature-resistant low-heat-conductivity ceramic fiber paper as a base material and high-temperature-resistant novolac epoxy resin as an adhesive to prepare the high-strength heat-insulating composite material, wherein the density of the high-strength heat-insulating composite material is controlled to be 1.5-1.8 g/cm3The glass transition temperature (Tg) of the obtained product is maintained to be above 160 ℃, the normal state compression strength is above 300MPa, and the product can be used for a long time at the temperature of 200 ℃.
Description
Technical Field
The invention relates to a method for manufacturing a high-strength laminated heat-insulation composite material, belonging to the technical field of laminated product composite materials.
Background
The application of the heat insulation material in industrial engineering has great significance for saving energy and reducing emission, while the traditional heat insulation material generally takes a porous or micro-nano composite structure material as a main material, such as aerogel, polyurethane foam material and the like, has low mechanical strength (the compressive strength is generally lower than 8MPa), is easy to break and damage, and has a plurality of limitations in practical application, in addition, the preparation process is generally complex, if the aerogel generally needs to be subjected to sol preparation, gelation treatment, alcohol aging, supercritical drying, heat treatment and other steps, the strength of the prepared sample is generally lower than 1 MPa; the difficulty of the polyurethane thermal insulation material lies in that a plurality of raw materials including polyether polyol, polyester polyol, isocyanate, a surfactant, a physical foaming agent and the like are screened, the subsequent processes of mixing, foaming, curing and the like are complex and time-consuming, the strength of a prepared sample is generally lower than 8MPa, the reported maximum compressive strength is only 42MPa, the cost is high, and the actual requirement under a high-pressure state cannot be met. The prepared novel heat-insulating composite material with high strength, low heat conductivity and aging resistance has wide market prospect and application requirements, and can solve the problem of energy loss in the high-temperature processing process to a great extent.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a method for manufacturing a high-strength laminated heat-insulating composite material, which has the following specific technical scheme:
a method for manufacturing a high-strength laminated heat-insulating composite material comprises the following steps:
weighing 100 parts by mass of novolac epoxy, 40-60 parts by mass of epoxy resin, 20-40 parts by mass of 4, 4' -diamino diphenyl sulfone, 0.45 part by mass of hindered phenol antioxidant and 1.2 parts by mass of silane coupling agent, dissolving in acetone, and uniformly stirring to obtain premixed slurry;
step two, taking the premixed slurry, weighing an accelerant according to the proportion that the solid content of resin in the premixed slurry is 10wt per thousand, dissolving the accelerant in acetone, and then uniformly stirring and mixing the accelerant and the premixed slurry, wherein the modulation and curing time is 160-180 s, so that mixed slurry is obtained for later use;
thirdly, gluing the insulating base material by using the mixed slurry;
step four, baking the rubberized insulating base material to obtain a prepreg;
laying layers, and pressing by a press;
step six, in the pressing process, the preheating temperature is 120 ℃, the preheating time is 30min, and the measured fluidity is 8-10%; after preheating, heating to 160 ℃ for curing, and obtaining the high-strength laminated heat-insulating composite material after curing.
As an improvement of the technical scheme, the accelerant is boron trifluoride monoethylamine.
As an improvement of the technical scheme, the insulating base material is one or more of ceramic paper, electronic cloth and checked cloth.
As an improvement of the technical scheme, the epoxy resin is one or more of E44 type epoxy resin, E50 type epoxy resin and E51 type epoxy resin.
As an improvement of the technical scheme, when the insulating base material is ceramic paper, dipping the insulating base material in a vacuum leading-in mode; cutting and weighing the ceramic paper, and checking the use amount of the mixed slurry according to the weight percent (45+5) by dry weight of the cut ceramic paper; introducing the mixed slurry, infiltrating the insulating base material, and standing for 30min to obtain a prepreg; and taking out the prepreg, and placing the prepreg in an oven at 120 ℃ for baking for 3min to obtain the prepreg.
As the improvement of the technical proposal, when the insulating base material is electronic cloth, the continuous gluing mode is adopted for operation; placing the mixed slurry in a glue tank, leading the electronic cloth to be dipped in glue by a single shaft of a tractor, controlling the glue amount by double-roller extrusion, adjusting the pressure of the double rollers, and controlling the glue applying amount to be 21 wt%; the dipped rubber material enters a chain type dryer to be dried under the action of the tension of a traction machine; the traction speed is 3m/min, the temperature of the dryer is 140 ℃, the length of a oven box of the dryer is 9m, and the impregnated material is dried to obtain the prepreg.
As the improvement of the technical proposal, when the insulating base material is the checked cloth, the operation is carried out by adopting a continuous gluing mode; placing the mixed slurry in a glue tank, guiding the checked cloth to be dipped in glue in a single shaft by a tractor, extruding by a pair of rollers to control the glue amount, adjusting the pressure of the pair of rollers, and controlling the glue applying amount to be not higher than 18 wt%; the dipped rubber material enters a chain type dryer to be dried under the action of the tension of a traction machine; the traction speed is 3m/min, the temperature of the dryer is set to be 140 ℃, and the length of a dryer oven is 9 m; and drying the dipped material to obtain a prepreg.
As an improvement of the technical scheme, in the pressing process, the curing time is set according to the thickness of the pressing material, and the curing time is increased by 30min every time the thickness of the pressing material is increased by 1 mm.
The invention has the beneficial effects that:
the manufacturing method of the high-strength laminated heat-insulation composite material takes high-temperature-resistant low-heat-conductivity ceramic fiber paper as a base material and high-temperature-resistant novolac epoxy resin as an adhesive to prepare the high-strength heat-insulation composite material, and the density of the high-strength laminated heat-insulation composite material is controlled to be 1.5-1.8 g/cm3The glass transition temperature (Tg) of the obtained product is maintained to be above 160 ℃, the normal state compression strength is above 300MPa, and the product can be used for a long time at the temperature of 200 ℃.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
Dissolving 100kg of 638S type novolac epoxy, 40kg of E44 type epoxy resin, 20kg of 4, 4' -diaminodiphenyl sulfone (DDS), 0.45kg of V85-P type hindered phenol antioxidant and 1.2kg of KH560 type silane coupling agent in acetone, uniformly stirring to obtain premixed slurry, and temporarily storing in a container for a storage period of not more than 3 months.
Weighing an accelerator boron trifluoride monoethylamine according to the solid content of resin in the premixed slurry being 10wt per mill, dissolving the accelerator boron trifluoride monoethylamine in acetone, uniformly stirring and mixing the accelerator boron trifluoride monoethylamine and the premixed slurry, and adjusting the curing time to be 160-180 s to obtain mixed slurry for later use, wherein the storage period is not more than 1 week;
the insulating substrate is ceramic paper (ceramic fiber paper) with the thickness of 2 mm. Cutting the ceramic paper to a defined size, for example 1250mm x 1000mm, or cutting according to requirements;
weighing the cut ceramic paper, and layering according to the rated thickness and 0.2mm of each layer; the amount of the mixed slurry was determined by dry weight (45+5) wt% based on the mass of the ceramic paper. Introducing the mixed slurry, standing for 30min after the ceramic paper is uniformly soaked to obtain a prepreg; and taking out the prepreg, and placing the prepreg in an oven at 120 ℃ for baking for 3min to obtain a prepreg A.
And layering the prepregs A according to a preset thickness in each layer of 0.2mm, and pressing by a press.
Preheating at 120 ℃ for 30min, measuring the fluidity of the composite material to be 8-10%, heating to 160 ℃ for curing, and setting the curing time according to the thickness of 30min/mm to obtain the high-strength laminated heat-insulating composite material X.
In the pressing process, the preheating temperature is 120 ℃, the preheating time is 30min, and the measured fluidity is 8-10%; after preheating, heating to 160 ℃ for curing, and obtaining the high-strength laminated heat-insulating composite material X after curing. In the pressing process, the curing time is set according to the thickness of the pressing material, and the curing time is increased by 30min every time the thickness of the pressing material is increased by 1 mm. For example, the thickness of the press was 10 mm and the curing time was 300 min.
Example 2
In the embodiment, the insulating base material is ceramic paper or electronic cloth, and the electronic cloth is of a model of 7628 Yangtze river.
The procedure of producing prepreg A by applying the mixed slurry to the ceramic paper was the same as in example 1.
The electronic cloth gluing step is as follows, and the gluing mode is continuous operation.
Placing the mixed slurry in a glue tank, guiding cloth to perform single-shaft glue dipping by a tractor, controlling the glue amount by double-roller extrusion, adjusting the pressure of the double rollers, and controlling the glue applying amount to be 21 wt%; the dipped rubber material enters a chain type dryer to be dried under the action of the tension of a traction machine; the traction speed is 3m/min, the temperature of the dryer is set to be 140 ℃, the length of a oven box of the dryer is 9m, and the dryer is provided with a self-made deviation correcting device; and drying the dipped material to obtain a prepreg B, and cutting according to the specification of the ceramic paper.
Compounding and layering: a mode that 7 layers of prepregs A clamp 1 layer of prepregs B is adopted (a plurality of prepregs A clamp a plurality of prepregs B according to the sample plate requirement, and the thickness of the pressed ceramic paper is 0.2mm, and the thickness of the electronic cloth is 0.1mm for accounting).
The pressing process was the same as example 1, and a high-strength laminated thermal insulation composite material Y was finally obtained.
Example 3
In the embodiment, the insulating base material is ceramic paper or a piece of check cloth, the check cloth is 300g-1050 type, and the check cloth is glass fiber check cloth.
The procedure of producing prepreg A by applying the mixed slurry to the ceramic paper was the same as in example 1.
The checked fabric is glued by adopting a gum dipping mode, and the gluing mode is continuous operation.
Placing the mixed slurry in a glue tank, guiding cloth to be dipped in glue in a single shaft mode through a tractor, extruding the mixed slurry through double rollers to control the glue amount, adjusting the pressure of the double rollers, and controlling the glue applying amount to be not higher than 18 wt%; the dipped rubber material enters a chain type dryer to be dried under the action of the tension of a traction machine; the traction speed is 3m/min, the temperature of the dryer is set to be 140 ℃, the length of a oven box of the dryer is 9m, and the dryer is provided with a self-made deviation correcting device; and drying the dipped material to obtain a prepreg C, and cutting according to the specification of the ceramic paper.
Compounding and layering: the mode that 7 layers of prepregs A clamp 1 layer of prepregs C is adopted (a plurality of prepregs A clamp a plurality of prepregs C according to the sample plate requirement, and the thickness is 0.2mm after the ceramic paper is pressed and 0.3mm after the checked cloth is pressed).
The pressing process was the same as example 1, and a high-strength laminated thermal insulation composite material Z was finally obtained.
The high strength laminated thermal insulation composite prepared in example 1, example 2 and example 3 was subjected to performance tests, and the test results are shown in table 1:
TABLE 1
| Test item | X | Y | Z |
| Compressive strength/Mpa | 325 | 473 | 575 |
| Glass transition temperature (Tg)/. deg.C | 168 | 164 | 161 |
| Thermal conductivity/W.m-1K-1 | 0.2404 | 0.3021 | 0.3523 |
According to the detection result, the high-strength laminated heat-insulation composite material has the advantages of high compression strength, high Tg, low heat conductivity coefficient and the like. From the comparison of examples 1 and 2, it is clear that the gradient doping of the electronic cloth greatly improves the compressive strength of the sample, but slightly reduces the thermal resistance effect of the composite material, even if the thermal conductivity of the material is increased. It is clear from the comparison of examples 1 and 3 that the incorporation of the graticule gradient significantly improves the compressive strength of the sample, but the thermal resistance effect is significantly reduced, even though the thermal conductivity of the material is significantly increased.
In the above examples, the properties in each aspect are compared in combination, and example 2 is preferred; meanwhile, the embodiment 1 and the embodiment 3 can be adaptively supplied according to the requirements of manufacturers.
In the above examples, the preparation method and key techniques of the product of the present invention are described in detail, including but not limited to: controlling the resin content to be below 45 wt%; baking base materials with different resin contents, and then performing gradient stacking pressing; adopting doped checked cloth or 7628 electronic cloth to construct gradient material; different resin is adopted to construct the resin gradient material. wt% means mass ratio. The epoxy resin is one or more of E44 type epoxy resin, E50 type epoxy resin and E51 type epoxy resin.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (2)
1. A method for manufacturing a high-strength laminated heat-insulating composite material is characterized by comprising the following steps:
weighing 100 parts by mass of 638S-type novolac epoxy, 40 parts by mass of E44-type epoxy resin, 20 parts by mass of 4, 4' -diaminodiphenyl sulfone, 0.45 part by mass of V85-P-type hindered phenol antioxidant and 1.2 parts by mass of KH 560-type silane coupling agent, dissolving in acetone, and uniformly stirring to obtain premixed slurry;
step two, taking the premixed slurry, weighing an accelerator boron trifluoride monoethylamine according to the proportion of 10wt per mill of the solid content of resin in the premixed slurry, dissolving the boron trifluoride monoethylamine in acetone, and then uniformly stirring and mixing the boron trifluoride monoethylamine and the premixed slurry, wherein the modulation and curing time is 160-180 s, so as to obtain the mixed slurry for later use;
thirdly, gluing the insulating base material by using the mixed slurry;
step four, when the insulating base material is ceramic paper, dipping the insulating base material in a vacuum leading-in mode; cutting and weighing the ceramic paper, and checking the use amount of the mixed slurry according to the weight percent (45+5) by dry weight of the cut ceramic paper; introducing the mixed slurry, infiltrating the insulating base material, and standing for 30min to obtain a prepreg; taking out the prepreg, and placing the prepreg in an oven at 120 ℃ for baking for 3min to obtain a prepreg A; wherein the thickness of the ceramic paper is 2 mm;
when the insulating base material is electronic cloth, continuous gluing operation is adopted; placing the mixed slurry in a glue tank, leading the electronic cloth to be dipped in glue by a single shaft of a tractor, controlling the glue amount by double-roller extrusion, adjusting the pressure of the double rollers, and controlling the glue applying amount to be 21 wt%; the dipped rubber material enters a chain type dryer to be dried under the action of the tension of a traction machine; the traction speed is 3m/min, the temperature of the dryer is 140 ℃, the length of a oven box of the dryer is 9m, and the dipped material is dried to obtain a prepreg B; wherein, the electronic cloth is selected from a Changjiang river 7628 type;
step five, laying layers in a mode that 7 layers of prepregs A are used for clamping 1 layer of prepreg B, and pressing by a pressing machine;
step six, in the pressing process, the preheating temperature is 120 ℃, the preheating time is 30min, and the measured fluidity is 8-10%; after preheating, heating to 160 ℃ for curing, and obtaining the high-strength laminated heat-insulating composite material after curing; wherein, the thickness of each layer of ceramic paper after pressing is 0.2mm, and the thickness of each layer of electronic cloth after pressing is 0.1 mm.
2. The method of claim 1, wherein the laminated insulation composite comprises: in the pressing process, the curing time is set according to the thickness of the pressing material, and the curing time is increased by 30min every time the thickness of the pressing material is increased by 1 mm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010549682.7A CN111660649B (en) | 2020-06-16 | 2020-06-16 | Method for manufacturing high-strength laminated heat-insulation composite material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010549682.7A CN111660649B (en) | 2020-06-16 | 2020-06-16 | Method for manufacturing high-strength laminated heat-insulation composite material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN111660649A CN111660649A (en) | 2020-09-15 |
| CN111660649B true CN111660649B (en) | 2022-04-12 |
Family
ID=72387747
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010549682.7A Active CN111660649B (en) | 2020-06-16 | 2020-06-16 | Method for manufacturing high-strength laminated heat-insulation composite material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111660649B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112812505A (en) * | 2020-12-28 | 2021-05-18 | 理诚动力传控技术(苏州)有限公司 | Composite heat-resistant material for engine heat shield and preparation method thereof |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102731969B (en) * | 2012-06-18 | 2014-12-17 | 航天材料及工艺研究所 | Flame retardant epoxy prepreg composite material |
| CN109825033A (en) * | 2018-12-29 | 2019-05-31 | 浙江华正新材料股份有限公司 | A kind of light composite material and preparation method thereof of high Tg |
-
2020
- 2020-06-16 CN CN202010549682.7A patent/CN111660649B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN111660649A (en) | 2020-09-15 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111098523B (en) | Composite material light cabin and preparation method thereof | |
| CN102167611B (en) | Method for preparing carbon/carbon composite material plate | |
| CN110790530B (en) | High-strength nano heat-insulating material and preparation method thereof | |
| CN111660649B (en) | Method for manufacturing high-strength laminated heat-insulation composite material | |
| CN114230990B (en) | Light wood fiber/polylactic acid composite material and preparation method thereof | |
| CN110951103A (en) | Carbon fiber reinforced phenolic aerogel composite material, preparation method thereof and carbon fiber reinforced carbon aerogel composite material | |
| CN114055818A (en) | Rubber-based flexible composite material and preparation method thereof | |
| CN109768296A (en) | A kind of bipolar plate of all-vanadium redox flow battery and its preparation process | |
| CN103146216A (en) | High-energy rubber product as well as preparation method and application thereof | |
| CN111532010B (en) | Preparation process of insulating and heat-insulating laminated composite material | |
| CN114149551A (en) | Hot-melt phenolic resin, prepreg, composite material and preparation method | |
| CN105109068B (en) | A kind of non-autoclave shaping preimpregnation preparation method for material | |
| CN115975346B (en) | Epoxy resin premix for OOA cured prepreg and preparation method thereof | |
| CN112481817A (en) | Carbon fiber heat insulation material and preparation method thereof | |
| CN110561648B (en) | Preparation method of non-autoclave molding medium-temperature curing prepreg | |
| CN112851384A (en) | Preparation method of low-temperature sintered ceramic matrix composite based on silicon carbide fiber reinforcement | |
| CN115259881B (en) | Carbon/carbon composite material bearing plate and preparation method thereof | |
| CN107759989B (en) | Basalt fabric reinforced polylactic acid composite material and preparation method thereof | |
| CN111844804B (en) | Microwave curing process and device for fiber winding composite material | |
| CN113997681A (en) | Method for improving shock resistance of thin ceramic plate | |
| CN115449219B (en) | Silica aerogel quartz fiber polyimide ternary composite material and preparation method and application thereof | |
| CN115160738B (en) | Epoxy prepreg and preparation method of molded product thereof | |
| CN111907086A (en) | Preparation method of SMC composite material containing fireproof heat-insulation ceramic silicone rubber | |
| CN115872766B (en) | Preparation method of carbon-carbon material heat preservation device and heat preservation device | |
| CN115196941B (en) | Preparation method of inorganic polymer prepreg and composite material prepared by using preparation method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |